CN104945855A - Quantum dot/epoxy resin microspheres and preparation method thereof as well as color conversion film - Google Patents
Quantum dot/epoxy resin microspheres and preparation method thereof as well as color conversion film Download PDFInfo
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- CN104945855A CN104945855A CN201410110333.XA CN201410110333A CN104945855A CN 104945855 A CN104945855 A CN 104945855A CN 201410110333 A CN201410110333 A CN 201410110333A CN 104945855 A CN104945855 A CN 104945855A
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Abstract
The invention discloses a quantum dot/epoxy resin microspheres and a preparation method thereof as well as a color conversion film. The quantum dot/epoxy resin microspheres are prepared by encapsulating quantum dots in epoxy resin microsphere cavities. By encapsulating the quantum dots in the epoxy resin microsphere cavities, the probability of causing agglomeration due to interaction of the quantum dots is effectively reduced, and the probabilities that the quantum dots are in contact with a photoresist external environment and are interfered and damaged during photoetching of a photoresist are reduced. Meanwhile, due to the interaction between the epoxy resin microspheres and a photoresist resin matrix, the quantum dots can be dispersed into the photoresist more easily, and are dispersed uniformly without agglomeration. Therefore, the photoluminescence properties of the quantum dots are beneficially ensured. A sub-pixel unit with R/G/B colors corresponding to the prepared color conversion film is purer in color and higher in saturation degree, and the backlight source energy utilization efficiency and the luminous efficiency are also improved obviously.
Description
Technical field
The present invention relates to LCD Technology field, particularly relate to a kind of quantum dot/epoxide resin microballoon and preparation method thereof and Colours conversion films.
Background technology
The important method that liquid-crystal display (LCD) realizes full-color display is exactly that backlight adds filter technology.Backlight is generally blue LED (Light Emitting Diode, LED) and excites YAG fluorescent powder to launch white backlight, and this white backlight is the mixed light of blue light and gold-tinted, and color is impure.And colored filter mainly plays filter action, the white light of backlight, by the red, green, blue three look pigment photoresistor in the corresponding each pixel of colored filter, forms red, green, blue, is finally mixed to form chromatic image.Colored filter becomes film preparation by the photoresist material of the pigment that is scattered here and there.Its light-filtering characteristic depends on the absorption Spectrum characteristic of pigment itself and size and distribution.Therefore often filter thorough not, picture colour gamut is lower, and color saturation is poor, and light source utilization rate is low.
Therefore, prior art need development.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of quantum dot/epoxide resin microballoon and preparation method and Colours conversion films, the optical filtering mode being intended to solve the use of available liquid crystal indicating meter is thorough not, picture colour gamut is lower, color saturation is poor, the problem that light source utilization rate is low.
Technical scheme of the present invention is as follows:
A kind of quantum dot/epoxide resin microballoon, wherein, described quantum dot/epoxide resin microballoon is encapsulated in epoxide resin microballoon cavity by quantum dot to be prepared from.
Described quantum dot/epoxide resin microballoon, wherein, in described quantum dot/epoxide resin microballoon, the massfraction of the quantum dot of compound is 0 ~ 50%, the content non-zero of described quantum dot.
Described quantum dot/epoxide resin microballoon, wherein, described quantum dot is made up of one or more compounds in CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgTe, GaN, GaAs, InP, InAs.
Described quantum dot/epoxide resin microballoon, wherein, described quantum dot is homogeneous mixed type, gradient mixed type, core-shell structure copolymer type or union type.
Described quantum dot/epoxide resin microballoon, wherein, described quantum dot/epoxide resin microballoon surface is simultaneously containing-OH, epoxide group and double bond group.
A preparation method for quantum dot/epoxide resin microballoon as above, wherein, said method comprising the steps of:
A, to count by weight, 1 ~ 10 part of emulsifying agent, 0 ~ 10 part of assistant for emulsifying agent and 500 ~ 1000 parts of deionized waters are mixed, is mixed with aqueous phase system;
B, under agitation, count by weight, by 100 parts of epoxy resin, 0 ~ 50 part of quantum dot, 80 ~ 100 portions of reactive thinners and 8 ~ 20 parts of obtained oil-based systems of solidifying agent mixing, wherein, described quantum dot content is not 0;
C, under agitation, described oil-based system is poured in aqueous phase system, two-phase mixtures evenly after emulsification 10 ~ 30min, be more slowly warming up to 80 ~ 85 DEG C, the reaction times is 2 ~ 5h;
D, after naturally cooling, product to be filtered, dry, obtain quantum dot/epoxide resin microballoon.
The preparation method of described quantum dot/epoxide resin microballoon, wherein, described emulsifying agent is one or both in Sudan Gum-arabic, alkylphenol polyoxyethylene;
Described assistant for emulsifying agent is one or more in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, Nonyl pheno chain, polyoxyethylene glycol, tween and Si Ban;
Described reactive thinner is epoxide resin reactive diluent;
Described solidifying agent is aliphatics amine, aromatic amine, tertiary amine class, imidazole and its derivants class, Versamid or organic acid anhydride class solidifying agent.
A kind of Colours conversion films, wherein, described Colours conversion films prepares in the photoresist by dispersed for quantum dot/epoxide resin microballoon as above.
Described Colours conversion films, wherein, in described Colours conversion films, the massfraction of the quantum dot of doping is 0 ~ 20%, wherein, the content non-zero of described quantum dot.
Beneficial effect: the invention provides a kind of quantum dot/epoxide resin microballoon and preparation method thereof and Colours conversion films, by quantum dot being encapsulated in epoxide resin microballoon cavity, effectively reduce the possibility that quantum dot interphase interaction occurs to reunite then, decrease the probability that quantum dot contacts with photoresist material external environment and is interfered in photoresist material photoetching process and destroys.Simultaneously due to the interaction of epoxide resin microballoon and photoresist material resin matrix, quantum dot is more easily distributed in photoresist material, is uniformly dispersed, soilless sticking.Thus the favourable photoluminescence property that ensure that quantum dot.The color of the sub-pixel unit of the R/G/B color that prepared Colours conversion films is corresponding is purer, and saturation ratio is higher, and backlight energy utilization efficiency and luminous efficiency are also improved significantly.
Embodiment
The invention provides a kind of quantum dot/epoxide resin microballoon and preparation method thereof and Colours conversion films, 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 quantum dot (Quantum Dot) of nano-scale has absorption peak width, emission peak is narrow, the activity beneficial that emission wavelength is adjustable, replace conventional pigment with it and be distributed in photoresist material, R/G/B monochromatic ray is directly produced by the mode of photoexcitation by playing the UV/ blue light that LED is sent, color is purer, saturation ratio is higher, and luminous efficiency is also higher.
And quantum dot disperses the photoluminescence property of the Colours conversion films prepared in the photoresist to depend on the chemical property of quantum dot surface and its distribution in the photoresist.
Atresia epoxy resin (EP) microballoon has the advantage that chemical stability is good, mechanical strength is high, uniform granularity, pH value try out a wider range, not easily produce irreversible adsorption effect, particularly its surface can reactive group containing-OH etc., can be given that it is different functional by autotelic surface modification.
Therefore, stablize to obtain surface atom, be uniformly dispersed quantum dot photoresist material, in advance quantum dot can be wrapped up one deck atresia epoxide resin microballoon shell.
Concrete, the invention provides a kind of quantum dot/epoxide resin microballoon, wherein, described quantum dot/epoxide resin microballoon is encapsulated in epoxide resin microballoon cavity by quantum dot to be prepared from.Wherein, described quantum dot/epoxide resin microballoon surface is simultaneously containing-OH, epoxide group and double bond group.
In described quantum dot/epoxide resin microballoon, the massfraction of the quantum dot of compound is 0 ~ 50%, the content non-zero of described quantum dot.
Above-mentioned quantum dot used is made up of one or more compounds in CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgTe, GaN, GaAs, InP, InAs.Wherein, described quantum dot is homogeneous mixed type, gradient mixed type, core-shell structure copolymer type or union type.
In preferred embodiment, described quantum dot is oil soluble quantum dot, and in addition, described quantum dot can be the quantum dot of doping or undoped.
Further, the part of described quantum dot is one or more in sour part, mercaptan part, amine ligand, (oxygen) Phosphine ligands, phosphatide, soft phosphatide, polyvinylpyridine etc.Wherein, described sour part comprises one or more in ten acid, undecylenic acid, TETRADECONIC ACID, oleic acid and stearic acid; Described mercaptan part comprise in eight alkyl sulfhydryls, lauryl mercaptan and Stearyl mercaptan one or more; Described amine ligand comprise in oleyl amine, stearylamine and eight amine one or more; Described (oxygen) Phosphine ligands comprise tri octyl phosphine, trioctylphosphine oxide (TOPO) one or more.
The present invention also provides a kind of preparation method of quantum dot/epoxide resin microballoon as above, wherein, said method comprising the steps of:
A, to count by weight, 1 ~ 10 part of emulsifying agent, 0 ~ 10 part of assistant for emulsifying agent and 500 ~ 1000 parts of deionized waters are mixed, is mixed with aqueous phase system;
B, under agitation, count by weight, by 100 parts of epoxy resin, 0 ~ 50 part of quantum dot, 80 ~ 100 portions of reactive thinners and 8 ~ 20 parts of obtained oil-based systems of solidifying agent mixing, wherein, described quantum dot content is not 0;
C, under agitation, described oil-based system is poured in aqueous phase system, two-phase mixtures evenly after emulsification 10 ~ 30min, be more slowly warming up to 80 ~ 85 DEG C, the reaction times is 2 ~ 5h;
D, after naturally cooling, product to be filtered, dry, obtain the micron order quantum dot/atresia epoxide resin microballoon of surface containing active group.
Wherein, described epoxy resin is monomer, and it can be one in the epoxy resin of any type or arbitrary combination.As bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin or phenol aldehyde type epoxy resin etc. after low viscosity glycidyl ether type epoxy resin, bisphenol A type epoxy resin, hydrogenation.
Described emulsifying agent is one or both in Sudan Gum-arabic, alkylphenol polyoxyethylene; Described assistant for emulsifying agent is one or more in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, Nonyl pheno chain, polyoxyethylene glycol, tween and Si Ban; Described reactive thinner is epoxide resin reactive diluent.
Described solidifying agent is amine curing agent, imidazole and its derivants class, Versamid or organic acid anhydride class solidifying agent.Wherein, described organic acid anhydride class solidifying agent is methyl hexahydrophthalic anhydride or HHPA etc., described amine curing agent is aliphatics amine, and aromatic amine, tertiary amine class solidifying agent, described amine curing agent is specifically as follows four butyl bromation amine or tetraethyl-amine bromide etc.Described imidazole and its derivants class solidifying agent is imidazoles, glyoxal ethyline, 2-ethyl-4-methylimidazole or vinyl imidazole etc.
The invention provides a kind of Colours conversion films, it is the optical conversion film that UV/ blue light for being sent by backlight is converted into R/G/B three primary colours.Described Colours conversion films prepares in the photoresist by dispersed for quantum dot/epoxide resin microballoon as above.Wherein, in described Colours conversion films, the massfraction of the quantum dot of doping is 0 ~ 20%, wherein, and the content non-zero of described quantum dot.Preferred undersaturated quantum dot/epoxide resin microballoon, crosslinking reaction can be there is with photoresist material in exposure in it, thus obtain the more stable and dispersion of quantum dot surface chemistry character evenly, the more stable Colours conversion films of physical and chemical performance.
Above-mentioned photoresist material major ingredient used is alkali soluble resin, light-cured resin, light trigger, organic solvent and other additives, and wherein, light-cured resin mainly comprises acrylic resin, polyimide based resin, polyvinyl alcohol resin etc.
The preparation method of described Colours conversion films comprises the steps:
I) described quantum dot/epoxide resin microballoon dispersion in the photoresist, and is coated on the transparency carrier of the black matrix" prepared;
Ii) by film described in mask exposure;
Iii) to develop described exposed film.
The purity of the Colours conversion films prepared by above method is significantly promoted, thus also improves colour gamut and the efficiency of the display frame of display unit.
By the following examples the present invention is further detailed.
Embodiment 1
Surface is containing the preparation method of the CdTe/CdS quantum dot/epoxide resin microballoon of-OH group: in 250ml tri-mouthfuls of reaction flasks, add 0.8g Sudan Gum-arabic, 0.4g Sodium dodecylbenzene sulfonate and a 100ml deionized water, stirs and makes it fully dissolve.Under agitation, the CdTe/CdS quantum dot of transmitting red light stable for 10g bisphenol A type epoxy resin E51,0.5g oleic acid, 10g epoxy propane butyl ether and 1.5g modification glyoxal ethyline are mixed and obtains oil-based system, then oil-based system is joined in there-necked flask, after stirring and emulsifying 20min, slowly be warming up between 80-85 DEG C, isothermal reaction 4h.After reaction terminates, stop heating, make it naturally cool to room temperature.By product filtration, drying, obtain head product.By head product after fixing 1h at 150 DEG C, namely obtain surface containing-OH group CdTe/CdS quantum dot/epoxide resin microballoon.
CdTe/CdS quantum dot/epoxide resin microballoon that two kinds are launched blueness, green light is respectively prepared according to ratio above.
The preparation method of described quantum dot Colours conversion films, comprises the steps:
I) the CdTe/CdS quantum dot/epoxide resin microballoon of prepare three kinds of colors is dispersed in the photoresist material of three kinds of same system respectively above;
Ii) by the photoresist material rotary coating containing a kind of color quantum dot on the transparency carrier of the black matrix" prepared;
Iii) by film described in mask exposure;
Iv) to develop described exposed film;
V) by other two kinds of photoresist materials containing quantum dot according to step I i-iv repetitive operation.Prepare the quantum dot Colours conversion films containing R/G/B sub-pixel.
Embodiment 2
Surface contains the preparation method of the CdSe/ZnS quantum dot/epoxide resin microballoon of-OH and epoxide group: in 250ml tri-mouthfuls of reaction flasks, add 1g alkylphenol polyoxyethylene, 0.6g sodium lauryl sulphate, 0.2g polyoxyethylene glycol and a 100ml deionized water, stirs and makes it fully dissolve.Under agitation, the CdSe/ZnS quantum dot of the transmitting green light of 5g bisphenol A type epoxy resin E51,5g alicyclic type epoxy resin 711,0.4g trioctylphosphine oxygen phosphorus stabilizer, 10g propylene oxide benzylic ether and 0.8g 2-ethyl-4-methylimidazole are mixed and obtains oil-based system, then oil-based system is joined in there-necked flask, after stirring and emulsifying 30min, slowly be warming up between 80-85 DEG C, isothermal reaction 3h.Reaction terminates rear stopping heating, makes it naturally cool to room temperature.By product filtration, drying, obtain CdSe/ZnS quantum dot/epoxide resin microballoon that surface contains-OH and epoxide group.
CdTe/CdS quantum dot/epoxide resin microballoon that two kinds are launched blueness, red light is respectively prepared according to ratio above.
The preparation method of described quantum dot Colours conversion films, comprises the steps:
I) the CdSe/ZnS quantum dot/epoxide resin microballoon of prepare three kinds of colors is dispersed in the photoresist material of three kinds of same system respectively above;
Ii) by the photoresist material rotary coating containing a kind of color quantum dot on the transparency carrier of the black matrix" prepared;
Iii) by film described in mask exposure, can there is crosslinked film forming in epoxide group further in photoresist material post bake process;
Iv) to develop described exposed film;
V) by other two kinds of photoresist materials containing quantum dot according to step I i-iv repetitive operation.Prepare the quantum dot Colours conversion films containing R/G/B sub-pixel.
Embodiment 3
Surface is containing the preparation method of the CdTe/CdS/ZnS quantum dot/epoxide resin microballoon of-OH, epoxide group and double bond group: in 250ml tri-mouthfuls of reaction flasks, add 0.7g Sudan Gum-arabic, 0.4g Sodium dodecylbenzene sulfonate and a 80ml deionized water, stirs and makes it fully dissolve.Under agitation, the CdTe/CdS/ZnS quantum dot of transmitting blue light stable for 10g bisphenol A type epoxy resin E44,0.5g oleic acid, 10g epoxy propane butyl ether and 0.8g vinyl imidazole are mixed, obtain oil-based system, then oil-based system is joined in there-necked flask, after stirring and emulsifying 20min, slowly be warming up between 80-85 DEG C, isothermal reaction 3h.After reaction terminates, stop heating, make it naturally cool to room temperature.By product filtration, drying, obtain the CdTe/CdS/ZnS quantum dot/epoxide resin microballoon of surface containing-OH, epoxide group and double bond group.
CdTe/CdS quantum dot/the epoxide resin microballoon of two kinds of difference transmitting greens, red light is prepared according to ratio above.
The preparation method of described quantum dot Colours conversion films, comprises the steps:
I) the CdTe/CdS/ZnS quantum dot/epoxide resin microballoon of prepare three kinds of colors is dispersed in the photoresist material of three kinds of same system respectively above;
Ii) by the photoresist material rotary coating containing a kind of color quantum dot on the transparency carrier of the black matrix" prepared;
Iii) by film described in mask exposure, on vinyl imidazole double bond further with acrylic ester monomer generation crosslinking reaction in photoresist material, also can there is crosslinked film forming further in photoresist material post bake process in epoxide group;
Iv) to develop described exposed film;
V) by other two kinds of photoresist materials containing quantum dot according to step I i-iv repetitive operation.Prepare the quantum dot Colours conversion films containing R/G/B sub-pixel.
The invention provides a kind of quantum dot/epoxide resin microballoon and preparation method thereof and Colours conversion films, by quantum dot being encapsulated in epoxide resin microballoon cavity, effectively reduce the possibility that quantum dot interphase interaction occurs to reunite then, decrease the probability that quantum dot contacts with photoresist material external environment and is interfered in photoresist material photoetching process and destroys.Simultaneously due to the interaction of epoxide resin microballoon and photoresist material resin matrix, quantum dot is more easily distributed in photoresist material, is uniformly dispersed, soilless sticking.Thus the favourable photoluminescence property that ensure that quantum dot.The color of the sub-pixel unit of the R/G/B color that prepared Colours conversion films is corresponding is purer, and saturation ratio is higher, and backlight energy utilization efficiency and luminous efficiency also obtain obviously higher.
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 domain that all should belong to claims of the present invention.
Claims (9)
1. quantum dot/epoxide resin microballoon, is characterized in that, described quantum dot/epoxide resin microballoon is encapsulated in epoxide resin microballoon cavity by quantum dot to be prepared from.
2. quantum dot/epoxide resin microballoon according to claim 1, is characterized in that, in described quantum dot/epoxide resin microballoon, the massfraction of the quantum dot of compound is 0 ~ 50%, the content non-zero of described quantum dot.
3. quantum dot/epoxide resin microballoon according to claim 1, is characterized in that, described quantum dot is made up of one or more compounds in CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgTe, GaN, GaAs, InP, InAs.
4. quantum dot/epoxide resin microballoon according to claim 1, is characterized in that, described quantum dot is homogeneous mixed type, gradient mixed type, core-shell structure copolymer type or union type.
5. quantum dot/epoxide resin microballoon according to claim 1, is characterized in that, described quantum dot/epoxide resin microballoon surface is simultaneously containing-OH, epoxide group and double bond group.
6. a preparation method for the quantum dot/epoxide resin microballoon as described in any one of claim 1 ~ 5, is characterized in that, said method comprising the steps of:
A, to count by weight, 1 ~ 10 part of emulsifying agent, 0 ~ 10 part of assistant for emulsifying agent and 500 ~ 1000 parts of deionized waters are mixed, is mixed with aqueous phase system;
B, under agitation, count by weight, by 100 parts of epoxy resin, 0 ~ 50 part of quantum dot, 80 ~ 100 portions of reactive thinners and 8 ~ 20 parts of obtained oil-based systems of solidifying agent mixing, wherein, described quantum dot content is not 0;
C, under agitation, described oil-based system is poured in aqueous phase system, two-phase mixtures evenly after emulsification 10 ~ 30min, be more slowly warming up to 80 ~ 85 DEG C, the reaction times is 2 ~ 5h;
D, after naturally cooling, product to be filtered, dry, obtain quantum dot/epoxide resin microballoon.
7. the preparation method of quantum dot/epoxide resin microballoon according to claim 6, is characterized in that, described emulsifying agent is one or both in Sudan Gum-arabic, alkylphenol polyoxyethylene;
Described assistant for emulsifying agent is one or more in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, Nonyl pheno chain, polyoxyethylene glycol, tween and Si Ban;
Described reactive thinner is epoxide resin reactive diluent;
Described solidifying agent is aliphatics amine, aromatic amine, tertiary amine class, imidazole and its derivants class, Versamid or organic acid anhydride class solidifying agent.
8. a Colours conversion films, is characterized in that, described Colours conversion films prepares dispersed for the quantum dot/epoxide resin microballoon as described in any one of claim 1 ~ 5 in the photoresist.
9. Colours conversion films according to claim 8, is characterized in that, in described Colours conversion films, the massfraction of the quantum dot of doping is 0 ~ 20%, wherein, and the content non-zero of described quantum dot.
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| CN105199322A (en) * | 2015-10-10 | 2015-12-30 | 苏州大学 | Epoxy resin microsphere and preparation method thereof |
| CN106876562A (en) * | 2017-03-30 | 2017-06-20 | 广东普加福光电科技有限公司 | A kind of new micro LED structure and preparation method thereof |
| CN108160013A (en) * | 2017-12-15 | 2018-06-15 | 华南理工大学 | A kind of Water-soluble carbon quantum dot slow-release microcapsule and preparation method and application |
| CN108752825A (en) * | 2018-05-30 | 2018-11-06 | 深圳市华星光电技术有限公司 | Quantum dot hydrogel, quantum dot patterning and transfer method |
| CN109423275A (en) * | 2017-08-29 | 2019-03-05 | 纳晶科技股份有限公司 | Quantum dot composition, quantum dot light emitting material, preparation method and the luminescent device containing it |
| CN114019762A (en) * | 2021-10-27 | 2022-02-08 | 电子科技大学 | Method for preparing nano array by laser evanescent wave near-field interference quantum lithography |
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| CN105199322A (en) * | 2015-10-10 | 2015-12-30 | 苏州大学 | Epoxy resin microsphere and preparation method thereof |
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| CN108160013B (en) * | 2017-12-15 | 2020-08-18 | 华南理工大学 | Water-soluble carbon quantum dot sustained-release microcapsule and preparation method and application thereof |
| CN108752825A (en) * | 2018-05-30 | 2018-11-06 | 深圳市华星光电技术有限公司 | Quantum dot hydrogel, quantum dot patterning and transfer method |
| CN114019762A (en) * | 2021-10-27 | 2022-02-08 | 电子科技大学 | Method for preparing nano array by laser evanescent wave near-field interference quantum lithography |
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