CN108987606B - Preparation method of light extraction film and O L ED device with light extraction film - Google Patents
Preparation method of light extraction film and O L ED device with light extraction film Download PDFInfo
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Abstract
The invention provides a preparation method of a light extraction film and an O L ED device with the light extraction film, wherein the light extraction film comprises a light extraction layer and a connecting layer arranged on one side of the light extraction layer, the light extraction layer comprises a matrix, nanoparticles and a dispersing agent, the nanoparticles and the dispersing agent are positioned in the matrix, and the light extraction film changes a transmission path of light penetrating through the light extraction film through the scattering effect of the microstructure of the nanoparticles on the light, reduces the total reflection of the light at an interface, and can effectively improve the luminous efficiency of the O L ED device when one side of the light extraction layer is attached to the luminous surface of a molded O L ED device.
Description
Technical Field
The invention relates to the technical field of photoelectricity, in particular to a light extraction film, a preparation method of the light extraction film and an O L ED device with the light extraction film.
Background
Organic light Emitting diodes (Organic L light-Emitting diodes, O L ED) have been widely used in lighting and display panels to meet the requirements of low power consumption, lightness, thinness, flexibility, folding, surface light source, etc. however, in O L ED devices, most of the light is lost due to total reflection at the interfaces of the layers, resulting in lower practical light Emitting efficiency.
Light loss is particularly severe at the interfaces between the high and low index layers, such as the interfaces between Indium Tin Oxide (ITO) and the substrate, and so the addition of light extraction films at these interfaces can greatly improve the luminous efficiency of O L ED devices.
However, the existing light extraction film has too many requirements on the process and preparation although the manufacturing process is simple, and on the other hand, the existing light extraction film directly prepares the light extraction film at the required interface in the process of preparing the O L ED device, so that the manufacturing time of the O L ED device is prolonged, and the manufactured O L ED device cannot be improved.
In view of the above, it is desirable to provide a light extraction film, a method for preparing the same, and an O L ED device having the same, so as to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a light extraction film, a preparation method thereof and an O L ED device with the light extraction film.
In order to achieve the above object, the present invention provides a light extraction film, which includes a light extraction layer, a coupling layer disposed on one side of the light extraction layer, wherein the light extraction layer includes a matrix, and nanoparticles and a dispersant disposed in the matrix.
As a further improvement of the invention, the light extraction film further comprises a protective layer disposed on a side of the tie layer remote from the light extraction layer.
As a further improvement of the invention, the protective layer is a silicon dioxide layer or an aluminum oxide layer film.
As a further improvement of the invention, the particle size of the nano-particles is between 100nm and 1 um.
As a further improvement of the invention, the tie layer is a cured layer of the same material as the substrate.
In order to achieve the above object, the present invention further provides a method for preparing a light extraction film, comprising the steps of: s1, adding a dispersing agent and nano particles into a solvent to prepare a mother solution; wherein the volume ratio of the solvent, the dispersant and the nano particles is as follows: 50-70 parts of solvent, 5-15 parts of dispersant and 20-40 parts of nano particles; s2, stirring and mixing the mother liquor; s3, adding the first curing adhesive and the solvent into the mother liquor obtained in the step S2 for secondary preparation; the volume ratio of the mother solution obtained after S2 mixing to the first curing adhesive to the solvent is as follows: the mother solution is 50-80 parts, the first curing adhesive is 5-20 parts, and the solvent is 20-40 parts; s4, preparing a film on the soft or hard smooth plane by using the solution mixed in the step S3 through glue homogenizing, slit coating, spraying, film scraping or screen printing; s5, curing the film to form a light extraction layer; s6, preparing a layer of second curing adhesive on the surface of the light extraction layer in a glue homogenizing, slit coating, spraying, film scraping or screen printing mode, and forming a connecting layer after curing.
As a further improvement of the present invention, the method for producing a light extraction film further includes step S7, which is located after step S6: and depositing a silicon dioxide layer or an aluminum oxide layer film on one side of the connecting layer far away from the light extraction layer to form a protective layer.
As a further improvement of the invention, the first curing adhesive is a thermal curing adhesive or a UV adhesive, and the second curing adhesive is a thermal curing adhesive or a UV adhesive.
As a further improvement of the invention, the preparation method of the light extraction film specifically comprises the following steps: in step S1, the volume ratio of the solvent to the dispersant to the nanoparticles is 60:10: 30; in the step S2, carrying out ball milling or ultrasonic mixing on the mother solution for 1-3 h; in the step S3, adding UV glue and a solvent into the mother liquor, and mixing for 10min to 1 h; wherein the volume ratio of the mother liquor to the UV adhesive to the solvent is 70:10: 30; in step S4, forming a thin film with a thickness of 1-20 μm on glass, PET or sapphire from the solution mixed in step S3; in step S5, curing the film under UV illumination for 5-10 min to form a light extraction layer, wherein the wavelength of the UV illumination is 356-256 nm; in step S6, a layer of UV glue is prepared on the surface of the cured film by glue homogenizing, slit coating, spraying, film scraping or screen printing, and then the UV glue is cured for 5min to 20min under the UV illumination with the wavelength of 356nm to 256nm to form a connecting layer.
To achieve the above object, the present invention further provides an O L ED device comprising a substrate, an anode, an organic light emitting layer, a cathode, wherein the O L ED device further comprises a light extraction film, wherein the light extraction film is located on the side of the substrate facing away from the anode, or the light extraction film is located between the substrate and the anode.
The light extraction film has the beneficial effects that the light extraction film changes the transmission path of light penetrating through the light extraction film through the scattering effect of the microstructure of the nano particles on the light, and reduces the total reflection of the light at the interface, and when one side of the light extraction layer is attached to the light-emitting surface of the formed O L DE device, the light extraction film can effectively improve the light-emitting efficiency of the O L ED device.
Drawings
FIG. 1 is a schematic view of a light extraction film on a substrate according to a preferred embodiment of the present invention;
FIG. 2 is a graph of current efficiency versus current intensity for an A-1/A-2 device of the present invention;
FIG. 3 is a graph of lumens and current levels for an A-1/A-2 device of the present invention;
FIG. 4 is a schematic view of the luminescence spectrum of the A-1/A-2 device of the present invention;
FIG. 5 is a schematic representation of the enhanced emission spectra of the A-2 device relative to the A-1 device of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments shown in the drawings. These embodiments are not intended to limit the present invention, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present invention.
Fig. 1 is a schematic view of a light extraction film 100 of the present invention on a substrate M. The light extraction film 100 includes a light extraction layer 1, and a coupling layer 2 on one side of the light extraction layer 1. The light extraction layer 1 comprises a matrix 11, nanoparticles 12 positioned in the matrix 11, and a dispersing agent.
As will be appreciated by those skilled in the art: the refractive indices of the substrate 11 of the light extraction layer 1 and the tie layer 2 may be different, with a boundary between them; the coupling layer 2 may be formed of the same material as the base 11 of the light extraction layer 1, and there is no boundary between them in light transmission. Preferably, the refractive index of the substrate 11 of the light extraction layer 1 is the same as or similar to that of the protective layer 2, and the influence on the transmission of light is small.
The light extraction film 100 changes the transmission path of light penetrating through the light extraction film 100 through the scattering effect of the microstructure of the nano-particles 12 on the light, and reduces the total reflection of the light at the interface, the light extraction film 100 is prepared independently of an O L ED device, and when one side of the light extraction layer 1 of the light extraction film is attached to the light emitting surface of a molded O L DE device, the light extraction film 100 can effectively improve the light emitting efficiency of the O L ED device.
Wherein, the nanoparticles 12 are inorganic nanoparticles and/or organic nanoparticles, as long as the nanoparticles can be dispersed in the matrix 11 to improve the light extraction rate; for example, the nanoparticles 12 are selected from titanium dioxide and/or PS beads. The shape and size of the nanoparticles 12 are not limited, the particle size is between 100nm and 1um, and the light extraction rate can be improved.
Of course, the nanoparticles 12 in the light extraction layer 1 may also be a combination of nanoparticles 12 of different particle sizes and different sizes.
The dispersing agent plays a role in uniformly dispersing the nanoparticles 12 in the matrix 11 in the process of preparing the light extraction layer 1, and can be selected correspondingly according to the properties of the nanoparticles 12, wherein the dispersing agent can be selected from L-ubrizol commercial Solsperse36600, Solsperse24000 or Solsperse36000, and the Solsperse36600 series has the best effect because of certain brightening effect on titanium dioxide white powder.
The substrate 11 is usually a resin capable of forming a transparent film, such as a curable adhesive. For example, the light extraction layer 1 is formed by adding nanoparticles 12, a dispersant, and a curing adhesive into a solvent, dispersing, forming a thin film, and then curing. The solvent mentioned in the present invention may be a lipid, benzene, or ether, etc., such as butyl acetate.
The connecting layer 2 is positioned at the outer side of the light extraction layer 1, after the nano-particles 12 are added into the light extraction layer 1, the strength of the light extraction layer 1 is reduced, the strength of the whole film layer along the extension direction of the film needs to be improved through the connecting layer 2, so that the light extraction film 100 cannot be broken when being peeled, and the connecting layer also has the functions of buffering and protecting. In the present invention, the tie layer 2 may be a cured layer cured by UV glue or thermosetting glue, and the tie layer 2 increases its adhesion and stability to the light extraction layer 1.
Further, the light extraction film 100 further includes a protective layer (not shown) such as a silicon oxide layer or an aluminum oxide layer on the side of the coupling layer 2 away from the light extraction layer 1, which can prevent scratches and reduce the decrease in light transmittance due to the coupling layer 2 adsorbing oil or dust in the air.
The present invention also provides a method for preparing the light extraction film 100, in which the preparation process and the required equipment are simple, and the method for preparing the light extraction film 100 includes the following steps:
s1, adding a dispersing agent and nano particles 12 into a solvent to prepare a mother solution; wherein the volume ratio of the solvent, the dispersant and the nano particles is as follows: 50-70 parts of solvent, 5-15 parts of dispersant and 20-40 parts of nano particles. In the present invention, the nanoparticles 12 and the dispersant refer to the description in the above light extraction film 100, which is not described herein again; the solvent may be a lipid, benzene, or ether, etc., such as butyl acetate.
S2, stirring and mixing the mother liquor for 1-3 h, wherein the process can adopt but not limited to ball milling or ultrasonic technology as long as the mother liquor can be uniformly mixed.
S3, adding the first curing adhesive and the solvent into the mother liquor dispersed in the step S2 for secondary preparation, and mixing for 10 min-1 h; the volume ratio of the mother solution obtained after S2 mixing, the first curing glue and the solvent is set as follows: the curing adhesive comprises, by weight, 50-80 parts of mother liquor, 5-20 parts of first curing adhesive and 20-40 parts of solvent. The solvent in this step may be a lipid, benzene, or ether, such as butyl acetate; the solvent in this step may be the same as or different from the solvent in S1, and is preferably the same, and has good compatibility.
S4, preparing the solution mixed in the step S3 on soft or hard smooth planes such as glass, PET, sapphire and the like by means of glue homogenizing, slit coating, spraying, film scraping, screen printing and the like, and preparing a thin film with the film thickness of 1-20 microns;
and S5, curing the film to form the light extraction layer 1.
S6, preparing a layer of second curing adhesive on the surface of the light extraction layer 1 through glue homogenizing, slit coating, spraying, film scraping, screen printing and the like, and forming the connecting layer 2 after curing.
The first curing glue in step S3 may be a thermal curing glue or a UV glue, and the curing step in step S5 is selected according to the applicability of the first curing glue. Preferably, the first curing adhesive is a UV adhesive, has low curing temperature, and can be suitable for hard substrates and flexible substrates; the curing step in S5 is: curing for 5-10 min under UV illumination with wavelength of 356-256 nm.
Preferably, the second curing glue is the same as the first curing glue, so that the refractive index between the substrate 11 of the light extraction layer 1 and the coupling layer 2 is the same, and light is not lost in the transmission process. For example, the second curing adhesive is the same UV adhesive as the first curing adhesive, and the coupling layer 2 can be formed by curing for 5min to 20min under the UV illumination with the wavelength between 356nm and 256 nm.
In the preparation method of the light extraction film 100, the curing glue is added into the mother solution in the step S3, so that on one hand, the problem of poor dispersion effect caused by viscosity can be avoided, and the formed light extraction film has uniformly dispersed nano-particles 12 and better light extraction effect; on the other hand, an additive with a certain function can be added into the curing adhesive during secondary timing to improve the performance of the light scattering film.
In the second dispensing, additives that may be added to the curing glue include, but are not limited to: 1) the defoaming agent is used for improving the film forming property of the light extraction film so that the surface of the light extraction film is more smooth and has no bubble phenomenon; because the added curing adhesive has certain viscosity, the defoaming agent is added to avoid the phenomenon of bubbles; 2) viscosity modifier, which increases the viscosity of the film formed subsequently and makes it not easy to separate and precipitate; 3) a reinforcing agent to increase the strength of the light extraction film; 4) due to the existence of the curing glue, intermolecular force is generated between the light extraction film 100 and the glass surface, and the light extraction film 100 after being transferred can be tightly attached for multiple times.
The following description will be made with respect to a specific method of manufacturing the light extraction film 100:
s1, selecting any one of the dispersing agent, the nano-particles 12 and the solvent, wherein the solvent, the dispersing agent and the nano-particles 12 are prepared into a mother solution according to the volume ratio of 60:10: 30; s2, carrying out ball milling or ultrasonic mixing on the mother liquor for 1-3 h; s3, adding UV glue and a solvent after the mother liquor is dispersed, and mixing and dispersing for 10 min-1 h; wherein the volume ratio of the dispersed mother liquor, the UV glue and the solvent is 70:10: 30; s4, preparing the solution mixed in the step S3 on soft or hard smooth planes such as glass, PET, sapphire and the like by means of glue homogenizing, slit coating, spraying, film scraping, screen printing and the like to form a thin film with the thickness of 1-20 microns; s5, curing the film for 5-10 min under UV illumination to form a light extraction layer 1, wherein the wavelength of the UV illumination is 356-256 nm; s6, preparing a layer of UV glue on the surface of the cured film through glue homogenizing, slit coating, spraying, film scraping, screen printing and other modes, curing for 5-20 min under UV illumination with the wavelength of 356-256 nm to form the connecting layer 2, and thus forming the transferable, adhesive, uniform and compact light extraction film 100.
The above-described preparation method of the present invention will be described in detail below by providing a more specific embodiment:
firstly, preparing a mother solution according to the proportion, which specifically comprises the following components: 30 parts of titanium dioxide nanoparticles, 60 parts of solvent and 10 parts of dispersant; then adding curing glue and solvent into the prepared mother liquor, and uniformly mixing to form a solution; wherein the mother liquor: solvent: the part ratio of the curing adhesive is 70: 30: 10. spin-coating the solution at 2000rpm for 30s to form a film; curing for 5min under UV illumination with the wavelength of 356 nm-256 nm after the spin coating is finished; and 3016 coating curing glue, and curing for 10min under the UV illumination with the wavelength of 356 nm-256 nm to form a uniform and compact light extraction film.
In addition, the method of manufacturing the light extraction film of any one of the above further includes a step S7 after the step S6: and a silicon dioxide layer or an aluminum oxide layer film is deposited on one side of the connecting layer, which is far away from the light extraction layer, to form a protective layer, so that scratches can be prevented, and the reduction of light transmittance caused by the fact that the connecting layer 2 absorbs oil stains or dust in the air can be reduced.
The invention also provides an O L ED device, which comprises a substrate, an anode, an organic light-emitting layer, a cathode and the light extraction film 100, wherein the light extraction film 100 is attached to one side of the substrate, which is far away from the anode, and compared with an O L ED device without the light extraction film 100, the light efficiency is increased by more than 85 parts.
The following tests were conducted with the light extraction film 100 attached to the side of the substrate facing away from the anode as an example:
as shown in fig. 2 to 4, it is shown that the light extraction efficiency of the light extraction film 100 is greatly improved after the light extraction film 100 is attached to the light emitting surface of the conventional O L ED device, and it can be seen from the above structure that the improvement of the light extraction film 100 to the O L ED device is over 85% with the adjustment of different solid content ratios, as can be seen from fig. 2, the improvement of the current efficiency cd/a of the light extraction film 100 of the present invention is close to 87%.
In summary, the light extraction film 100 of the present invention changes the transmission path of light passing through the light extraction film 100 by the scattering effect of the microstructure of the nanoparticles 12 on the light, and reduces the total reflection of light at the interface, and when the light extraction layer 1 side is attached to the light emitting surface of the formed O L ED device, the light extraction film 100 can effectively improve the light emitting efficiency of the formed O L ED device.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method of making a light extraction film, comprising the steps of:
s1, adding a dispersing agent and nano particles into a solvent to prepare a mother solution; wherein the volume ratio of the solvent, the dispersant and the nano particles is as follows: 50-70 parts of solvent, 5-15 parts of dispersant and 20-40 parts of nano particles;
s2, stirring and mixing the mother liquor;
s3, adding the first curing adhesive and the solvent into the mother liquor obtained in the step S2 for secondary preparation; the volume ratio of the mother solution obtained after S2 mixing to the first curing adhesive to the solvent is as follows: the mother solution is 50-80 parts, the first curing adhesive is 5-20 parts, and the solvent is 20-40 parts;
s4, preparing a film on the soft or hard smooth plane by using the solution mixed in the step S3 through glue homogenizing, slit coating, spraying, film scraping or screen printing;
s5, curing the film to form a light extraction layer;
s6, preparing a layer of second curing adhesive on the surface of the light extraction layer in a glue homogenizing, slit coating, spraying, film scraping or screen printing mode, and forming a connecting layer after curing.
2. The method of producing a light extraction film according to claim 1, characterized in that: the method of manufacturing a light extraction film further includes a step S7, which is located after the step S6: and depositing a silicon dioxide layer or an aluminum oxide layer film on one side of the connecting layer far away from the light extraction layer to form a protective layer.
3. The method of producing a light extraction film according to claim 1, characterized in that: the first curing glue is thermal curing glue or UV glue, and the second curing glue is thermal curing glue or UV glue.
4. The method of producing a light extraction film according to claim 1, characterized in that: the preparation method of the light extraction film comprises the following specific steps:
in step S1, the volume ratio of the solvent to the dispersant to the nanoparticles is 60:10: 30;
in the step S2, carrying out ball milling or ultrasonic mixing on the mother solution for 1-3 h;
in the step S3, adding UV glue and a solvent into the mother liquor, and mixing for 10min to 1 h; wherein the volume ratio of the mother liquor to the UV adhesive to the solvent is 70:10: 30;
in step S4, forming a thin film with a thickness of 1-20 μm on glass, PET or sapphire from the solution mixed in step S3;
in step S5, curing the film under UV illumination for 5-10 min to form a light extraction layer, wherein the wavelength of the UV illumination is 356-256 nm;
in step S6, a layer of UV glue is prepared on the surface of the cured film by glue homogenizing, slit coating, spraying, film scraping or screen printing, and then the UV glue is cured for 5min to 20min under the UV illumination with the wavelength of 356nm to 256nm to form a connecting layer.
5. An O L ED device, comprising a substrate, an anode, an organic light-emitting layer and a cathode, wherein the O L ED device further comprises a light extraction film prepared by the method for preparing the light extraction film of any one of claims 1 to 4, the light extraction film is positioned on the side of the substrate away from the anode, or the light extraction film is positioned between the substrate and the anode.
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| CN102368540A (en) * | 2011-08-22 | 2012-03-07 | 友达光电股份有限公司 | Organic light emitting diode structure and manufacturing and using method of optical film |
| CN103608295A (en) * | 2011-07-14 | 2014-02-26 | Ltc有限公司 | Inorganic particle scattering film having good light-extraction performance |
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| CN102683231B (en) * | 2012-05-31 | 2015-07-08 | 昆山维信诺显示技术有限公司 | Preparation method of high-refractive-index scattering film and application |
| KR102313052B1 (en) * | 2016-02-02 | 2021-10-15 | 버세리엔 피엘씨 | Method of preparing a graphene-based thin-film laminate and the graphene-based thin-film laminate |
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| CN103608295A (en) * | 2011-07-14 | 2014-02-26 | Ltc有限公司 | Inorganic particle scattering film having good light-extraction performance |
| CN102368540A (en) * | 2011-08-22 | 2012-03-07 | 友达光电股份有限公司 | Organic light emitting diode structure and manufacturing and using method of optical film |
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