CN109585685B - Light extraction structure, manufacturing method thereof and light emitting device - Google Patents
Light extraction structure, manufacturing method thereof and light emitting device Download PDFInfo
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Abstract
The invention provides a light extraction structure, a manufacturing method thereof and a light emitting device. The manufacturing method comprises the following steps: providing a substrate; wet-manufacturing a first film layer on a substrate by using a first solution, wherein the first solution comprises a material A and a solvent B; and drying the first film layer to form a first film layer with a porous structure, wherein the first film layer with the porous structure is the light extraction structure. The membranous layer through the random porous structure of wet process formation on the basement, perhaps, utilize this random porous structure to further set up the light extraction structure of random protruding type, such light extraction structure not only helps improving the luminous angle homogeneity that promotes luminescent device, but also is favorable to improving luminescent device's light efficiency.
Description
Technical Field
The invention relates to the field of light emitting diodes, in particular to a light extraction structure, a manufacturing method thereof and a light emitting device.
Background
Through the development of Organic Light Emitting Diodes (OLEDs) in about 30 years, abundant results are obtained in material development and device structure design, OLEDs are already in large-scale commercial use on display, especially high-end smart phones, the market is not formed in the field of illumination due to reasons of price, service life and the like, but the efficiency of the OLED device is required to be improved no matter the OLED device is used for display or illumination, the limit of the layered structure characteristics of the device is met, only about 20% of photons generated under current driving can smoothly break through the fact that an emitting device is captured by human eyes, and the rest photons are dissipated inside the device, so that the heat is generated, the electric energy is wasted, and the service life of the device is also influenced. In recent years, quantum dot light emitting diodes (QLEDs) which have attracted attention due to characteristics such as wide color gamut and high luminance are also layered structures, and it is also important to improve device efficiency by an efficient light extraction technique in order to realize commercialization.
Light extraction techniques are classified into external light extraction techniques and internal light extraction techniques according to the difference in the device site of interface modification. The external light extraction technology is mainly used for inhibiting the total reflection of an interface by modifying the outer surface of a substrate and utilizing the principle of scattering or converging beams. Common methods include surface roughening, microlens arrays, surface patterned films, and surface scattering dielectric layers. These external structures can only couple light trapped in the substrate mode. The internal light extraction technique can extract light in a waveguide mode such as an ITO-organic layer and a surface plasmon mode. The external light extraction technology is widely applied because the technology is simple and can be independently processed with an organic layer. And the internal light extraction relates to the internal structure of the device, the regulation and control are relatively complex, but the internal light extraction can obtain higher device efficiency improvement.
However, in both the external light extraction and the internal light extraction, the interfaces modified by the prior art are mostly fabricated by means of photolithography and the like to realize light extraction, which can improve the device efficiency, but are expensive in manufacturing cost, and the angle uniformity is not improved due to the regular structure, and the color rendering uniformity is extremely important in both the display and illumination fields.
Disclosure of Invention
The invention mainly aims to provide a light extraction structure, a manufacturing method thereof and a light-emitting device, so as to solve the problem that the light extraction structure in the prior art is difficult to improve the uniformity of the light-emitting angle of a corresponding device.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method of fabricating a light extraction structure, the method comprising the steps of: providing a substrate; wet-manufacturing a first film layer on a substrate by using a first solution, wherein the first solution comprises a material A and a solvent B; and drying the first film layer to form a first film layer with a porous structure, wherein the first film layer with the porous structure is the light extraction structure.
Further, after the step of forming the first film layer having a porous structure, the manufacturing method further includes: arranging a material C on the first membrane layer with the porous structure to form a second membrane layer, wherein part of the material C is arranged on the substrate through the porous structure; and removing the first film layer and the second film layer arranged on the surface of the first film layer, and reserving the material C positioned on the substrate to form a protruding structure, wherein the protruding structure is the light extraction structure.
Furthermore, the thickness of the first film layer is larger than that of the second film layer, and the thickness of the first film layer is 10 nm-10 μm.
Further, removing the first film layer and the second film layer arranged on the surface of the first film layer by adopting a solvent washing or adhesive tape stripping mode; preferably, the solvent rinse is performed with a good solvent for the first film layer.
Further, the substrate is a functional film layer, an electrode layer or a nonfunctional carrier; preferably, the functional film layer is selected from any one of a hole injection layer, a hole transport layer, a light emitting layer, an electron injection layer, an electron transport layer, a hole blocking layer, and an electron blocking layer; preferably, the non-functional support is a transparent substrate.
Further, the solvent B comprises a first boiling point solvent, and the first boiling point solvent is selected from one or more organic solvents with the boiling point of 80-300 ℃.
Further, the solvent B also comprises a second boiling point solvent, and the second boiling point solvent is selected from one or more organic solvents with the boiling point of 60-120 ℃; preferably, the volume ratio of the first boiling point solvent to the second boiling point solvent in the solvent B is 95: 5-5: 95.
Furthermore, the melting point of the first boiling point solvent is more than or equal to 15 ℃.
Further, material a is selected from one or more of the following materials: the nano silver ink comprises a high polymer material, oxide nanocrystals, nano silver wires, silver ink, inorganic particles, a photo-curing glue composition, a thermosetting glue composition and sol-gel.
Further, the material A is selected from one or more of high molecular materials, the molecular weight of the high molecular materials is not less than 1000, and the glass transition temperature Tg≥80℃。
Further, material C is selected from one or more of the following materials: metal oxides, nitrides, oxynitrides, fluorides, and metals.
According to a second aspect of the present application, there is provided a light extraction structure fabricated by any one of the above-described fabrication methods.
According to a third aspect of the present application, a bottom emission light emitting device is provided, the bottom emission light emitting device includes a non-functional carrier, a semi-transparent electrode layer, a functional film layer and a reflective electrode layer, which are sequentially disposed from bottom to top, wherein the functional film layer includes a plurality of sub-functional film layers, the bottom emission light emitting device further includes a light extraction structure, the light extraction structure is located between any two adjacent layers of the non-functional carrier, the semi-transparent electrode layer, the functional film layer and the reflective electrode layer, or between any two adjacent sub-functional film layers of the functional film layer, or is located on a side surface of the non-functional carrier far away from the semi-transparent electrode layer, and the light extraction structure is the above light extraction structure.
Further, the light extraction structure is positioned between any layers from the semitransparent electrode layer to the reflecting electrode layer, and the refractive index value of the light extraction structure is 1.5-2; or the light extraction structure is positioned between the non-functional carrier and the semitransparent electrode layer, and the refractive index value of the light extraction structure is 1.5-1.8; or the light extraction structure is positioned on the surface of one side, far away from the semi-transparent electrode layer, of the non-functional carrier, and the refractive index value of the light extraction structure is 1-1.5.
According to a fourth aspect of the present application, a top emission light emitting device is provided, which includes a non-functional carrier, a reflective electrode layer, a functional film layer, a semi-transparent electrode layer, and an encapsulation layer, which are sequentially disposed from bottom to top, and further includes a light extraction structure, wherein the functional film layer includes a plurality of sub-functional film layers, the light extraction structure is located between any two adjacent layers, and the light extraction structure is the light extraction structure.
Further, the packaging layer is a packaging cover plate or a film; preferably, the light extraction structure is positioned between any two adjacent layers from the semi-transparent electrode layer to the reflective electrode layer, and the refractive index value of the light extraction structure is 1.5-2; or the light extraction structure is positioned between the packaging layer and the semitransparent electrode, and the refractive index value of the light extraction structure is 1-1.8.
By applying the technical scheme of the invention, the film layer with the irregular porous structure is formed on the substrate by a wet method, or the irregular porous structure is further provided with the irregular convex light extraction structure, so that the light extraction structure is not only beneficial to improving the uniformity of the light emitting angle of the light emitting device, but also beneficial to improving the light efficiency of the light emitting device.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a graph showing the results of comparing the luminous efficiencies as a function of angle of the light-emitting devices according to examples 1 to 5 of the present invention and comparative examples 1 and 2.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
Interpretation of terms:
the functional film layer and the functional polymer material have functions of a device, that is, a film layer or a polymer material having functions of hole injection, hole transport, electron injection, electron transport, light emission, electron blocking, and the like.
Refractive index, as used herein, does not refer to the refractive index value of the bulk material, but rather the refractive index value of the light extraction structure formed as a whole. For example, if the ratio of the volume of the holes (air refractive index of 1) to the volume of material A (refractive index of 1.5 itself) in the first film layer is 1:1, then the refractive index value of the first film layer would be approximately 1.25. Effective refractive index value n of mixture film layerIs effectiveThe following formula can be used for approximate calculation: n isIs effective＝f*n1+(1-f)*n2Wherein f is the volume fraction of the material 1 and the refractive index of the material itself is n1(ii) a (1-f) is the volume fraction of material 2, the refractive index of the material itself being n2。
In order to improve the current situation, a typical embodiment of the present application provides a method for manufacturing a light extraction structure, which includes the following steps: providing a substrate; wet-processing a first film layer on a substrate by using a first solution; drying the first film layer to form a first film layer with a porous structure, wherein the first film layer with the porous structure is the light extraction structure; wherein the first solution comprises a material A and a solvent B.
According to the manufacturing method of the light extraction structure, the film layer with the irregular porous structure is formed on the substrate through the solution of the material A in a wet method, and the light extraction structure is not only beneficial to improving the angle uniformity of light, but also beneficial to improving the lighting effect of the applied light-emitting device.
In the step of drying the first membrane layer to form the first membrane layer having a porous structure, the drying is not limited to a specific manner, including but not limited to drying by rapid heating or vacuum pumping, so that the solvent B is volatilized.
The manufacturing method is a wet method, the solvent is volatilized after the first solution is dried, a random porous light extraction structure is formed, and the light extraction structure belongs to a concave light extraction structure when the light extraction structure is subsequently applied to a light-emitting device. The LED lamp can improve the light effect and the angle uniformity of light, and the preparation process is simple.
Further, the convex light extraction structure can also achieve the same effect. In order to meet the manufacturing requirements of a wider range of light emitting devices, in a preferred embodiment, after the step of forming the first film layer having a porous structure, the manufacturing method further comprises the steps of: arranging a material C on the first membrane layer with the porous structure to form a second membrane layer, wherein part of the material C is arranged on the substrate through the porous structure; and removing the first film layer and the second film layer on the surface of the first film layer, and reserving the material C on the substrate to form a convex structure, wherein the convex structure is the light extraction structure and belongs to a convex light extraction structure.
In the above preferred embodiment, since the first film layer is a porous structure, when the material C is disposed thereon, a part of the material C contacts the base layer through the porous structure, and after the first film layer and the second film layer on the surface of the first film layer are removed, the material C disposed in contact with the base layer forms a convex light extraction structure on the base layer.
In the manufacturing process of the convex light extraction structure, the specific thicknesses of the first film layer and the second film layer are not specially limited, so long as the material C can leak from the porous structure of the first film layer, and when the material C is removed, the first film layer can be completely removed together with the second film layer. In a preferred embodiment, the thickness of the first film layer is greater than that of the second film layer, and the thickness of the first film layer is 10 nm-10 μm. The thickness of the first film layer is larger than that of the second film layer, so that the subsequent stripping removal is facilitated.
In the manufacturing process of the convex light extraction structure, the thickness of the second film layer is smaller than that of the first film layer, so that the first film layer and the second film layer on the surface of the first film layer can be peeled off completely. When the convex light extraction structure is positioned between any two functional film layers of the device or between the electrode layer and the non-functional carrier, the thickness of each functional film layer is only a few nanometers to a hundred nanometers, and the thickness of the electrode layer is also only a few tens to a few hundreds nanometers, so that the thickness of the convex light extraction structure (corresponding to the thickness of the second film layer) is also in the range, and the thickness of other functional film layers is not uniform due to large fluctuation; when the convex light extraction structure is located at other positions, such as the side of the non-functional carrier far away from the functional film layer of the device, the thickness of the convex light extraction structure can be hundreds of nanometers to several micrometers, and the large fluctuation in the light extraction structure does not affect the uniformity of each functional film layer of the device, and the size of the convex light extraction structure is equivalent to the wavelength of light, so that the light extraction of the device is also obviously improved. The thickness range of the first film layer is also selected in accordance with the above principles.
In the step of wet-forming the first film layer on the substrate using the first solution, the substrate may be divided into a functional film layer, an electrode layer, and a non-functional carrier. The functional film layer can be selected from any one of a hole injection layer, a hole transport layer, a light-emitting layer, an electron injection layer, an electron transport layer, a hole blocking layer and an electron blocking layer; but not the functional support, may be selected from transparent substrates, preferably glass or polymer films. And the specific method for forming the first film layer by the wet method includes, but is not limited to, any one of spin coating, ink jet printing, slit coating, spray coating and embossing.
In the step of forming the second film layer by disposing the material C on the first film layer having the porous structure, the material C may be disposed in a deposition method such as CVD (chemical vapor deposition) or PVD (physical vapor deposition).
In the step of removing the first film layer and the second film layer on the surface of the first film layer to form the convex light extraction structure, the specific removing method may be solvent rinsing or tape stripping. Preferably, the solvent washing is carried out by using the good solvent of the first film layer; the good solvent should be a poor solvent for the substrate material, and should not damage the substrate.
The solvent B is different depending on the kind of the material a, and the material a is dissolved in the solvent B. In one or more embodiments, solvent B comprises a first boiling point solvent selected from one or more of organic solvents having a boiling point of 80 ℃ to 300 ℃; when the boiling point of the first boiling point solvent is within the above range, after the film is formed by a conventional wet process, a certain amount of the first boiling point solvent is necessarily contained in the wet film, and at this time, when the wet film is treated by a rapid drying method (such as high-temperature heating or vacuum pumping), the first boiling point solvent in the wet film rapidly escapes from the film to form pores, so that the first film layer with a porous structure is obtained. Preferably, the first boiling point solvent may be selected from organic solvents having a boiling point within the above range, such as aromatic hydrocarbons, esters, ethers, alcohols, and alcohol ethers.
The solvent B can also comprise a second boiling point solvent according to actual needs on the basis of containing the first boiling point solvent, and the second boiling point solvent is selected from one or more organic solvents with the boiling point of 60-120 ℃; preferably, the volume ratio of the first boiling point solvent to the second boiling point solvent in the solvent B is 95:5 to 5:95, and more preferably 1:9 to 8: 2. The second boiling point solvent has a lower boiling point, so that the second boiling point solvent is preferentially and quickly volatilized during wet film forming, the viscosity of the system is quickly increased to enable the wet film to be shaped earlier, at the moment, the first boiling point solvent is slowly volatilized, so that more residues are left in the wet film, and after the wet film is treated by a quick drying mode, the first film layer with a porous structure can be obtained. Specifically, the organic solvent having a boiling point of 60 to 120 ℃ includes, but is not limited to, n-hexane, cyclohexane, acetone, tetrahydrofuran, toluene, ethanol, and the like.
In a more preferred embodiment, the first boiling solvent has a melting point of 15 ℃ or higher. When the first film layer is manufactured by a wet method, generally, the second boiling point solvent with a relatively low boiling point is preferentially volatilized; in certain embodiments, the second boiling point solvent has the same boiling point as the first boiling point solvent (or the second boiling point solvent has a boiling point higher than the first boiling point solvent, but each is still within the respective boiling point range), and the two are close in volatility while gradually evaporating. In both cases, the system temperature of the solvent B is lowered, and the first boiling point solvent is solidified and separated out when the system temperature is lowered to the freezing point thereof or the amount of the second boiling point solvent remaining in the wet film is insufficient to maintain the second boiling point solvent in a liquid state distributed in the solvent B due to the high melting point of the first boiling point solvent. These solidified first boiling solvents are then quickly removed, and the area originally occupied by the "solid" first boiling solvents is "emptied" to form pores in the first film layer. Therefore, the first membrane layer having the porous structure with different sizes, numbers and distributions can be obtained by adjusting the combination (including the combination of different kinds or volumes) of the first boiling point solvent and the second boiling point solvent.
In one or more embodiments, material a is selected from one or more of the following materials: high polymer material, oxide nanocrystal, nano silver wire, silver ink, inorganic particulate matter, light curing glue composition, heat curing glue composition and sol-gel.
In the step of preparing the first film layer having a porous structure (i.e., the concave light extraction structure), the material a includes, but is not limited to, one or more of the following materials: the nano silver ink comprises a high polymer material, oxide nanocrystals, nano silver wires, silver ink, inorganic particles, a photo-curing glue composition, a thermosetting glue composition and sol-gel. Wherein the polymer material is a functional polymer material or a non-functional polymer material; in some embodiments, the functional polymer material is selected from one or more of Polyvinylcarbazole (PVK), poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), polyvinylpyrrolidone (PVP), and the non-functional polymer material is selected from one or more of Polymethylmethacrylate (PMMA), Polystyrene (PS), polyethylene terephthalate (PET), Polycarbonate (PC), Polyimide (PI), Polyurethane (PU), and polyvinyl chloride (PVC). The inorganic particulate matter is selected from one or more of oxide particles, nitride particles, oxynitride particles and fluoride particles; in some embodiments, the inorganic particulate material has a particle size of 3nm to 400 nm. The photo-curing glue composition or the thermosetting glue composition is selected only by considering that the cured photo-curing glue composition or the thermosetting glue composition can resist the heating temperature in the subsequent manufacturing process of other films of the device, and does not deform or yellow.
In the above examples, the oxide nanocrystals were different from the inorganic particles in particle size. The light extraction structures are arranged at different positions of the light emitting device, and the selected particle size requirements are different. When the light extraction structure is disposed adjacent to the functional film layer of the device, it is preferable to use oxide nanocrystals, the particle size of which is generally several nanometers to several tens of nanometers, for example, a concave light extraction structure is disposed between the electron transport layer and the light emitting layer, and the material a (zinc oxide nanocrystals) can be selected as the material a, and after the first film layer prepared by wet process is dried, the material a (zinc oxide nanocrystals) is retained in the device as the light extraction structure, so that the effect of improving the angular uniformity of light is achieved, and the effect of the second electron transport layer is also achieved, and the uniformity of other functional film layers of the device is not significantly affected by the waviness caused by the material a. When the light extraction structure is arranged at a position not adjacent to the functional film layer, inorganic particles are preferably used, the relatively larger particle size of the inorganic particles is equivalent to the light-emitting wavelength of the light-emitting layer, the scattering capability of light is strong, and the effects of improving the light-emitting efficiency and the angle uniformity can be realized.
The functional polymer material or the non-functional polymer material has a function of injecting or transporting holes in a device.
In other embodiments, the material A is selected from one or more non-functional polymer materials, the molecular weight of the polymer materials is not less than 1000, and the glass transition temperature T isgNot less than 80 ℃. Further, material C is selected from one or more of the following materials: metal oxides, nitrides, oxynitrides, fluorides, and metals.
In the step of forming the convex light extraction structure, the material a is selected from one or more non-functional polymer materials, the polymer materials have a molecular weight of not less than 1000 and a glass transition temperature TgNot less than 80 ℃, and controlling the glass transition temperature TgThe temperature of not less than 80 ℃ is used for ensuring that the porous structure appearance of the first film layer can be maintained and cannot be deformed due to slight heating when the second film layer is arranged, so that the second film layer material cannot smoothly pass through the holes to be deposited on the substrate.
The material C may be chosen appropriately according to the position of the raised light extraction structure to be subsequently located in the device. In a preferred embodiment, material C is selected from one or more of the following materials: metal oxides, nitrides, oxynitrides, fluorides, and metals. More preferably, the material is selected from molybdenum oxide (MoO)3) Nickel oxide (NiO), zinc oxide (ZnO), aluminum oxide (Al)2O3) Indium Tin Oxide (ITO), silicon dioxide (SiO)2) AZO (aluminum zinc oxide), titanium dioxide (TiO)2) Silicon nitride (Si)3N4) One or more of silver (Ag) and aluminum (Al). It should be noted that the contribution of the material C to the improvement of the light emitting effect of the device is derived from the shape of the protruding structure, the protruding structure changes the propagation direction of light, and increases the proportion of light overflowing to air, thereby increasing the light emitting efficiency, and due to the fact that the material C is different in size and distribution, the random arrangement is favorable for improving the light emitting angle uniformity of the device.
In a second exemplary embodiment of the present application, a light extraction structure is provided, which is fabricated by any one of the fabrication methods described above. By adopting the method, the preparation method is simple, and the formed light extraction structure is of a random porous structure, so that the angle uniformity of light is improved. In addition, the method of the present application can be used for preparing a convex light extraction structure and a concave light extraction structure according to practical application requirements, and the light extraction structure of the present application has a wide application range, and can be used in a plurality of positions of a device, for example, as a part of a substrate, or a part of a substrate electrode, or on the back of the substrate, or as a functional layer inside the device.
In a third exemplary embodiment of the present application, a bottom emission light emitting device is provided, where the bottom emission light emitting device includes a light extraction structure, and a non-functional carrier, a semi-transparent electrode layer, a functional film layer, and a reflective electrode layer sequentially arranged from bottom to top, where the functional film layer includes a plurality of sub-functional film layers, and the light extraction structure is located between any two adjacent layers of the non-functional carrier, the semi-transparent electrode layer, the functional film layer, and the reflective electrode layer, or between any two sub-functional film layers of the functional film layer, or on a side surface of the non-functional carrier away from the semi-transparent electrode layer, where the light extraction structure is any one of the light extraction structures, and may be the concave light extraction structure or the convex light extraction structure.
Further, according to the shape of the light extraction structure (here, a concave light extraction structure or a convex light extraction structure), the arrangement position in the device, and the difference of the used materials, the obtained light extraction structure has different refractive indexes, which is helpful for improving the uniformity of the light extraction angle of the bottom emission light emitting device. The device has wide application range and can be arranged at a plurality of positions of the device.
In some preferred embodiments, the light extraction structure is located between any two layers from the semi-transparent electrode layer to the reflective electrode layer, i.e. the light extraction structure may be located between the semi-transparent electrode and the functional film layer, or between any two sub-functional film layers, or between the functional film layer and the reflective electrode layer, and the refractive index value of the light extraction structure at the above location is 1.5-2. In one or more embodiments, the concave light extraction structure is disposed between any two layers from the semitransparent electrode layer to the reflective electrode layer, and the material a may be selected from various functional polymer materials or oxide nanocrystals, or electrode layer materials such as nano silver wires, silver paste, and ITO (sol-gel), where the functional polymer materials and the oxide nanocrystals are explained above and are not described herein again. In one or more embodiments, the convex light extraction structure is arranged between any two layers from the semitransparent electrode layer to the reflecting electrode layer, the material A is selected from one or more non-functional high polymer materials, the molecular weight of the high polymer materials is not less than 1000, and the glass transition temperature Tg is not less than 80 ℃; the material C is selected from metal oxides, such as molybdenum oxide, nickel oxide, zinc oxide and the like, is arranged by adopting a CVD or PVD method, and forms a convex light extraction structure after being processed, and can simultaneously play a functional role in hole injection or electron transport and the like according to the specific position of the material in a device.
In some preferred embodiments, the light extraction structure is located between the non-functional carrier and the translucent electrode layer, the refractive index value of the light extraction structure is 1.5-1.8, and the reason why the refractive index value of the light extraction structure is controlled to be in the above range when the light extraction structure is located between the non-functional carrier and the translucent electrode layer is that the refractive index of the non-functional carrier is generally about 1.5, the refractive index of the translucent electrode is 1.8, and the refractive index of the light extraction structure is located between the non-functional carrier and the translucent electrode layer, so as to improve the light transmittance.
In one or more embodiments, the concave light extraction structure is disposed between the non-functional carrier and the translucent electrode layer, and the material a may be one or more selected from the group consisting of non-functional polymer materials, inorganic particles, photo-curable glue compositions, and thermal-curable glue compositions. In one or more embodiments, the light extraction structure of convex shape is disposed between the non-functional carrier and the translucent electrode layer, the material a is selected from one or more of non-functional polymer materials, and the material C is selected from one or more of metal oxides, nitrides, oxynitrides, and fluorides.
In some preferred embodiments, the light extraction structure is located on one side surface of the non-functional carrier far away from the semi-transparent electrode layer, and the refractive index value of the light extraction structure is 1-1.5. When the light extraction structure is arranged on the surface of one side of the non-functional carrier far away from the semitransparent electrode layer, the light extraction structure is located between the non-functional carrier and air, the refractive index of the non-functional carrier is about 1.5 generally, the refractive index of the air is about 1, and the refractive index of the light extraction structure is located between the non-functional carrier and the air, so that the light transmittance is improved.
In a fourth exemplary embodiment of the present application, a top-emission light-emitting device is provided, which includes a light extraction structure, and a nonfunctional carrier, a reflective electrode layer, a functional film layer, a translucent electrode layer, and an encapsulation layer, which are sequentially disposed from bottom to top, where the functional film layer includes a plurality of sub-functional film layers, the light extraction structure may be located between any two adjacent layers, and the light extraction structure is the above-mentioned light extraction structure.
Any two adjacent layers described above include any two adjacent layers of the plurality of sub-functional film layers. The top emission light-emitting device adopting the light extraction structure has the advantage of uniform and consistent light-emitting angle.
The packaging layer can be formed by adopting the existing packaging structure. In a preferred embodiment, the encapsulation layer is an encapsulation cover or film. The thin film herein refers to a thin film used in a thin film encapsulation process commonly used for a light emitting device, which is a stacked structure of organic and inorganic materials, and is not a single polymer.
In order to further improve the uniformity of the light emitting angle of the top emission light emitting device, in a preferred embodiment, the light extraction structure is located between any two adjacent layers from the semitransparent electrode layer to the reflective electrode layer, that is, the light extraction structure may be located between the semitransparent electrode layer and the functional film layer, or between any two functional film layers, or between the functional film layer and the reflective electrode layer, and the refractive index value of the light extraction structure located at the above position is 1.5-2. The selection of the material of the light extraction structure in the preferred embodiment is the same as that of the light extraction structure in the bottom emission light emitting device between any two layers of the semitransparent electrode layer and the reflective electrode layer, and therefore, the description thereof is omitted.
In another preferred embodiment, the light extraction structure is located between the packaging layer and the semi-transparent electrode, and the refractive index value of the light extraction structure is 1-1.8. In a further preferred embodiment, the light extraction structure is located between the non-functional carrier and the reflective electrode layer, and the refractive index value of the light extraction structure is not required, since the reflective electrode layer can reflect light without the light passing through the light extraction structure.
The advantageous effects of the present application will be further described with reference to specific examples.
Example 1
The concave light extraction structure is applied to a bottom-emitting light-emitting device:
spin-coating a 1 wt% polyimide N-methyl pyrrolidone solution on alkali-free white glass with a thickness of 0.7mm at 2500rpm, placing the glass in a vacuum drying oven (DZF desk type vacuum drying oven) after the spin-coating is finished, and performing vacuum drying at 150 ℃ for 60min to obtain a light extraction structure, wherein the pit depth of the glass is about 25nm when the light extraction structure is tested by a DEKTAK XT type step profiler;
after 150nm ITO (150W, Ar:48sccm) is subjected to radio frequency sputtering on the glass provided with the light extraction structure (containing a mask plate convenient for electrode extraction), PEDOT (PSS (40nm, Heraeus E100), a toluene solution (the thickness of the toluene solution is 30nm) of TFB, an octane solution (the thickness of the octane solution is 30nm) of green quantum dots (CdSe/CdS) and an ethanol solution (the thickness of the ethanol solution is 50nm) of ZnO nanocrystals are sequentially subjected to spin coating, the thickness of Ag is 100nm, and the bottom-emitting QLED device is obtained after packaging.
Example 2
The convex light extraction structure is applied to a bottom emission light emitting device:
dissolving polystyrene particles in anisole to prepare a 5 wt% solution, spin-coating at 1500rpm on alkali-free white glass to form a film, vacuum-drying at 100 ℃ for 30min, transferring the substrate to a radio frequency sputtering cavity, sputtering for 1000s at 150W and 48sccm of argon gas flow, wherein the target material is ITO, washing the substrate with tetrahydrofuran solvent after sputtering is finished, removing the polystyrene material, drying to obtain a light extraction structure, and measuring the height of the highest part of the bump by a step profiler to be about 50 nm;
after 150nm ITO (150W, Ar:48sccm) is subjected to radio frequency sputtering on the substrate provided with the light extraction structure (containing a mask plate convenient for electrode extraction), PEDOT (PSS (40nm, Heraeus E100), a toluene solution (the thickness of the toluene solution is 30nm) of TFB, an octane solution (the thickness of the octane solution is 30nm) of green quantum dots (CdSe/CdS) and an ethanol solution (the thickness of the ethanol solution is 50nm) of ZnO nanocrystals are sequentially subjected to spin coating, the thickness of Ag is 100nm, and the bottom-emitting QLED device is obtained after packaging.
Example 3
The concave light extraction structure is applied to a top-emitting light-emitting device:
spin-coating a 1 wt% polyimide N-methyl pyrrolidone solution on alkali-free white glass with a thickness of 0.7mm at 2500rpm, placing the glass in a vacuum drying oven (DZF desk type vacuum drying oven) after the spin-coating is finished, and performing vacuum drying at 150 ℃ for 60min to obtain a light extraction structure;
and performing radio frequency sputtering on the glass provided with the light extraction structure (containing a mask plate convenient for electrode extraction) to form 100nm Ag (150W, Ar:48sccm) and 15nm ITO (150W, Ar:48sccm) in sequence, then performing spin coating on PEDOT (PSS (40nm in film thickness, Heraeus E100), a toluene solution (30nm in film thickness) of TFB, an octane solution (30nm in film thickness) of green quantum dots (CdSe/CdS) and an ethanol solution (50nm) of ZnO nanocrystals, evaporating the Ag with the film thickness of 20nm, and packaging to obtain the top-emitting QLED device.
Example 4
The convex light extraction structure is applied to a top emission light emitting device:
dissolving polystyrene particles in anisole to prepare a 5 wt% solution, spin-coating the solution on alkali-free white glass at the rotating speed of 1500rpm to form a film, drying the film in vacuum at the temperature of 100 ℃ for 30min, transferring the substrate to a radio frequency sputtering cavity, sputtering the film for 1000s at the argon flow of 150W and 48sccm to obtain a target material of ITO, washing the substrate with a tetrahydrofuran solvent after the sputtering is finished, removing the polystyrene material, and drying to obtain a light extraction structure;
and performing radio frequency sputtering on the substrate provided with the light extraction structure (containing a mask plate convenient for electrode extraction) to obtain 100nm Ag (150W, Ar:48sccm) and 15nm ITO (150W, Ar:48sccm) in sequence, performing spin coating on PEDOT (PSS (40nm in film thickness, Heraeus E100), a toluene solution (30nm in film thickness) of TFB, an octane solution (30nm in film thickness) of green quantum dots (CdSe/CdS) and an ethanol solution (50nm in film thickness) of ZnO, performing vapor deposition on Ag with a film thickness of 20nm, and packaging to obtain the top-emitting QLED device.
Examples 5 to 26 were prepared by referring to the above examples, and the raw materials used in the respective steps of examples 1 to 26 are shown in tables 1 and 2, and the preparation conditions in the respective steps are shown in table 3. Examples 1 and 3 are steps of fabricating a concave light extraction structure and steps of fabricating a corresponding device, and examples 2 and 4 are steps of fabricating a convex light extraction structure and steps of fabricating a corresponding device. Of examples 5 to 26, the odd-numbered examples were concave light extraction structures, the even-numbered examples were convex light extraction structures, examples 5 to 16 were top-emission light-emitting devices, and examples 17 to 26 were bottom-emission light-emitting devices.
In the above method for fabricating the convex structure, the solvent B that dissolves the material a at the previous stage (or other solvents that are soluble to the material a but insoluble to the material C) is used for rinsing or directly removing the material a by using an adhesive tape, and no specific description is given in the table.
Table 1:
table 2: physical Properties of the raw materials used in Table 1
Table 3: preparation conditions of examples
In addition, since the position of the bottom emission glass substrate away from the functional layers of the device is an important position for disposing the concave and convex light extraction structures, which precede all the processes in the fabrication of the device, the following examples 27 and 28 were provided (see tables 4 and 5).
Examples 27 and 28 were carried out under the production conditions shown in tables 4 and 5, and then a transparent electrode, a functional layer, and a reflective electrode were formed in this order on the other side of the glass, thereby finally completing the production of a bottom-emitting device.
Table 4:
table 5:
comparative example 1
After 150nm ITO (150W, Ar:48sccm) is subjected to radio frequency sputtering on 0.7mm glass (containing a mask plate convenient for electrode extraction), PEDOT (PSS (40nm, Heraeus E100), a toluene solution (30nm) of TFB, an octane solution (30nm) of green quantum dots (CdSe/CdS) and an ethanol solution (50nm) of ZnO are sequentially spin-coated, 100nm Ag is evaporated, and the bottom-emitting QLED device is obtained after packaging.
Comparative example 2
And performing radio frequency sputtering on 0.7mm glass (containing a mask plate convenient for electrode extraction) to obtain 100nm Ag (150W, Ar:48sccm) and 15nm ITO (150W, Ar:48sccm) in sequence, then performing spin coating on PEDOT, PSS (40nm, Heraeus E100), a toluene solution (30nm) of TFB, an octane solution (30nm) of green quantum dots (CdSe/CdS) and an ethanol solution (50nm) of ZnO, evaporating Ag with the thickness of 20nm, and packaging to obtain the top-emitting QLED device.
And (3) testing:
PR670(photo research) for light emitting devices of comparative examples 1 and 2 and examples 1 to 5 was set at 3mA/cm2The external quantum efficiency EQE of the device is tested under the current density (the detection result is shown in table 6), the lens is positioned right in front of the light emitting area of the device (the device is defined to be positioned at a zero angle at the moment), the included angle between the light emitting area of the device and the lens is adjusted to be 0-80 degrees by 10 degrees through rotating the platform (the light sheet and the lens are approximately a straight line when the angle is 90 degrees, the lens obviously cannot focus the light emitting area well, so the test cannot be carried out), the light emitting efficiency at different angles is tested, and the graph 1 is obtained after normalization processing.
Table 6:
| numbering | External quantum efficiency EQE (%) |
| Comparative example 1 | 8.8 |
| Comparative example 2 | 7.5 |
| Example 1 | 13.3 |
| Example 2 | 14.1 |
| Example 3 | 9.5 |
| Example 4 | 9.7 |
| Example 5 | 10.1 |
It can be seen from fig. 1 that, no matter the light extraction structure obtained by the preparation method of the present application is added to the bottom emission light-emitting device or the top emission light-emitting device, the efficiency decrease trend becomes slow along with the change of the angle, that is, the light extraction structure and the preparation method thereof of the present application not only can effectively improve the light-emitting effect of the device, but also can improve the light-emitting from different angles of the device, and reduce the angle dependence.
In the top emission light emitting device of embodiments 6 to 16, according to the difference of the position of the light extraction structure in the device, the concave or convex light extraction structure of the present application may be disposed between the substrate glass and the ITO anode layer, between the ITO anode and the hole injection layer, or between the electron transport layer and the reflective electrode layer.
In the bottom emission light emitting device of embodiments 17 to 26, according to the difference of the position of the light extraction structure in the device, the concave or convex light extraction structure of the present application may be disposed between the substrate glass and the reflective electrode layer, between the reflective electrode layer and the hole injection layer, or between the electron transport layer and the translucent electrode layer, and when the light extraction structure is disposed at these positions, the light extraction structure can directly improve the light extraction at different angles, thereby improving the uniformity of the light extraction.
In addition, in both the bottom emission light-emitting device and the top emission light-emitting device, the concave or convex light extraction structure may be provided between the hole injection layer and the hole transport layer, between the hole transport layer and the quantum dot light-emitting layer, and between the quantum dot light-emitting layer and the electron transport layer.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the membrane layer of the irregular porous structure is formed by the wet method on the substrate, or the irregular protruding light taking-out structure is further arranged by the irregular porous structure, so that the light taking-out structure not only contributes to improving the uniformity of the light emitting angle of the light emitting device, but also is beneficial to improving the light efficiency of the light emitting device.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (20)
1. A method of fabricating a light extraction structure, the method comprising:
providing a substrate;
wet-manufacturing a first film layer on the substrate by using a first solution, wherein the first solution comprises a material A and a solvent B;
drying the first membrane layer to form a first membrane layer with a porous structure, wherein at least part of the porous structure is directly communicated with the substrate, and after the step of forming the first membrane layer with the porous structure, the manufacturing method further comprises the following steps:
disposing a material C on the first membrane layer having a porous structure to form a second membrane layer, wherein a portion of the material C is disposed on the substrate through the porous structure; and
and removing the first film layer and the second film layer arranged on the surface of the first film layer, and reserving the material C on the substrate to form a protruding structure, wherein the protruding structure is the light extraction structure.
2. The method of claim 1, wherein a thickness of the first film layer is greater than a thickness of the second film layer, and the thickness of the first film layer is 10nm to 10 μm.
3. The method of claim 1, wherein the first film layer and the second film layer disposed on the surface of the first film layer are removed by solvent washing or tape stripping.
4. The method of claim 3, wherein the solvent rinsing is performed with a good solvent of the first film layer.
5. The method of any one of claims 1 to 4, wherein the substrate is a functional film layer, an electrode layer or a nonfunctional carrier.
6. The method according to claim 5, wherein the functional film layer is selected from any one of a hole injection layer, a hole transport layer, a light-emitting layer, an electron injection layer, an electron transport layer, a hole blocking layer, and an electron blocking layer.
7. The method of claim 5, wherein the non-functional carrier is a transparent substrate.
8. The manufacturing method according to any one of claims 1 to 4, wherein the solvent B comprises a first boiling point solvent, and the first boiling point solvent is selected from one or more organic solvents with a boiling point of 80 ℃ to 300 ℃.
9. The manufacturing method of claim 8, wherein the solvent B further comprises a second boiling point solvent, and the second boiling point solvent is selected from one or more organic solvents with boiling points of 60 ℃ to 120 ℃.
10. The method according to claim 9, wherein a volume ratio of the first boiling point solvent to the second boiling point solvent in the solvent B is 95:5 to 5: 95.
11. The method according to claim 8, wherein the first boiling point solvent has a melting point of 15 ℃ or higher.
12. The method of manufacturing of claim 1, wherein the material a is selected from one or more of the following materials: the nano silver ink comprises a high polymer material, oxide nanocrystals, nano silver wires, silver ink, inorganic particles, a photo-curing glue composition, a thermosetting glue composition and sol-gel.
13. The method according to claim 1, wherein the material A is one or more selected from polymer materials having a molecular weight of not less than 1000 and a glass transition temperature Tg≥80℃。
14. The method of manufacturing according to any one of claims 1 or 12, wherein the material C is selected from one or more of the following materials: metal oxides, nitrides, oxynitrides, fluorides, and metals.
15. A light extraction structure, characterized in that it is manufactured by the manufacturing method of any one of claims 1 to 14.
16. A bottom emission light emitting device, comprising a non-functional carrier, a semi-transparent electrode layer, a functional film layer and a reflective electrode layer sequentially arranged from bottom to top, wherein the functional film layer comprises a plurality of sub-functional film layers, the bottom emission light emitting device further comprises a light extraction structure, and the light extraction structure is located between any two adjacent layers of the non-functional carrier, the semi-transparent electrode layer, the functional film layer and the reflective electrode layer, or between any two adjacent sub-functional film layers of the functional film layer, or on a side surface of the non-functional carrier away from the semi-transparent electrode layer, wherein the light extraction structure is the light extraction structure of claim 15.
17. Bottom-emitting light-emitting device according to claim 16,
the light extraction structure is positioned between any two layers from the semitransparent electrode layer to the reflecting electrode layer, and the refractive index value of the light extraction structure is 1.5-2;
or the light extraction structure is positioned between the non-functional carrier and the semitransparent electrode layer, and the refractive index value of the light extraction structure is 1.5-1.8;
or the light extraction structure is positioned on the surface of one side, far away from the semi-transparent electrode layer, of the non-functional carrier, and the refractive index value of the light extraction structure is 1-1.5.
18. A top-emission light-emitting device comprising a non-functional carrier, a reflective electrode layer, a functional film layer, a semi-transparent electrode layer and an encapsulation layer, which are sequentially arranged from bottom to top, and a light extraction structure, wherein the functional film layer comprises a plurality of sub-functional film layers, and the light extraction structure is located between any two adjacent layers, wherein the light extraction structure is the light extraction structure of claim 15.
19. The top-emitting light-emitting device of claim 18, wherein the encapsulation layer is an encapsulation cover sheet or film.
20. The top-emitting light-emitting device according to claim 18, wherein the light extraction structure is located between any two adjacent layers from the translucent electrode layer to the reflective electrode layer, and the light extraction structure has a refractive index value of 1.5 to 2;
or the light extraction structure is positioned between the packaging layer and the semitransparent electrode, and the refractive index value of the light extraction structure is 1-1.8.
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