CN111146364B - Preparation method of micro-nano composite structure for improving light-emitting efficiency of light-emitting device - Google Patents
Preparation method of micro-nano composite structure for improving light-emitting efficiency of light-emitting device Download PDFInfo
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- CN111146364B CN111146364B CN202010070974.2A CN202010070974A CN111146364B CN 111146364 B CN111146364 B CN 111146364B CN 202010070974 A CN202010070974 A CN 202010070974A CN 111146364 B CN111146364 B CN 111146364B
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating
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Abstract
The invention relates to a method for preparing a micro-nano composite structure for improving the light-emitting efficiency of a light-emitting device, which comprises the following steps of firstly heating polymers and substrates with different thermal expansion coefficients to generate thermal expansion of different degrees; then filling an inorganic material in the holes in a layer on the surface of the polymer by using an atomic layer deposition method, wherein in the process of cooling, the polymer shrinks to cause a layer of bulges on the surface, and forming a micro-nano wrinkle pattern; and finally, the micro-nano composite structure is used for a light-emitting display device, so that the light propagation path of the light-emitting display device is changed, and the light-emitting efficiency of the device is improved.
Description
Technical Field
The invention relates to the field of photoelectric devices, in particular to a method for preparing a micro-nano composite structure for improving the light emitting efficiency of a light emitting device.
Background
For display and lighting devices, improving the light extraction efficiency of the device is a key factor affecting the performance of the device, and is receiving much attention from the scientific and industrial fields. In the transmission process of light generated inside the light-emitting device, due to the influence of the aspects of total reflection, interference effect and the like, the light is limited in an internal functional layer or a substrate, so that the light output efficiency of the light-emitting device is reduced, and meanwhile, a large amount of heat energy is accumulated inside the device, so that the service life of the device is greatly influenced.
To improve the coupling-out efficiency, allowing confined light to be emitted from the front side of the substrate, different light extraction techniques have been used. Light extraction techniques can be divided into two types of modification methods, internal and external, depending on the position of the modification layer.
Aiming at the problem of the light emitting efficiency of the existing display and lighting device, the invention provides a preparation method of a micro-nano composite structure for improving the light emitting efficiency of a light emitting device by utilizing the characteristic that an atomic layer deposition reactant can permeate into polymer holes under the pressure maintaining condition of a cavity and combining the characteristic that a micro-nano structure can be generated due to uneven stress distribution of a film layer, and the light emitting efficiency of the light emitting device is improved.
Disclosure of Invention
In view of this, the present invention provides a method for preparing a micro-nano composite structure for improving the light-emitting efficiency of a light-emitting device, which can improve the light-emitting efficiency of the light-emitting device.
The invention is realized by adopting the following scheme: a method for preparing a micro-nano composite structure for improving the light-emitting efficiency of a light-emitting device is disclosed, wherein the micro-nano composite structure is a multiple composite pattern structure, namely a multiple inorganic/organic fusion film layer;
the specific preparation process of the micro-nano composite structure comprises the following steps:
step S1: preparing a layer of patterned polymer with a thermal expansion coefficient different from that of the glass substrate on a cleaned glass sheet, curing the patterned polymer, placing the cured polymer in an atomic layer deposition reaction cavity, and vacuumizing the reaction cavity until 10 percent of the polymer is generated in the reaction cavity4Pa~10-4Pa negative pressure;
step S2: heating the reaction cavity to ensure that the polymer and the glass substrate expand by heating, wherein the thermal expansion degree of the polymer is higher than that of the glass substrate;
step S3: introducing a first reaction precursor into the atomic layer deposition reaction cavity, and maintaining the pressure for a certain time to ensure that the first reaction precursor effectively permeates into the polymer;
step S4: vacuumizing to a vacuum degree lower than 10-1Pa, discharging excessive first precursor, and introducing inert gas N2After washing for 5 minutes, introducing a second precursor, and maintaining the pressure for a certain time to ensure that the second precursor effectively permeates into the polymer and reacts with the first precursor to generate an inorganic filling material in a hole structure on one layer of the surface of the polymer;
step S5: inert gas N is introduced2Washing until the excessive second reaction precursor and the reaction residual product are discharged;
step S6: repeating the steps S3 to S5 for m periods to form a dense fusion film filled with inorganic materials on the surface of the polymer; when the temperature is reduced, the polymer and the fusion film are integrally shrunk to cause a layer of bulges on the surface, and a random wrinkle pattern with a nano structure is formed on the surface of the micron patterned polymer, so that the patterned polymer with the micro-nano composite structure is obtained;
step S7: and placing the micro-nano composite structure on the light emitting surface of the light emitting device coated with the refractive index matching liquid in advance, and curing the refractive index matching liquid to enable the micro-nano composite structure to be completely adhered with the light emitting surface so as to improve the light emitting efficiency of the device.
Further, the polymer includes PDMS (polydimethylsiloxane), PMMA (acryl), ABS (thermoplastic resin), EP (epoxy resin), PE (polyethylene), PS (polystyrene), PC (polycarbonate), PF (phenol resin), or PI (polyimide); the polymer has a coefficient of linear thermal expansion in the range of 10-200 x 10-6/deg.C and the substrate has a coefficient of linear thermal expansion in the range of 0.1-10 x 10-6/deg.C.
Further, m is greater than or equal to 1 in step S6, m is a natural number, and m is the number of cycles of atomic layer deposition.
Furthermore, the vacuum degree of the vacuum cavity in the reaction cavity is less than or equal to 10-1Pa, and the heating temperature range of the cavity is 50-300 ℃.
Further, the dwell time in steps S3 and S4 is 200 ms to 5 min, respectively, for regulating the pattern size by the dwell time.
Further, the inorganic material generated in step S4 includes Al2O3、TiO2、ZrO2、HfO2、Ta2O5ZnO or In2O3。
Further, the refractive index of the refractive index matching fluid described in step S7 ranges from 1.4 to 1.6.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention has simple process, can be prepared in large area, can be simply and conveniently applied to luminescent devices, and provides a new technology for manufacturing high-luminous-efficiency display and lighting devices.
(2) The fluctuation and the period of the random fold pattern can be regulated and controlled by the pressure maintaining time of the atomic layer deposition precursor; the amount of penetration of the inorganic material can be precisely controlled by the number of cycles of atomic layer deposition.
Drawings
Fig. 1 is a schematic diagram of a micro-nano composite structure according to an embodiment of the present invention, where 1 is a light emitting device, 2 is a patterned polymer, and 3 is an inorganic/organic fusion film layer on the surface of the patterned polymer.
FIG. 2 is a flow chart of a process of making an embodiment of the present invention.
Fig. 3 shows a random wrinkle pattern of a micro-nano composite structure obtained by an experiment according to an embodiment of the present invention.
Fig. 4 is a graph showing a relationship between a relative intensity of light emitted from the micro-nano composite structure and a light emitting angle obtained through an experiment according to an embodiment of the present invention, where the light emitting angle is an included angle between a viewing line and a central axis perpendicular to the light emitting surface.
Detailed Description
The invention is further explained below with reference to the drawings and the embodiments.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As shown in fig. 1, this embodiment further provides a method for preparing a micro-nano composite structure for improving the light extraction efficiency of a light emitting device, where the micro-nano composite structure is a multiple composite pattern structure, that is, a multiple inorganic/organic fusion film layer 3;
the specific preparation process of the micro-nano composite structure comprises the following steps:
step S1: preparing a layer of patterned polymer 2 with a thermal expansion coefficient different from that of the glass substrate on a cleaned glass sheet, curing the patterned polymer 2, placing the cured polymer in an atomic layer deposition reaction cavity, and vacuumizing the reaction cavity until 10 percent of the polymer 2 is generated in the body4Pa~10-4Pa negative pressure;
step S2: heating the reaction cavity to ensure that the polymer 2 and the glass substrate expand by heating, and the thermal expansion degree of the polymer 2 is higher than that of the glass substrate;
step S3: introducing a first reaction precursor into the atomic layer deposition reaction cavity, and maintaining the pressure for a certain time to ensure that the first reaction precursor effectively permeates into the polymer 2;
step S4: vacuumizing to a vacuum degree lower than 10-1Pa, discharging excessive first precursor, and introducing inert gas N2After washing for 5 minutes, introducing a second precursor, and maintaining the pressure for a certain time to ensure that the second precursor effectively permeates into the polymer 2 and chemically reacts with the first precursor to generate an inorganic filling material in a hole structure on a layer of the surface of the polymer 2;
step S5: inert gas N is introduced2Washing until the excessive second reaction precursor and the reaction residual product are discharged;
step S6: repeating the steps S3 to S5 for m cycles, and forming a dense fusion film 3 filled with inorganic materials on the surface of the polymer 2; when the temperature is reduced, the polymer substrate 2 and the fusion film 3 are integrally shrunk to cause a layer of bulges on the surface, and a random wrinkle pattern with a nano structure is formed on the surface of the micron patterned polymer, so that the patterned polymer with the micro-nano composite structure is obtained;
step S7: and placing the micro-nano composite structure on the light emitting surface of the light emitting device coated with the refractive index matching liquid in advance, and curing the refractive index matching liquid to enable the micro-nano composite structure to be completely adhered with the light emitting surface so as to improve the light emitting efficiency of the device.
In the present embodiment, the polymer includes PDMS (polydimethylsiloxane), PMMA (acryl), ABS (thermoplastic resin), EP (epoxy resin), PE (polyethylene), PS (polystyrene), PC (polycarbonate), PF (phenol resin), or PI (polyimide); the polymer has a linear thermal expansion coefficient in the range of 10-200X 10-6/DEG C, and the substrate has a linear thermal expansion coefficient in the range of 0.1-10X 10-6/℃。
In this embodiment, m is greater than or equal to 1 in step S6, m is a natural number, and m is the number of cycles of atomic layer deposition. In this embodiment, the degree of vacuum of the vacuum chamber in the reaction chamber is less than or equal to 10-1Pa, and the heating temperature of the chamber is 50-300 ℃.
In this embodiment, the dwell time ranges from 200 ms to 5 min in steps S3 and S4, respectively, so as to control the pattern size by the dwell time. The light emitting device has different light emitting efficiency due to the fact that the light emitting device has different size regulation and control of the patterns, the dwell time is different, the amount and the depth of inorganic materials penetrating into the polymer material are different, the fluctuation and the period change of the random fold patterns are from nanometer to micron.
In the present embodiment, the inorganic material generated in step S4 includes Al2O3、TiO2、ZrO2、HfO2、Ta2O5ZnO or In2O3。
In the present embodiment, the refractive index of the refractive index matching fluid described in step S7 is in the range of 1.4 to 1.6.
In this embodiment, the polymerization is a patterned surface with a micro pattern, and then a nano pattern is generated by atomic layer deposition to form a micro-nano composite structure.
Preferably, in order to make the present invention better understood by those skilled in the art, the following application examples are listed:
as shown in fig. 2, in the present embodiment,
step S1: coating a layer of PDMS101 with a thermal expansion coefficient different from that of the glass substrate on a cleaned glass sheet, heating and curing at 90 deg.C, placing the glass substrate and PDMS101 in a reaction chamber for atomic layer deposition, and vacuumizing the reaction chamber to 5 × 10-2Pa, maintaining the vacuum condition for 60 minutes, and exhausting the residual air in the substrate PDMS 101;
step S2: heating the reaction cavity to 90 ℃ to ensure that the substrate PDMS101 and the glass expand under heat, wherein the thermal expansion degree of the substrate PDMS101 is higher than that of the glass substrate;
step S3: introducing a first precursor TMA into the atomic layer deposition reaction cavity, and maintaining the pressure for 5 minutes to enable the first precursor TMA to effectively permeate into the substrate PDMS 101;
step S4: vacuumizing to a vacuum degree lower than 10-1Pa, discharging excessive first precursor TMA, and introducing inert gas N2After rinsing for 5 minutes, a second precursor H is introduced2O, maintaining the pressure for 5 minutes to ensure that the second precursor H2The O effectively permeates into the substrate PDMS101 and chemically reacts with the first precursor TMA to generate an inorganic filling material Al2O3 in the hole on the surface of the substrate PDMS 101;
step S5: inert gas N is introduced2Rinsing for 5 minutes to drain off excess second precursor H2O and residual products;
step S6: repeating the steps of 3-5100 cycles, forming a dense fusion film PDMS/Al2O 3102 filled with an inorganic material Al2O3 on the surface of the substrate PDMS101 at a certain depth, wherein the thickness of the fusion film PDMS/Al2O 3102 is about 10nm, and when the temperature is reduced, the substrate PDMS101 and the fusion film PDMS/Al2O 3102 shrink integrally to cause a layer of protrusion on the surface, so as to form a micro-nano structured random wrinkle pattern 103; as shown in fig. 3, after the reaction is finished, randomly distributed wrinkle patterns with an undulation height of 1 micron and a period of 2.5 microns are generated on the upper surface of the substrate PDMS 101;
step S7: tearing the substrate PDMS101 from the glass substrate, placing the substrate PDMS on the light emitting surface of the light emitting device 104 coated with the refractive index matching liquid PDMS in advance, curing the refractive index matching liquid PDMS to enable the micro-nano composite structure to be completely adhered to the light emitting surface, wherein the light emitting surface of the light emitting device 104 is the upper surface of the substrate PDMS101, light passes through the substrate PDMS101 and is emitted through the random wrinkle patterns 103 of the micro-nano structure, as shown in fig. 4, after the light emitting device is adhered to the micro-nano composite structure, the relative intensity of light emitting at different light emitting angles is improved.
According to the technical process, the micro-nano composite structure for improving the light emitting efficiency of the light emitting device is prepared, and a basic process is laid for obtaining the display and lighting device with stable long service life and high light efficiency.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of a micro-nano composite structure for improving the light extraction efficiency of a light-emitting device is characterized by comprising the following steps: the micro-nano composite structure is a multiple composite pattern structure, namely a multiple inorganic/organic fusion film layer;
the specific preparation process of the micro-nano composite structure comprises the following steps:
step S1: preparing a layer of patterned polymer with a thermal expansion coefficient different from that of the glass substrate on a cleaned glass sheet, curing the patterned polymer, placing the cured polymer in an atomic layer deposition reaction cavity, and vacuumizing the reaction cavity until 10 percent of the polymer is generated in the reaction cavity4Pa~10-4Pa negative pressure;
step S2: heating the reaction cavity to ensure that the polymer and the glass substrate expand by heating, wherein the thermal expansion degree of the polymer is higher than that of the glass substrate;
step S3: introducing a first reaction precursor into the atomic layer deposition reaction cavity, and maintaining the pressure for a certain time to ensure that the first reaction precursor effectively permeates into the polymer;
step S4: vacuumizing to a vacuum degree lower than 10-1Pa, discharging excessive first reaction precursor, and introducing inert gas N2After washing for 5 minutes, introducing a second reaction precursor, and maintaining the pressure for a certain time to ensure that the second reaction precursor effectively permeates into the polymer and reacts with the first reaction precursor to generate an inorganic filling material in a hole structure on a layer of the surface of the polymer;
step S5: inert gas N is introduced2Washing until the excessive second reaction precursor and the reaction residual product are discharged;
step S6: repeating the steps S3 to S5 for m periods to form a dense fusion film filled with inorganic materials on the surface of the polymer; when the temperature is reduced, the polymer and the fusion film are integrally shrunk to cause a layer of bulges on the surface, and a random wrinkle pattern with a nano structure is formed on the surface of the micron patterned polymer, so that the patterned polymer with the micro-nano composite structure is obtained;
step S7: and placing the micro-nano composite structure on the light emitting surface of the light emitting device coated with the refractive index matching liquid in advance, and curing the refractive index matching liquid to enable the micro-nano composite structure to be completely adhered with the light emitting surface so as to improve the light emitting efficiency of the device.
2. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: the polymer comprises PDMS, PMMA, ABS, EP, PE, PS, PC, PF or PI; the linear thermal expansion coefficient of the polymer is in the range of 10 x 10-6/℃-200 ×10-6A linear thermal expansion coefficient of the substrate in a range of 0.1 x 10/° C-6/℃-10 × 10-6/℃。
3. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: in the step S6, m is more than or equal to 1, m is a natural number, and m is the cycle number of atomic layer deposition.
4. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: the vacuum degree of the vacuum pumping cavity in the pair of reaction cavities is less than or equal to 10-1Pa, the heating temperature of the cavity is 50-300 ℃.
5. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: the dwell time in steps S3 and S4 is 200 ms to 5 min, respectively, to control the pattern size by the dwell time.
6. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: the inorganic material generated in step S4 includes Al2O3、TiO2、ZrO2、HfO2、Ta2O5ZnO or In2O3。
7. The preparation method of the micro-nano composite structure for improving the light extraction efficiency of the light-emitting device according to claim 1, wherein the preparation method comprises the following steps: the refractive index of the refractive index matching fluid described in step S7 ranges from 1.4 to 1.6.
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