CN113354762A - Photocurable formed scattering medium, photoelectric device and preparation method thereof - Google Patents

Photocurable formed scattering medium, photoelectric device and preparation method thereof Download PDF

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CN113354762A
CN113354762A CN202110537197.2A CN202110537197A CN113354762A CN 113354762 A CN113354762 A CN 113354762A CN 202110537197 A CN202110537197 A CN 202110537197A CN 113354762 A CN113354762 A CN 113354762A
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scattering medium
photoelectric device
nanocrystalline particles
treating agent
light
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宋世超
曹耀宇
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Jinan University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F122/00Homopolymers of compounds having one or more unsaturated aliphatic radicals each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides or nitriles thereof
    • C08F122/10Esters
    • C08F122/1006Esters of polyhydric alcohols or polyhydric phenols, e.g. ethylene glycol dimethacrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/46Polymerisation initiated by wave energy or particle radiation
    • C08F2/48Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • HELECTRICITY
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    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract

The invention belongs to the technical field of photoelectric devices, and discloses a light-curable formed scattering medium, a photoelectric device and a preparation method thereof. The scattering medium includes: nanocrystalline particles, a treating agent and a light-curing material; the treating agent is selected from a surfactant and/or a coupling agent. The scattering medium can be directly formed into a planar or stereoscopic photoelectric device through photocuring, and the design and manufacturing process difficulty of the photoelectric device is greatly reduced.

Description

Photocurable formed scattering medium, photoelectric device and preparation method thereof
Technical Field
The invention belongs to the technical field of photoelectric devices, and particularly relates to a light-curable formed scattering medium, a photoelectric device and a preparation method thereof.
Background
Speckle phenomena arise when transmitting light through a scattering body or space with suspended particles, which results from scattering by the scattering medium. The scattering is a phenomenon that light is affected by molecules or atoms in a propagation medium to change the spatial distribution, polarization state or frequency of the light intensity when the light propagates, and the principle of the scattering is widely applied to the fields of optical imaging and optical communication, such as adaptive optical imaging technology, optical coherence tomography imaging technology, "ghost" imaging technology, time reversal imaging technology, wavelength division multiplexing and demodulation technology, and the like.
At present, the scattering medium is generally prepared by spin-coating an aqueous dispersion of zinc oxide and titanium dioxide particles on the surface of an object and drying the aqueous dispersion, however, the method can only form a thin-film type scattering medium, and if a photoelectric device is formed by further patterning, post-treatment needs to be performed by processing methods such as etching and the like, so that the manufacturing complexity of the photoelectric device is increased, the alignment precision is influenced, and the reliability of the photoelectric device is further reduced.
It is therefore desirable to provide a scattering medium with improved processability, thereby producing optoelectronic devices with improved reliability.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a light-curable formed scattering medium, a photoelectric device and a preparation method thereof. The scattering medium can be directly formed into a planar or stereoscopic photoelectric device through photocuring, and the design and manufacturing process difficulty of the photoelectric device is greatly reduced.
The present invention provides a scattering medium comprising: nanocrystalline particles, a treating agent and a light-curing material; the treating agent is selected from a surfactant and/or a coupling agent. The invention adopts the treating agent to coat the nanocrystalline particles for modification, and the modified nanocrystalline particles are dispersed in the light-cured material. The proportion of the nanocrystalline particles in the scattering medium can be regulated and controlled according to requirements.
Preferably, the coating thickness of the treating agent to the nanocrystalline particles is 0.1-10 nm.
Preferably, the nanocrystalline particles are selected from at least one of silicon oxide, titanium oxide, aluminum oxide, iron oxide, tungsten oxide, vanadium oxide, indium tin oxide, silicon nitride, magnesium fluoride, or zinc selenide.
Preferably, the grain size of the nanocrystalline grains is 1-500 nm.
More preferably, the nanocrystalline particles have a particle size of 1-200 nm.
Preferably, the treating agent is selected from at least one of an ionic surfactant, a non-ionic surfactant, a silane coupling agent, a titanate coupling agent, or an aluminate coupling agent.
Preferably, the light-curable material includes a photosensitive polymer material.
More preferably, the light-curable material further includes at least one of a photoinitiator, a photosensitizer, or a polymerization inhibitor.
The photo-curing material can perform photochemical reaction under the action of an optical field, such as photopolymerization to form a high polymer. From the photochemical analysis, it is found that the polymerized high polymer has a network skeleton structure and can provide certain mechanical properties.
The invention also provides a preparation method of the scattering medium, which comprises the following steps:
(1) mixing a treating agent with the nanocrystalline particles for surface modification to obtain surface-modified nanocrystalline particles;
(2) and (2) dispersing the surface-modified nanocrystalline particles prepared in the step (1) in a photocuring material to obtain the scattering medium.
The invention also provides a preparation method of the photoelectric device, which comprises the following steps:
(1) manufacturing a substrate containing a control circuit;
(2) coating the scattering medium on the surface of the substrate;
(3) and carrying out photocuring one-step molding on the scattering medium to obtain the photoelectric device.
Preferably, the substrate in step (1) is selected from a quartz substrate, a borosilicate substrate, a titanium dioxide substrate, a sapphire substrate, a transparent conductive oxide glass substrate or a silicon substrate.
Preferably, the coating in step (2) is performed by coating, spin coating or casting.
Preferably, the optoelectronic device in step (3) is a planar type optoelectronic device or a stereoscopic type optoelectronic device.
The invention also provides a photoelectric device prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, after the nano-crystalline particles are modified by the treating agent, the nano-crystalline particles are dispersed in the light-cured material to construct a scattering medium system, and the plasticity of the light-cured material is utilized to realize the manufacturing of a planar or stereoscopic photoelectric device based on a scattering medium, so that the difficulty in the design and manufacturing process of the photoelectric device is greatly reduced, and the manufactured photoelectric device has good photoelectric response characteristics and is easy to realize the regulation and control of the light field scattering performance.
Drawings
FIG. 1 is a schematic diagram of a photovoltaic device;
FIG. 2 is a schematic diagram of a three-dimensional stacked photovoltaic device;
FIG. 3 is a schematic diagram of a three-dimensional hemispherical optoelectronic device;
FIG. 4 is a graph of scattering characteristics of a three-dimensional hemispherical optoelectronic device versus device size;
FIG. 5 is a graph of scattering characteristics of a three-dimensional hemispherical photoelectric device as a function of nanocrystal specific gravity concentration.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are only preferred embodiments of the present invention, and the claimed protection scope is not limited thereto, and any modification, substitution, combination made without departing from the spirit and principle of the present invention are included in the protection scope of the present invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
The present embodiment provides a scattering medium, including: nanocrystalline particles, a treating agent and a light-curing material; the treating agent is used for coating and modifying the nanocrystalline particles, and the modified nanocrystalline particles are dispersed in the light-cured material.
Wherein the nanocrystalline particles are titanium dioxide nanocrystalline, the particle size of the nanocrystalline particles is 5nm, and the mass fraction of the nanocrystalline particles in the scattering medium is 30%; the treating agent is a silane coupling agent KH-570, and the coating thickness of the silane coupling agent KH-570 on the titanium dioxide nanocrystal is 0.5 nm; the light-cured material comprises pentaerythritol tetraacrylate (PETTA) and Isopropyl Thioxanthone (ITX), and the specific gravity of the PETTA and the ITX is 97: 3.
The preparation method of the scattering medium comprises the following steps:
(1) mixing a treating agent with the nanocrystalline particles for surface modification to obtain surface-modified nanocrystalline particles;
(2) and (2) dispersing the surface-modified nanocrystalline particles prepared in the step (1) in a photocuring material to obtain a scattering medium.
Example 2
The present embodiment provides a scattering medium, including: nanocrystalline particles, a treating agent and a light-curing material; the treating agent is used for coating and modifying the nanocrystalline particles, and the modified nanocrystalline particles are dispersed in the light-cured material.
Wherein the nanocrystalline particles are titanium dioxide nanocrystalline, the particle size of the nanocrystalline particles is 5nm, and the mass fraction of the nanocrystalline particles in the scattering medium is 0%, 10%, 20% or 30%; the treating agent is a silane coupling agent KH-570, and the coating thickness of the silane coupling agent KH-570 on the titanium dioxide nanocrystal is 0.3 nm; the light curing material comprises pentaerythritol tetraacrylate (PETTA) and Irgacure-369 (photoinitiator, available from Pasteur), wherein the specific gravity of the PETTA and the Irgacure-369 is 98: 2.
The preparation method of the scattering medium comprises the following steps:
(1) mixing a treating agent with the nanocrystalline particles for surface modification to obtain surface-modified nanocrystalline particles;
(2) and (2) dispersing the surface-modified nanocrystalline particles prepared in the step (1) in a photocuring material to obtain a scattering medium.
Example 3
The embodiment provides a planar photoelectric device, and a preparation method thereof comprises the following steps:
(1) preparing a substrate comprising a control circuit on a silicon chip by using a standard CMOS (complementary metal oxide semiconductor) process to serve as a supporting platform of a photoelectric device;
(2) coating the scattering medium prepared in example 1 on the surface of a substrate to be combined with the substrate;
(3) adopting ultraviolet light source with wavelength of 390nm at 1000mJ/cm2The light power of the light source is used for carrying out photocuring one-step molding on the scattering medium, and interconnection electrode manufacturing is carried out through a micro-nano processing method, so that the planar photoelectric device is manufactured.
Fig. 1 is a schematic structural diagram of the prepared photoelectric device, wherein the substrate 00, the organic polymer material 11, the treating agent 22, and the nanocrystalline particles 33 are provided.
Example 4
The embodiment provides a stereoscopic photoelectric device, and a preparation method thereof comprises the following steps:
(1) preparing a substrate comprising a control circuit on a silicon chip by using a standard CMOS (complementary metal oxide semiconductor) process to serve as a supporting platform of a photoelectric device;
(2) coating the scattering medium prepared in example 1 on the surface of a substrate to be combined with the substrate;
(3) adopting femtosecond laser with wavelength of 532nm, carrying out photocuring one-step molding on the scattering medium under the parameter conditions of pulse width 220fs, repetition frequency 80MHz, optical power 1.0mW and scanning speed of 200 mu m/s, and carrying out interconnection electrode manufacturing by a micro-nano processing method to obtain the three-dimensional photoelectric device (three-dimensional stacked type).
Fig. 1 is a schematic structural diagram of the prepared photoelectric device, wherein a substrate 00, an organic polymer material 11, a treating agent 22, and nanocrystalline particles 33; fig. 2 is a schematic structural diagram of a three-dimensional photoelectric device (three-dimensional stacked) manufactured in this embodiment.
Example 5
The embodiment provides a stereoscopic photoelectric device, and a preparation method thereof comprises the following steps:
(1) preparing a substrate comprising a control circuit on a silicon chip by using a standard CMOS (complementary metal oxide semiconductor) process to serve as a supporting platform of a photoelectric device;
(2) coating the scattering medium prepared in example 1 on the surface of a substrate to be combined with the substrate;
(3) adopting femtosecond laser with the wavelength of 532nm, carrying out photocuring one-step molding on the scattering medium under the parameter conditions of the pulse width of 220fs, the repetition frequency of 80MHz, the optical power of 1.0mW and the scanning speed of 200 mu m/s, and manufacturing an interconnection electrode by a micro-nano processing method to prepare the three-dimensional photoelectric device with the size of 1-3 mu m.
Fig. 1 is a schematic structural diagram of the prepared photoelectric device, wherein a substrate 00, an organic polymer material 11, a treating agent 22, and nanocrystalline particles 33; FIG. 3 is a schematic structural diagram of a three-dimensional photoelectric device (three-dimensional hemispherical) manufactured in this embodiment; as shown in FIG. 4, when the size of the prepared photoelectric device is increased from 1 μm to 3 μm, the scattering peak position is shifted from 745 nm red to 780 nm, and the scattering intensity is significantly enhanced.
Example 6
The embodiment provides a stereoscopic photoelectric device, and a preparation method thereof comprises the following steps:
(1) preparing a substrate comprising a control circuit on indium tin oxide glass by using a standard CMOS (complementary metal oxide semiconductor) process to serve as a supporting platform of a photoelectric device;
(2) coating the scattering medium prepared in example 2 on the surface of a substrate to be combined with the substrate;
(3) adopting femtosecond laser with the wavelength of 532nm, carrying out photocuring one-step molding on the scattering medium under the parameter conditions of the pulse width of 220fs, the repetition frequency of 80MHz, the optical power of 1.0mW and the scanning speed of 200 mu m/s, and carrying out interconnection electrode manufacturing by a micro-nano processing method to prepare the three-dimensional photoelectric device with the titanium dioxide nanocrystal specific weight concentration of 10-30%.
Fig. 1 is a schematic structural diagram of the prepared photoelectric device, wherein a substrate 00, an organic polymer material 11, a treating agent 22, and nanocrystalline particles 33; FIG. 3 is a schematic structural diagram of a three-dimensional photoelectric device (three-dimensional hemispherical) manufactured in this embodiment; as shown in FIG. 5, when the specific gravity concentration of the nanocrystalline particles in the photoelectric device is increased from 10% to 30%, the scattering peak position is shifted from 747 nanometer red to 780 nanometer, and the scattering intensity is obviously enhanced.

Claims (10)

1. A scattering medium, comprising: nanocrystalline particles, a treating agent and a light-curing material; the treating agent is selected from a surfactant and/or a coupling agent.
2. The scattering medium of claim 1, wherein the nanocrystalline particles are selected from at least one of silicon oxide, titanium oxide, aluminum oxide, iron oxide, tungsten oxide, vanadium oxide, indium tin oxide, silicon nitride, magnesium fluoride, or zinc selenide.
3. The scattering medium of claim 1, wherein the nanocrystalline particles have a particle size of 1-500 nm; preferably, the grain diameter of the nanocrystalline grains is 1-200 nm.
4. The scattering medium of claim 1, wherein the treating agent is selected from at least one of an ionic surfactant, a non-ionic surfactant, a silane coupling agent, a titanate coupling agent, or an aluminate coupling agent.
5. The scattering medium of claim 1, wherein the light curable material comprises a photosensitive polymeric material.
6. The scattering medium of claim 5, wherein the light-curable material further comprises at least one of a photoinitiator, a photosensitizer, or a polymerization inhibitor.
7. The method for producing a scattering medium as claimed in any of claims 1 to 6, characterized in that it comprises the following steps:
(1) mixing a treating agent with the nanocrystalline particles for surface modification to obtain surface-modified nanocrystalline particles;
(2) and (2) dispersing the surface-modified nanocrystalline particles prepared in the step (1) in a photocuring material to obtain the scattering medium.
8. A method for manufacturing a photoelectric device, comprising the steps of:
(1) manufacturing a substrate containing a control circuit;
(2) coating the scattering medium of any of claims 1-6 on the substrate surface;
(3) and carrying out photocuring one-step molding on the scattering medium to obtain the photoelectric device.
9. The production method according to claim 8, wherein the photoelectric device in the step (3) is a planar type photoelectric device or a stereoscopic type photoelectric device.
10. An opto-electronic device characterized by being produced by the production method according to claim 8 or 9.
CN202110537197.2A 2021-05-18 2021-05-18 Photocurable formed scattering medium, photoelectric device and preparation method thereof Pending CN113354762A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115232267A (en) * 2022-07-27 2022-10-25 吉林大学 Polymer/nanocrystal hybrid light guide plate and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020106884A1 (en) * 2018-11-20 2020-05-28 Pixelligent Technologies Llc Solvent-free formulations and nanocomposites

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020106884A1 (en) * 2018-11-20 2020-05-28 Pixelligent Technologies Llc Solvent-free formulations and nanocomposites

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
辛智青 等: "《印刷制造原理与技术》", 30 June 2019, 文化发展出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115232267A (en) * 2022-07-27 2022-10-25 吉林大学 Polymer/nanocrystal hybrid light guide plate and preparation method thereof
CN115232267B (en) * 2022-07-27 2023-12-08 吉林大学 Polymer/nanocrystalline hybrid light guide plate and preparation method thereof

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Application publication date: 20210907