WO2011032356A1 - 一种光转换柔性高分子材料及其用途 - Google Patents

一种光转换柔性高分子材料及其用途 Download PDF

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WO2011032356A1
WO2011032356A1 PCT/CN2010/001413 CN2010001413W WO2011032356A1 WO 2011032356 A1 WO2011032356 A1 WO 2011032356A1 CN 2010001413 W CN2010001413 W CN 2010001413W WO 2011032356 A1 WO2011032356 A1 WO 2011032356A1
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light
fluorescent material
polymer material
flexible polymer
silicone oil
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PCT/CN2010/001413
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English (en)
French (fr)
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肖志国
常英
隋玉龙
吴粤宁
李茂龙
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大连路明发光科技股份有限公司
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Priority to KR1020127009143A priority Critical patent/KR101397204B1/ko
Priority to EP20100816560 priority patent/EP2479220A4/en
Priority to US13/496,548 priority patent/US9068077B2/en
Priority to JP2012529092A priority patent/JP2013504668A/ja
Publication of WO2011032356A1 publication Critical patent/WO2011032356A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
    • F21V9/40—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters with provision for controlling spectral properties, e.g. colour, or intensity
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • 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
    • H01L33/48—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 semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • 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
    • H01L33/48—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 semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/505—Wavelength conversion elements characterised by the shape, e.g. plate or foil

Definitions

  • the invention relates to the field of optoelectronic display and illumination technology, and more particularly to a polymer material doped with a fluorescent material, a preparation method thereof and a use thereof, in particular to a light-emitting device for LED backlight, digital display and illumination Light conversion flexible polymer material, its preparation method and use. Background technique
  • the current LED backlights, digital display and illumination devices are usually obtained by encapsulating fluorescent materials.
  • Such patents have also been widely used as Chinese patents 200510030192. 1 "White light-emitting elements and their manufacturing methods", Chinese patent 200310120736 Mounted white light-emitting diodes>, Chinese patent 200710151099. 5 ⁇ Blue-violet or blue-light-excited phosphors and manufacturing methods and packaged white light diodes> are all mixed with fluorescent materials and coated on LED chips to form white light-emitting devices.
  • the white light-emitting device prepared by the method is difficult to ensure the consistency of brightness, color coordinates, color temperature and color rendering, and since the phosphor is close to the chip, it is easily affected by heat and causes aging, and the life is lowered.
  • International Patent WO2007105853 describes a method for preparing a photoluminescence film, which uses a luminescent material which is an inorganic luminescent material.
  • the photoluminescence film described in this patent is prepared by using a silicone resin as a film-forming material, but is not photo-induced.
  • the relationship between the luminescent material of the luminescent film and the color coordinates, color temperature, and brightness is introduced, and at the same time, it is not cast molding, and various shapes cannot be formed.
  • International Patent WO2007/049187 describes a sealing film agent for silicone-doped phosphor, which is mounted on a blue LED to achieve the purpose of converting blue light into white light, but the material itself is a film structure.
  • US patent US2008/0280957 Al describes a method for fabricating an LED using a plastic device having a lens structure.
  • the plastic device having a lens structure is a structure containing a layer of a fluorescent material, and is formed by die casting or injection molding, and the structure and process are complicated. The shape cannot be changed after molding.
  • the present invention adopts silicone rubber as a molding material, and adds a diluent, a fluorescent material, and an auxiliary agent to be mixed and then solidified by heating in a form of casting.
  • molds of various shapes can be designed.
  • the mold can be designed into a structure with a lens form for casting.
  • the molded polymer material is soft and elastic, has a certain strength, can be bent and deformed at will, and can be assembled in the device as needed.
  • the invention provides a light-converting flexible polymer material, and the mass percentage composition of the material is as follows:
  • Silicone rubber 20 0% ⁇ 75. 0%
  • Fluorescent material 15. 0% ⁇ 65. 0% 0. 0% ⁇ 5. 0%
  • the silicone rubber is a two-component addition molding vulcanization liquid silicone rubber
  • the diluent is sulfhydryl silicone oil, dimethicone, ethyl silicone oil, phenyl silicone oil, mercapto ethoxy silicone oil or hydrazine a vinyl silicone oil
  • the auxiliary agent is a leveling agent, an antifoaming agent, a coupling agent or a wetting and dispersing aid or a combination thereof;
  • the fluorescent material is a combination of one or both of an aluminate fluorescent material, a silicate fluorescent material, a silicon nitride fluorescent material, and a sulfur oxide fluorescent material; the emission spectrum of the fluorescent material used as an excitation light source is 440 ⁇
  • the blue LED in the 475nm excitation excites at least one emission spectrum with a peak wavelength in the range of 525 ⁇ 650nm; the light emitted by the fluorescent material is combined with the light emitted by the blue LED to form white or other color light.
  • the particle diameter of the fluorescent material to be used is preferably from 3 to 15 ⁇ m.
  • the light-converting flexible polymer material of the invention has various uses and can be used in light source devices such as lamps, digital tubes or backlights.
  • the light-converting flexible polymer material prepared by the present invention can effectively avoid the problems in the prior art.
  • the material is soft, has certain strength and toughness, and can be designed into various shapes of molds for casting according to the use condition, and the light-transferred flexible polymer material after molding is dispersed in the fluorescent material.
  • the light-emitting device prepared by the material has uniform light color, and since the material is not in close contact with the chip structure in use, the aging problem caused by heat is avoided, and the life of the product can be effectively improved. detailed description
  • the light-converting flexible polymer material of the invention is composed of a silicone rubber, a diluent, a fluorescent material and an auxiliary agent, and the composition components and the mass percentage components are as follows: Silicone rubber 20.0-75.0 Thinner 10.0-20
  • the fluorescent material is excited by a blue LED having an emission spectrum of the excitation source in the range of 440 to 475 nm, and the absorption excites at least one emission spectrum having a peak wavelength in the range of 525 to 650 nm;
  • the light emitted by the fluorescent material is combined with the light emitted by the blue LED to form white light or other color light.
  • the fluorescent material may be an aluminate fluorescent material, a silicate fluorescent material, a silicon nitride fluorescent material, and a sulfur oxide fluorescent material. One or a combination of several.
  • the main chemical composition of the aluminate fluorescent material is expressed as:
  • 11 is a combination of one or more elements of ⁇ , Tb, Gd;
  • R' is one of Al, Ga or a combination of two elements
  • a, x, y, z are molar coefficients, 0.45 ⁇ a ⁇ 0.65; 0.0 ⁇ x ⁇ 0.04; 0.0 ⁇ y ⁇ 0.04; 0.0 ⁇ z ⁇ 0.2; the emission main peak wavelength of the material varies with the composition in the range of 525 ⁇ 560nm ;
  • the main chemical composition of the silicate fluorescent material is expressed as:
  • Si0 2 xEu, yLi, zF;
  • M is a combination of one or more of Sr, Ca, Ba, Mg;
  • b, x, y, z are molar coefficients, 1.4 ⁇ b ⁇ 3.1; 0.015 ⁇ x ⁇ 0.1; 0.0 ⁇ y ⁇ 0.05; 0.0 ⁇ z ⁇ 0.25; the emission main peak wavelength of the material varies with the composition in the range of 525 - 580nm .
  • the main chemical composition of the silicon nitride fluorescent material is expressed as:
  • e, x, y, z are molar coefficients, 0.1 ⁇ e ⁇ l; 0.01 ⁇ x ⁇ 0.1;0.0 ⁇ y ⁇ 0.1; 0.0 ⁇ z ⁇ 0. 5;
  • the main peak wavelength of the material varies with the composition in the range of 580 ⁇ 650nm;
  • the main chemical composition of the sulfur oxide fluorescent material is expressed as:
  • Y 2 -x0 2 S Eux, Mgy, Tiz, Li ⁇ , Fy;
  • x, y, z, ⁇ , Y are molar coefficients, 0.01 ⁇ x ⁇ 0.1; 0.005 ⁇ y ⁇ 0.02; 0.05 ⁇ z ⁇ 0.25; 0.0 ⁇ ⁇ ⁇ 0.1; 0.0 ⁇ ⁇ ⁇ 0.5; the main peak wavelength of the material
  • the composition varies from 610 to 630 nm.
  • the particle size of the fluorescent material is preferably 3-15 microns, and the prepared fluorescent material is dispersed and has a good luminescent effect.
  • the fluorescent material can be excited by light emitted by ultraviolet or blue LEDs and combined with residual ultraviolet or blue light to form white light or other various colors of light.
  • the various fluorescent materials have different characteristics of body color and luminescent color, and can be selected according to different conditions in the manufacture of flexible polymer materials of fluorescent materials. Select silicate, aluminate luminescent fluorescent material as orange, yellow luminescent fluorescent material, select silicon nitride, sulphur oxide luminescent fluorescent material as red luminescent fluorescent material, yellow luminescent fluorescent material, orange luminescent fluorescent material and red luminescent
  • the composite material of fluorescent materials is used in combination, and the color coordinate, color temperature and color rendering index can be adjusted to achieve the purpose of being suitable for various purposes.
  • the fluorescent material emitting yellow light is used in combination with the fluorescent material emitting red light to improve the color rendering index.
  • the high color rendering index of white light makes it suitable for use in light-emitting devices that require a high color rendering index.
  • the light-converting flexible polymer material is combined with an LED to synthesize white light or other color light, and is used in a light source device of a lamp, a digital tube, or a backlight.
  • the silicone rubber used is a two-component addition-heating vulcanized liquid silicone rubber which is transparent, soft and elastic.
  • This resin has thermal oxidative stability. Good, excellent electrical insulation properties, excellent resistance to Zhejiang, waterproof, Anti-rust, cold, ozone and weather resistance.
  • the resin does not yellow when it is used for a long time under high temperature, and has the characteristics of softness and elasticity after curing, and has a certain strength, can be bent and deformed at will, and is suitable for use in irregularly shaped devices.
  • the diluent is one of a mercapto silicone oil, a dimercapto silicone oil, an ethyl silicone oil, a phenyl silicone oil, a mercaptoethoxy silicone oil or a mercapto vinyl silicone oil.
  • the adjuvant may be a combination of one or more of a leveling agent, an antifoaming agent, a coupling agent, and a wetting and dispersing aid.
  • the silicone resin, the diluent, the fluorescent material, and the auxiliary agent are all mixed and formed by heating in a cast form.
  • the material can be used in luminaires, digital tubes, backlights, etc., and can be directly fixed on the blue light source after casting according to the shape required by the device.
  • the material can also be bent and deformed according to the shape of the device after molding.
  • Casting is a method of processing organic polymer materials.
  • a liquid monomer or polymer was injected into a mold under normal pressure, and solidified by polymerization to form a product having the same shape as that of the mold cavity.
  • the traditional casting concept has changed, and polymer solutions, dispersions and melts can also be used for casting.
  • the fluorescent material is an inorganic material
  • the material is easily blackened and loses luminescent properties during the rubbing with the metallic material, and therefore, it is necessary to avoid contact with the metallic material during manufacturing and processing.
  • the use of a casting process can effectively avoid the drawbacks of conventional polymer materials that are blackened or lose luminescent properties caused by extrusion or friction during material fabrication and processing.
  • the silicone rubber, the diluent, the fluorescent material and the auxiliary agent are uniformly mixed and injected into the mold, and are solidified by heating polymerization to form a product having the same shape as the cavity of the mold.
  • the casting method can change the traditional LED packaging process, greatly reduce the process steps, and its production efficiency is high, production automation is easy, and the operation loop is improved.
  • the luminescent fluorescent material is uniformly dispersed in the polymer resin, and the illuminating device made of the luminescent device has greatly improved uniformity of light emission, good light conversion effect, and flexible product.
  • the light-transforming flexible polymer material can be cast into a suitable shape according to the actual use, such as casting a shape with a lens structure, which can effectively improve the efficiency of light conversion and simultaneously achieve secondary light distribution design and enhance light output.
  • Efficiency optimized optical distribution.
  • the installation, maintenance and replacement of the light-emitting device prepared in this way is very convenient, simplifies the construction process, and the produced product is more flexible and diverse.
  • the material of the present invention is excellent in flexibility and strength, the material can be bent and folded at will, and is particularly suitable for the preparation of special light-emitting devices having irregular shapes.
  • Another aspect of the present invention is that the material is formed by a casting method. Since the fluorescent material is an inorganic material, the material is easily blackened and loses luminescent properties in the process of rubbing with the metal material, when using, for example, injection molding. When molding, the fluorescent material may become black due to friction and extrusion, and the luminescent property may be degraded. This method can be effectively avoided by using a casting method.
  • Example 1 The light-converting flexible polymer material of the present invention will be exemplified below by way of specific examples.
  • Example 1 The light-converting flexible polymer material of the present invention will be exemplified below by way of specific examples.
  • Example 1 The light-converting flexible polymer material of the present invention will be exemplified below by way of specific examples.
  • the casting formula is as follows:
  • Fluorescent material (aluminate yellow)
  • the silicone rubber is a two-component addition-heating vulcanized liquid silicone rubber.
  • Implementation process Add the liquid raw material in the formula into the ingredient container, stir evenly, add the fluorescent material under stirring, stir and hook and perform vacuum defoaming treatment. The liquid raw material mixture is added to the mold and placed in an oven for curing for 2 minutes. After curing, the formed light-converting flexible polymer material is taken out from the mold.
  • the prepared light-converting flexible polymer material can be applied to the surface of the blue LED.
  • the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED and combined with the remaining blue light to form white light.
  • the casting formula is as follows:
  • Silicone rubber 20 0% Thinner Dimethicone 10. 0% Auxiliary Wetting agent 2. 0%
  • Coupling agent 2 0% defoamer 1. 0% silicate green fluorescent material
  • the silicone rubber is a two-component addition molding and vulcanization liquid silicone rubber.
  • Implementation process Add the liquid raw material in the formula into the ingredient container, stir evenly, add the fluorescent material under stirring, stir and hook and perform vacuum defoaming treatment. The liquid raw material mixture is added to the mold, and is solidified in a 140 ⁇ oven for 3 mii. After curing, the formed light-converting flexible polymer material is taken out from the mold.
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED, and the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED and combined with the remaining blue light to form white light.
  • Example 3
  • the casting formula is as follows:
  • Silicone rubber 75 0% Thinner Ethylene silicone oil 9. 0% Additives Defoamer 1. 0% Fluorescent material (silicate yellow)
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED, and the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED and combined with the remaining blue light to form white light.
  • Example 4
  • the casting formula is as follows:
  • Silicone rubber 34 0% Thinner Phenyl silicone oil 10. 0% Auxiliary leveling agent 1. 0% fluorescent material (yellow)
  • the silicone rubber is a two-component addition-formed vulcanized liquid silicone rubber.
  • Implementation process Add the liquid raw material in the formula into the ingredient container, stir evenly, add the fluorescent material under stirring, stir and hook and perform vacuum defoaming treatment. The liquid raw material mixture is added to the mold from the bottom, and the feeding is stopped when the raw material overflows from the upper rubber mouth, the glue ports at both ends are sealed, and the curing is carried out in an oven for 2 minutes, and the light-transferring flexible polymer is formed after curing. The material can be removed from the mold.
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED for use, and the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED and combined with the remaining blue light to form a warm White light.
  • Example 5
  • the casting formula is as follows:
  • Silicone rubber 40 0% Thinner Mercapto vinyl silicone oil 10. 0% Fluorescent material (silicate orange)
  • the silicone rubber is a two-component addition-heating vulcanized liquid silicone rubber.
  • Implementation process Add the liquid raw material in the formula into the ingredient container, stir evenly, add the fluorescent material under stirring, stir and hook and perform vacuum defoaming treatment. The liquid raw material mixture is added to the mold and placed in a 145 ⁇ oven for curing for 2 minutes. After curing, the formed light-converting flexible polymer material is taken out from the mold.
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED, and the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED to emit orange-red light.
  • Example 6
  • the casting formula is as follows:
  • the silicone rubber is a two-component addition-formed vulcanized liquid silicone rubber.
  • Implementation process The liquid raw material in the formula is added into the ingredient container, stirred uniformly, and the fluorescent material is added under stirring, and the mixture is stirred and vacuum defoamed. Add the liquid raw material mixture from the bottom to the mold, stop feeding when the raw material overflows from the upper rubber port, seal the glue ports at both ends, and put it into the oven: for curing.
  • the formed light-converting flexible polymer material can be taken out from the mold after curing.
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED for use, and the fluorescent material in the light-converting flexible polymer material can be Excited by the light emitted by the blue LED, emitting green light.
  • Example 7
  • the casting formula is as follows:
  • Silicone rubber 53 0% Thinner Mercaptoethoxy silicone oil 10. 0% Auxiliary leveling agent 2. 0% Fluorescent material (aluminate yellow)
  • the silicone rubber is a two-component addition-formed vulcanized liquid silicone rubber.
  • Implementation process Add the liquid raw material in the formula into the ingredient container, stir evenly, add the fluorescent material under stirring, stir and hook and perform vacuum defoaming treatment. The liquid raw material mixture is added into the mold from the bottom, and the feeding is stopped when the raw material overflows from the upper rubber mouth, the glue ports at both ends are sealed, and the rubber is sealed in a 140 oven for 3 minutes, and the formed light is converted into a flexible high after curing. The molecular material can be taken out of the mold.
  • the prepared light-converting flexible polymer material can be directly placed or bonded on the surface of the blue LED, and the fluorescent material in the light-converting flexible polymer material can be excited by the light emitted by the blue LED to emit warm white light.

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Description

一种光转换柔性高分子材料及其用途
技术领域
本发明涉及光电子显示和照明技术领域， 且更具体涉及一种 掺杂了荧光材料的高分子材料及其制法及用途， 尤其是用于 LED 背光源、 数码显示及照明在内的发光装置的光转换柔性高分子材 料及其制法及用途。 背景技术
目前的 LED背光源、 数码显示及照明装置通常是采用封装荧 光发光材料方式得到的， 此类专利也已经有很多如中国专利 200510030192. 1〈白 色发光元件及其制造方法〉， 中国专利 200310120736〈表面安装型白 色发光二极管〉， 中国专利 200710151099. 5〈蓝紫光或蓝光激发的荧光体及制造方法与封装 的白光二极管〉，均为荧光材料混合在树脂中涂抹在 LED芯片上制 成白色发光器件。 该方法制备出的白光发光器件很难保证亮度、 色坐标、 色温和显色性的一致性， 并且由于荧光粉贴近芯片， 受 到热量的影响很容易引起老化， 寿命降低。
国际专利 WO2007105853介绍了一种光致发光膜的制备方法， 所采用的发光材料为无机发光材料， 该专利仅介绍的光致发光膜 采用硅树脂作为成膜材料进行制备， 但并未对光致发光膜的发光 材料与色坐标， 色温以及亮度的关系进行介绍， 同时也不是浇铸 成型， 不能形成多种形状。 国际专利 WO2007/ 049187介绍了一种 釆用硅酮掺杂磷光体的密封膜剂， 将这种膜材料安装在蓝光 LED 上， 达到蓝光转换为白光的目的，但是这种材料本身为膜状结构， 需根据使用情况采用层压的方式二次成型， 工艺复杂。 美国专利 US2008/0280957 Al 介绍了一种采用具有透镜结构的塑料器件制 备 LED的方法， 具有透镜结构的塑料器件^部为含有荧光材料层 的结构， 并且为压铸或注塑而成， 结构和工艺比较复杂并且成型 后不能改变形状。 中国专利 200810067358. 0《一种低衰减高光效 LED照明装置及制备方法》和中国专利 CN 185892 OA《一种白光 LED 等的封装方法》 均涉及一种将荧光发光材料加入到高分子材料中 经用模具成型制成透明罩的方法， 比较合适单颗 LED的封装， 该 方法成型后材料不可改变形状， 在安装和使用上受到限制。 中国 专利 CN101012916A《一种以 LED为光源的灯具》介绍了一种将光 转换材料固定在灯壳外罩上的方法， 该方法虽避免了荧光材料高 温老化的问题， 但材料距离光源有一定距离， 导致荧光材料发光 效率下降。 这种方式只适合灯具等产品的制备， 在应用上受到限 制。 发明内容
为了克服上述缺陷， 本发明采用有机硅橡胶作为成型材料， 添加稀释剂、 荧光材料、 助剂混合均勾后通过浇铸的形式经加热 固化成型。 根据使用的情况可设计成各种形状的模具， 针对 LED 蓝光光源的光学特性还可以将模具设计成带有透镜形式的结构进 行浇铸成型。 成型后的高分子材料柔软有弹性， 并具有一定的强 度， 可以随意弯曲变形， 可以根据需要在器件中进行组装。
本发明提供了一种光转换柔性高分子材料， 该材料的质量百 分比组成如下：
有机硅橡胶 20. 0% ~ 75. 0%
稀释剂 10. 0% ~ 20. 0%
荧光材料 15. 0% ~ 65. 0% 助剂 0. 0% ~ 5. 0%
其中： 所述有机硅橡胶为双组分加成型加温硫化液体硅橡胶； 所 述稀释剂为曱基硅油、 双甲基硅油、 乙基硅油、 苯基硅油、 曱基 乙氧基硅油或者曱基乙烯基硅油； 所述助剂为流平剂、 消泡剂、 偶联剂或润湿分散助剂或者它们的组合；
所述荧光材料为铝酸盐荧光材料、 硅酸盐荧光材料、 硅氮化 物荧光材料及硫氧化物荧光材料中的一种或两种的组合； 荧光材 料被作为激发光源的发射光谱在 440 ~ 475nm 范围内的蓝光 LED 激发，激发出至少一个以上峰值波长在 525 ~ 650nm范围内的发射 光谱； 荧光材料所发的光与蓝光 LED所发的光复合成白色或其它 颜色的光。
在本发明的光转换柔性高分子材料中， 所使用的荧光材料的 粒径优选为 3- 15 μ πι。
本发明的光转换柔性高分子材料具有多种用途，可用于灯具、 数码管或背光源等光源器件中。 釆用本发明制备的光转换柔性高分子材料可有效避免现有技 术中的问题。 这种材料柔软、 具有一定的强度和韧性， 可根据使 用的情况可设计成各种形状的模具进行浇铸成型， 成型后的光转 换柔性高分子材料， 荧光材料均勾分散在其中， 采用这种材料制 备的发光器件光色均匀， 并且由于材料在使用中并非紧贴芯片结 构， 避免了由于热量导致的老化问题， 可有效提高产品的寿命。 具体实施方式
本发明的光转换柔性高分子材料由有机硅橡胶、 稀释剂、 荧 光材料、助剂共同组成，各组成成分组分和质量百分比组成如下： 有机硅橡胶 20.0-75.0 稀释剂 10.0-20
荧光材料 15.0-65.0
助剂 0.0-5.0
其中：荧光材料被作为激发光源的发射光谱在 440 ~ 475nm范围内 的蓝光 LED 激发， 吸收激发出至少一个以上峰值波长在 525 ~ 650nm范围内的发射光谱；
荧光材料所发的光与蓝光 LED所发的光复合成白色的光或其 它色彩的光， 荧光材料可以是铝酸盐荧光材料、硅酸盐荧光材料、 硅氮化物荧光材料及硫氧化物荧光材料中的一种或几种的组合。
所述的铝酸盐荧光材料的主要化学组成表示式为：
aR203'R' 203： xCe, yLi， zF;
11为 ¥、 Tb、 Gd中的一种或多种元素的组合；
R' 为 Al、 Ga中的一种或两种元素的组合;
a、 x、 y、 z 为摩尔系数， 0.45<a<0.65; 0.0<x<0.04； 0.0<y<0.04; 0.0<z<0.2; 该材料的发射主峰波长随组成在 525 ~ 560nm范围内变化；
所述的硅酸盐荧光材料的主要化学组成表示式为：
Si02: xEu, yLi, zF;
M为 Sr、 Ca、 Ba、 Mg中的一种或多种元素的组合；
b、 x、y、z为摩尔系数， 1.4<b<3.1; 0.015<x<0.1; 0.0<y<0.05; 0.0<z<0.25; 该材料的发射主峰波长随组成在 525 - 580nm 范围 内变化。
所述的硅氮化物荧光材料的主要化学组成表示式为：
( SreCai-e ) 2-xSi5N8： Eux, Liy, Fz;
e、 x、 y、 z 为摩尔系数， 0.1 <e< l; 0.01 <x< 0.1; 0.0<y< 0.1; 0.0<z< 0. 5; 该材料的发射主峰波长随組成在 580 ~ 650nm 范围内变化；
所述的硫氧化物荧光材料的主要化学组成表示式为：
Y2-x02S: Eux, Mgy, Tiz， Li β， Fy;
x、 y、 z、 β、 Y为摩尔系数， 0.01 <x< 0.1; 0.005 <y< 0.02; 0.05<z< 0.25; 0.0< β < 0.1; 0.0< γ < 0.5; 该材料的发射主 峰波长随组成在 610~ 630nm范围内变化。
荧光材料粒径釆用 3-15微米比较合适，制备出的产品荧光材 料分散均勾， 发光效果好。
荧光材料可以被紫外或蓝光 LED所发出的光激发发光， 并且 与剩余紫外或蓝光复合成白光或其他各种颜色的光。 所述的各种 荧光材料其体色及发光颜色具有不同的特征， 在制造荧光发光材 料的柔性高分子材料时可依据各自不同的情况加以选用。 选择硅 酸盐、 铝酸盐发光荧光材料作为橙色、 黄色发光荧光材料， 选择 硅氮化物、 硫氧化物发光荧光材料作为红色发光荧光材料， 可将 黄色发光荧光材料、 橙色发光荧光材料和红色发光荧光材料复合 使用， 复合使用可调整色坐标、 色温和显色指数， 达到适用于多 种用途的目的， 采用发出黄色光的荧光材料与发出红色光的荧光 材料复合使用， 提高显色指数， 得到高显色指数的白光， 使其适 用于需要高显色指数的发光器件中。 所述光转换柔性高分子材料 与 LED复合， 合成白色的光或其它色彩的光， 用于灯具、 数码管、 背光源的光源器件中。
采用的有机硅橡胶为透明性好、 柔软、 弹性好的双组分加成 型加温硫化液体硅橡胶。 如双组分有机硅材料 SR- 5G0()A/B、 TCS-1310T/A/B, SN130P/A/B, ZS - 0020A/B, 170/A/B. 这种树 脂具有热氧化稳定性好、 优异的电绝缘性能、 卓越的耐浙、 防水、 防锈、 耐寒、 耐臭氧和耐候性能。 该树脂在长时间高温状态下工 作也不会黄变， 并且固化后仍然具有柔软有弹性的特点， 并具有 一定得强度， 可以随意弯曲变形，适用于不规则形状的器件使用。
稀释剂采用曱基硅油、 双曱基硅油、 乙基硅油、 苯基硅油、 曱基乙氧基硅油或曱基乙烯基硅油中一种。
助剂可以是流平剂、 消泡剂、 偶联剂、 润湿分散助剂中一种 或多种的组合。
有机硅树脂、 稀释剂、 荧光发光材料、 助剂混合均勾后通过 浇铸的形式经加热固化成型。 该材料可以用在灯具、 数码管、 背 光源等器件中， 根据器件所需的形状进行浇注成型后直接固定在 蓝光光源之上， 本材料也可在成型后根据器件的形状进行弯曲， 变形。
浇铸是有机高分子材料进行加工的一种方法。 早期的浇铸是 在常压下将液态单体或聚合物注入模具内， 经聚合而固化成型， 变成与模具内腔形状相同的制品。 随着成型技术的发展， 传统的 浇铸概念有所改变， 聚合物溶液、 分散体和熔体也可用于浇铸成 型。
由于荧光材料是一种无机材料， 这种材料在与金属材料摩擦 的过程中极易变黑、 失去发光性能， 因此， 在制造、 加工过程中 需要避免与金属材料接触。 使用浇铸工艺可以有效的避免传统的 高分子材料在材料制造和加工过程挤压或者摩擦导致的荧光发光 材料变黑或者失去发光性能的弊端。
本发明釆用的是有机硅橡胶、 稀释剂、 荧光材料和助剂混合 均匀后注入模具内， 经加热聚合而固化成型， 变成与模具内腔形 状相同的制品。 采用浇铸的方法可改变传统 LED封装工艺， 大大 减化工艺步骤， 其生产效率高、 易实现生产自动化、 改善操作环 境， 更重要的是发光荧光材料在高分子树脂中分散均匀， 用它制 成的发光器件发光的一致性大大改良、 光转换效果好、 产品灵活 多变。
釆用这种光转换柔性高分子材料摆脱了传统的封装方法制备
LED 的形式， 只需要在芯片上黏贴或者直接将光转换柔性高分子 材料组装在芯片上即可， 发光效果与封装形式制备出的 LED十分 接近。 同时， 釆用光转换柔性高分子材料还可以根据实际使用情 况浇铸出合适的形状， 如浇铸出带有透镜结构的形状， 可以 有 效提高光转化的效率并同时实现二次配光设计、 提高出光效率、 优化光学分布。 采用这种方式制备的发光器件安装、 维修、 更换 十分方便， 简化了施工工艺， 生产出的产品更加灵活多样。 由于 本发明的材料柔韧性和强度都十分优秀， 材料可以随意弯曲、 折 叠， 特别适合不规则形状的特殊发光器件的制备。 本发明的另外 一个有点是采用浇铸的方法进行材料成型， 由于荧光材料是一种 无机材料， 这种材料在与金属材料摩擦的过程中极易变黑、 失去 发光性能， 当采用如注塑等方式进行成型时， 荧光材料由于摩擦、 挤压会出现变黑， 发光性能下降的问题， 釆用浇铸方式则可以有 效的避免这种现象。
下面通过具体的实施例对本发明的光转换柔性高分子材料 进行举例说明。 实施例 1 :
浇铸配方如下：
有机硅橡胶 50. 0%
稀释剂 曱基硅油 20. 0%
助剂 润湿剂 0. 5% 偶联剂 1. 0%
消泡剂 0. 2%
荧光材料（铝酸盐 黄色）
0. 56Υ203 ·Α12Ο3·0· lGd203： 0. 04Ce, 0. 02F 23. 8%
其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物加入到模具中， 放入 烘箱中进行固化， 时间 2min， 固化后将成型的光转换柔性高分子材料从模具中取出 即可。
制备出的光转换柔性高分子材料可以应用于在蓝光 LED表面 进行使用， 光转换柔性高分子材料中的荧光材料可以被蓝光 LED 所发出的光激发发光， 并且与剩余蓝光复合成白光。 实施例 2:
浇铸配方如下：
有机硅橡胶 20. 0% 稀释剂 双甲基硅油 10. 0% 助剂 润湿剂 2. 0%
偶联剂 2. 0% 消泡剂 1. 0% 硅酸盐绿色荧光材料
0. 9SrO-l. IBaO-O. lMgO-S i02: 0. 2Eu, 0. OOlLi , 0. 05F; 26. 0% 硫氧化物红色荧光材料
Y02S: 0. 3Eu, 0. 02Mg, 0. 15Ti ; 39. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物加入到模具中， 放入 140 Ό烘箱中进行固化， 时间 3miri， 固化后将成型的光转换柔性高分子材料从模具中取出 即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材料可以 被蓝光 LED所发出的光激发发光， 并且与剩余蓝光复合成白光。 实施例 3:
浇铸配方如下：
有机硅橡胶 75. 0% 稀释剂 乙基硅油 9. 0% 助剂 消泡剂 1. 0% 荧光材料 （硅酸盐 黄色）
0. lCaO-1. 5SrO-0. 4BaO-0. lMgO-S i02: 0. lEu， 0. 2Li, 0. 05F 15. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物从底部加入到模具中， 待原料从上部胶口溢出 时停止加料， 封住两端胶口， 放入 143 TC烘箱中进行固化， 时间 3min，固化后将成型的光转换柔性高分子材料从模具中取出即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材料可以 被蓝光 LED所发出的光激发发光， 并且与剩余蓝光复合成白光。 实施例 4:
浇铸配方如下：
有机硅橡胶 34. 0% 稀释剂 苯基硅油 10. 0% 助剂 流平剂 1. 0% 荧光材料（黄色）
0. 58Υ203 ·Α12Ο3·0. lGa2O3: 0. 008Ce, 0. 004Li, 0. 02F 53. 0% 荧光材料（红色）
(Sr。.5Ca。 5) 2— yS i 5N8: 0. 05Eu, 0. 003Li , 0. 001F 2. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物从底部加入到模具中， 待原料从上部胶口溢出 时停止加料， 封住两端胶口， 放入 烘箱中进行固化， 时间 2min,固化后将成型的光转换柔性高分子材料从模具中取出即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材料可以 被蓝光 LED所发出的光激发发光， 并且与剩余蓝光复合成暖白色 光。 实施例 5:
浇铸配方如下：
有机硅橡胶 40. 0% 稀释剂 曱基乙烯基硅油 10. 0% 荧光材料（硅酸盐 橙色）
1. 4SrO · 0. 2BaO · S i02: 0. 05Eu, 0. 005Li 50. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物加入到模具中， 放入 145 Ό烘箱中进行固化， 时间 2min, 固化后将成型的光转换柔性高分子材料从模具中取出 即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材料可以 被蓝光 LED所发出的光激发， 发光出橙红色光。 实施例 6:
浇铸配方如下：
有机硅橡胶 67. 0% 稀释剂 甲基乙氧基硅油 10. 0% 助剂 消泡剂 1. 0%
润湿分散剂 2. 0 % 荧光材料（硅酸盐 绿色）
0. 9Sr0 · 1. IBaO · S i02: 0. 03Eu, 0. 005Li 20. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均 并进行真空脱泡处理。 将 液态的原料混合物从底部加入到模具中， 待原料从上部胶口溢出 时停止加料， 封住两端胶口， 放入 or:烘箱中进行固化， 时间
3min,固化后将成型的光转换柔性高分子材料从模具中取出即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材 ^H"可以 被蓝光 LED所发出的光激发， 发出绿色光 实施例 7:
浇铸配方如下：
有机硅橡胶 53. 0% 稀释剂 曱基乙氧基硅油 10. 0% 助剂流平剂 2. 0% 荧光材料 （铝酸盐 黄色）
0. 58Υ203 ·Α12Ο3·0· lGa203: 0. 008Ce, 0. 004Li , 0. 02F 15. 0% 荧光材料（硅酸盐 橙红色）
1. 4SrO-0. 2BaO-S i02: 0. 05Eu, 0. 005Li 20. 0% 其中的有机硅橡胶为双组分加成型加温硫化液体硅橡胶。 实施工艺： 将配方中的液体原料加入配料容器中，搅拌均匀， 在搅拌状态下加入荧光材料， 搅拌均勾并进行真空脱泡处理。 将 液态的原料混合物从底部加入到模具中， 待原料从上部胶口溢出 时停止加料， 封住两端胶口， 放入 140 烘箱中进行固化， 时间 3min,固化后将成型的光转换柔性高分子材料从模具中取出即可。
制备出的光转换柔性高分子材料可以直接放置或者粘结在蓝 光 LED表面进行使用， 光转换柔性高分子材料中的荧光材料可以 被蓝光 LED所发出的光激发， 发出暖白色光。

Claims

权 利 要 求 一种光转换柔性高分子材料， 其特征在于按质量百分比 由下列成分组成:
有机硅橡胶 20. 0% ~ 75. 0%
稀释剂 10. 0% ~ 20. 0%
荧光材料 15. 0°/ο ~ 65. 0%
助剂 0. 0% ~ 5. 0%
其中：所述有机硅橡胶为双组分加成型加温硫化液体硅橡胶； 所述稀释剂为甲基硅油、 双曱基硅油、 乙基硅油、 苯基硅油、 甲基乙氧基硅油或者曱基乙烯基硅油；
所述助剂为流平剂、 消泡剂、 偶联剂或润湿分散助剂或者它 们的组合；
所述荧光材料为铝酸盐荧光材料、 硅酸盐荧光材料、 硅氮化 物荧光材料及硫氧化物荧光材料中的一种或两种的组合； 荧光材 料被作为激发光源的发射光谱在 440 ~ 475mn 范围内的蓝光 LED 激发，激发出至少一个以上峰值波长在 525 ~ 650nm范围内的发射 光谱； 荧光材料所发的光与蓝光 LED所发的光复合成白色或其它 颜色的光。
2、 根据权利要求 1 所述的光转换柔性高分子材料， 其特征 为所述荧光材料的粒径为 3-15 μ πι。
3、 根据权利要求 1 所述的光转换柔性高分子材料在光源器 件中的用途， 所述光源器件是灯具、 数码管或背光源。
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