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High refractive index curable liquid light emitting diode encapsulant formulation

A technology of light-emitting diodes and sealants, applied in electroluminescent light sources, semiconductor/solid-state device parts, light sources, etc., can solve the problems of difficult processing of composites, uneven products, and inability to flow.

Active Publication Date: 2012-11-21
ROHM & HAAS ELECTRONICS MATERIALS LLC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nonetheless, these materials have a lower than desired refractive index because the products produced are not uniform and these composites are difficult to process (that is, the materials are not uniform and cannot flow)

Method used

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  • High refractive index curable liquid light emitting diode encapsulant formulation
  • High refractive index curable liquid light emitting diode encapsulant formulation
  • High refractive index curable liquid light emitting diode encapsulant formulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: POP monomer preparation

[0049] To a 500 mL Schlenk flask was added diethyl ether (400 mL); metallic magnesium powder (3.3 g; 135 mmol); and methyl iodide (0.1 mL). 4-Bromodiphenylether (32.161 g; 129 mmol) was then added to the flask and the reaction mixture was stirred for 4 hours. Phenyltrimethoxysilane (25.601 g, 129 mmol) was then added to the flask and the contents were stirred for an additional hour. The contents of the flask were then transferred to a 1 liter separatory funnel and the material was washed twice with 400 ml of distilled water. The ether layer was collected and volatiles were removed under reduced pressure. The purity of the crude product was further purified by short-path distillation to obtain the product POP monomer with a purity ≥ 97%. The product POP monomer contains < 500 ppm of phenoxyphenyl halide.

Embodiment 9-12

[0064] Examples 9-12: Curable Liquid Polysiloxane / TiO 2 Preparation of complex

[0065] Using the following general procedure, using the specific amounts shown in Table 3, a curable liquid polysiloxane / TiO 2 Complex. Specifically, the amounts of POP and PTMS shown in Table 3 and 15 ml of propylene glycol methyl ether acetate (PGMEA) were added to a 100 ml three-neck round bottom flask. A solution of 5 grams of methanol, 1 gram of water, and 0.16 grams of concentrated hydrochloric acid (37% in water, purchased from Fisher Scientific) was then added dropwise to the flask. The contents of the flask were then heated to 70°C and maintained at this temperature for 1.5 hours using a thermostatic heating mantle with a temperature probe and reflux condenser. Then through the addition funnel, the tetrabutyl titanate polymer (purchased from DuPont, trade name BTP) and 1 ml of anhydrous tetrahydrofuran (THF) were added dropwise into the flask, while maintaining the contents of ...

Embodiment VA

[0077] Embodiment VA and VC-VE, and embodiment V2-V11

[0078]In Comparative Examples VA and VC-VE and Examples V2-V11, Rheometric Scientific Inc. (now TA Instruments, New Castle, Delaware, USA) was used. ) RMS-800 Rheometrics Mechanical Spectrometer (Rheometrics Mechanical Spectrometer), the following general steps were used to measure the viscosity of the products prepared in Comparative Examples A and C-E, and Examples 2-11 respectively. Specifically, in each case, a sample of the material to be tested was loaded, sandwiching the sample of the material to be tested between two parallel aluminum plates with a diameter of 8 mm. The rheometer stand and plates were preheated to 60°C, equilibrated at this temperature for 15 minutes, and then the gap between the plates was zeroed. Then, for liquid samples with viscosities greater than 100 Pa-s, the temperature of the parallel plate was raised to 90°C to facilitate sample loading. After loading the sample material onto the bas...

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Abstract

A curable liquid polysiloxane / TiO2 composite for use as a light emitting diode encapsulant is provided, comprising: a polysiloxane prepolymer with TiO2 domains having an average domain size of less than 5 nm, wherein the curable liquid polysiloxane / TiO2 composite contains 20 to 60 mol % TiO2 (based on total solids); wherein the curable liquid polysiloxane / TiO2 composite exhibits a refractive index of >1.61 to 1.7 and wherein the curable liquid polysiloxane / TiO2 composite is a liquid at room temperature and atmospheric pressure. Also provided is a light emitting diode manufacturing assembly.

Description

technical field [0001] The present invention relates to a curable liquid polysiloxane / TiO 2 A composite comprising: a polysiloxane prepolymer having TiO having an average domain size of less than 5 nanometers 2 Area (domain); The average compositional formula of the polysiloxane prepolymer is: [0002] (R 4 3 SiO 1 / 2 ) a (R 1 (R 2 )SiO 2 / 2 ) b (R 3 SiO 3 / 2 ) c (R 5 x Z y SiO (4-x-y) / 2 ) d [0003] Based on the total weight of solids, the curable liquid polysiloxane / TiO 2 Composite contains 20-60 mol% TiO 2 ; The curable liquid polysiloxane / TiO 2 The composite has a refractive index greater than 1.61 to 1.7, the curable liquid polysiloxane / TiO 2 The complex is liquid at room temperature and pressure. The invention also relates to light emitting diode manufacturing components. Background technique [0004] Light emitting diode (LED) devices typically include an LED die encapsulated in an optically transparent, thermally stable material. The encapsulatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/06C08K3/22C09K3/10H01L33/56
CPCC08K3/22H01L33/00C09D183/04H05B33/20H01L33/56H01L33/52C09K3/10C08L83/04C08L83/06C08K2003/2237C08G77/04H01L23/29C08K2003/2241
Inventor G·卡纳里昂P·J·鲍帕J·R·埃尔W·周
Owner ROHM & HAAS ELECTRONICS MATERIALS LLC
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