WO2016074207A1 - Matière à mouler époxy blanche - Google Patents

Matière à mouler époxy blanche Download PDF

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Publication number
WO2016074207A1
WO2016074207A1 PCT/CN2014/091065 CN2014091065W WO2016074207A1 WO 2016074207 A1 WO2016074207 A1 WO 2016074207A1 CN 2014091065 W CN2014091065 W CN 2014091065W WO 2016074207 A1 WO2016074207 A1 WO 2016074207A1
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WO
WIPO (PCT)
Prior art keywords
moulding compound
white
epoxy
compound according
wax
Prior art date
Application number
PCT/CN2014/091065
Other languages
English (en)
Inventor
Qingxu YANG
Yuting Wang
Original Assignee
Ablestik (Shanghai) Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ablestik (Shanghai) Ltd filed Critical Ablestik (Shanghai) Ltd
Priority to PCT/CN2014/091065 priority Critical patent/WO2016074207A1/fr
Priority to TW104136591A priority patent/TWI676651B/zh
Publication of WO2016074207A1 publication Critical patent/WO2016074207A1/fr

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Classifications

    • 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
    • H01L33/58—Optical field-shaping elements
    • H01L33/60—Reflective elements
    • 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
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • 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
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
    • 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
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
    • 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
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/688—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing phosphorus
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide

Definitions

  • This invention relates to a white epoxy moulding compound, a process to prepare a white epoxy moulding compound and use of a white epoxy moulding compound.
  • optical semiconductor devices including a combination of an optical semiconductor element such as LED (Light Emitting Diode) and a fluorescent substance have grown.
  • LED Light Emitting Diode
  • Various applications including outdoor displays, portable liquid crystal backlights, and automotive applications have been found because of their advantages such as high energy efficiency and long life for such devices.
  • Brightness of LED devices have increased, however at the same time the working temperature has increased due the heat increase in the chip. This heat increase leads to the degradation of the device materials.
  • PPA Polyphthalamide
  • thermosetting light-reflecting resin compositions used in the optical semiconductor element mounting boards require specific characteristics.
  • the thermosetting light-reflecting resins need to have good optical properties and good thermal discolouration resistance, and in addition, high releasability during moulding is required.
  • thermosetting light-reflecting resin compositions available, which have these characteristics. However, there is still room for an improvement.
  • thermosetting light-reflecting resin which would exhibit good optical properties
  • thermosetting light-reflecting resin also with good thermal discolouration resistance in addition with high releasability during moulding.
  • a present invention relates to a white epoxy moulding compound comprising (a) an epoxy resin; (b) a white pigment; (c) a releasing agent; (d) a curing agent; (e) a curing agent catalyst; (f) a filler; and (g) a coupling agent, wherein said releasing agent is selected from the group consisting of polyolefin wax, polyester wax, mixture of polyolefin wax and polyester wax montan wax, carnauba wax and mixtures thereof.
  • the present invention further encompasses a process to manufacture a white epoxy moulding compound according to the present invention, comprising steps of: (1) kneading all of the white epoxy moulding compound components to form kneaded product, or mixing all of the white epoxy moulding compound components and extruding said mixture through an extruder; and (2) aging said kneaded or extruded product at 30°C-150°C.
  • the present invention encompasses a use of a white epoxy moulding compound according to the present invention as a reflector material in a LED device.
  • the present invention provides a white epoxy moulding compound comprising (a) an epoxy resin; (b) a white pigment; (c) a releasing agent; (d) a curing agent; (e) a curing agent catalyst; (f) a filler; and (g) a coupling agent, wherein said releasing agent is selected from the group consisting of polyolefin wax, polyester wax, mixture of polyolefin wax and polyester wax, montan wax, carnauba wax and mixtures thereof.
  • a white epoxy moulding compound according to the present invention has good optical properties, good thermal discolouration resistance and good releasebility during moulding.
  • a white epoxy moulding compound according to the present invention comprises an epoxy resin.
  • epoxy resin refers to oligomeric and polymeric materials comprising at least one epoxy group as part of their molecular structure.
  • An epoxy resin is preferred in the moulding compounds according to the present invention due to their good anti-aging performance.
  • the epoxy resin is not particularly limited, and there may be employed resins ordinarily used as epoxy resin moulding materials.
  • the epoxy resin used is colourless or comparatively uncoloured being for example pale yellow hue.
  • thermosetting epoxy resin which is capable of being B-staged.
  • solid epoxy resins and in particular, tri-or multi-functional epoxy resins.
  • useful epoxy resins include solid epoxy resins derived from bisphenol A or F or S, tetramethyl and/or biphenyl, epichlorohydrin, novalacs, diglycidyl isocyanurate (DGIC) and mixtures thereof.
  • the epoxy resin suitable for use in the present invention is solid at room temperature and has a melting point over 40°C but melting point less than 150°C.
  • the melting point is measured by using DSC.
  • the epoxy resin suitable for use in the present invention contains alicyclic structure.
  • the epoxy resin suitable for use used in the present invention has the light transmission at 460nm more than 80%when dissolved into methanol (5 mg/cm 3 ) .
  • the epoxy resin suitable for use in the present invention has the light transmission at 460nm greater than 70%, when heated in an air oven at 175°C for 48h, and subsequently dissolved into methanol (5 mg/cm 3 ) .
  • Examples of other useful epoxy components include epoxy monomers characterized by
  • X can be present at least once (i.e., mono-, di-, or tri-substituted) and may be chosen from H or D n A, where n can range between 0 and 1, with at least one X being D n A.
  • A can be represented by structure III below:
  • E can be a member selected from H, linear, branched or cyclic alkyl, alkenyl, alkynyl, alkoxy or aryl groups, having from 1 to 20 carbon atoms with or without substitution by halogen, silicon, hydroxy, nitrile, ester, amide or sulfate.
  • R can be selected from H, linear, branched or cyclic alkyl, alkenyl, alkynyl, alkoxy or aryl groups, having from 1 to 20 carbon atoms, with or without substitution by halogen, silicon, hydroxy, nitrile, ester, amide or sulfate.
  • Another suitable epoxy component can be represented as:
  • D and A can be as described above and can be present at least once and can also be present together attached to ring atoms which are in alpha-beta relation to one another.
  • a white epoxy moulding compound according to the present invention comprises an epoxy resin preferably selected from the group consisting of bisphenol A epoxy resins, bisphenol F epoxy resins, bisphenol S epoxy resins, diglycidyl isocyanurate, triglycidyl isocyanurate, poly [ (2-oxinaryl) -1, 2-cyclohexanediol] -2-ethyl- (hydroxymethyl) -1, 3-propanetriol and mixtures thereof, preferably said epoxy resin is selected from the group consisting of poly [ (2-oxinaryl) -1,2-cyclohexanediol] -2-ethyl- (hydroxymethyl) -1, 3-propanetriol, triglycidyl isocyanurate and mixtures thereof.
  • an epoxy resin preferably selected from the group consisting of bisphenol A epoxy resins, bisphenol F epoxy resins, bisphenol S epoxy resins, diglycidyl isocyanurate, triglycidyl isocyanurate, poly [
  • Epoxy resin poly [ (2-oxinaryl) -1, 2-cyclohexanediol] -2-ethyl- (hydroxymethyl) -1, 3-propanetriol and triglycidyl isocyanurate are preferred due their good thermal reflectance and their structural stability at elevated temperatures.
  • a white epoxy moulding compound according to the present invention comprises an epoxy resin from 3.0%to 10.5%by weight of the total weight of the moulding compound, preferably from 3.5%to 10.0%, more preferably from 3.75%to 9.0%.
  • the epoxy resin content is less than 3%by weight of the total weight of the moulding compound, it will result in poor wetting of the filler. While the epoxy resin content is more than 10.5 %by weight of the total weight of the moulding compound it will cause poor release-ability during moulding.
  • a white epoxy moulding compound according to present invention comprises a releasing agent.
  • an essential element of a white epoxy moulding compound according to the present invention is a releasing agent.
  • a function of releasing agent is to aid release of moulded item from the mould cavity. This easy release is important to ensure smooth and continuous production of final products with optimal optical and physical properties.
  • the conventionally moulded items have been black, and therefore, thermostability of the moulding compound has not been an issue. However, while white moulded articles are more demanded, requirement for the thermostability increases.
  • the white epoxy moulding compound according to the present invention does not have yellow colour. Yellow colouration decreases the reflectance. Therefore, suitable releasing agents used herein are preferably colourless or relatively colourless compounds and have excellent temperature stability.
  • Suitable releasing agents to be used in the present invention are for example carboxylic polyester waxes, polyolefin waxes, mixtures of carboxylic polyester waxes and polyolefin waxes, carnauba wax, montan wax and mixtures thereof.
  • waxes used as releasing agents in the present invention are synthetic waxes, which contain fewer impurities vs. natural waxes. Fewer impurities improve the performance of the wax as a releasing agent.
  • synthetic waxes which contain fewer impurities vs. natural waxes. Fewer impurities improve the performance of the wax as a releasing agent.
  • synthesized polyester waxes are very stable, and at the same time, their comb structure helps to demould.
  • the releasing agent wax suitable for use used in the present invention is solid at room temperature and has a melting point over 40°C and less than 150°C.
  • the melting point is measured by using DSC.
  • the releasing agent wax suitable for use used in the present invention does not contain any double bond or any conjugated structure.
  • the releasing agent wax suitable for use in the present invention has a melting viscosity at 120°C more than 100mPa. sand less than 10 Pa. s, wherein viscosity is measured by Brookfield viscometer with constant shear rate at 120°C.
  • the polyolefin releasing agent is a polyethylene wax.
  • polyethylene wax suitable for use in the present invention is a low molecular weight polyethylene, having an average molecular weight from 4000 to 6000, measured by gel permeation chromatography, preferably from 4500 to 5500 and more preferably 5000.
  • polyethylene wax suitable for use in the present invention has a density from 0.92 g/cm 3 to 0.94 g/cm 3 , measured according to ASTM D 792 T, preferably from 0.925 g/cm 3 to 0.935 g/cm 3 and more preferably 0.93 g/cm 3 .
  • polyethylene wax suitable for use in the present invention has a softening point from 110°C to 113°C, measured according to ASTM E 28-58T, preferably from 110, 5°C to 112°C and more preferably 111°C.
  • polyethylene wax suitable for use in the present invention has a viscosity from 3900 mPa ⁇ sto 4500 mPa ⁇ smeasured by Brookfield viscometer with constant shear rate at 120°C, preferably from 4100 mPa ⁇ sto 4300 mPa ⁇ sand more preferably 4200 mPa ⁇ s.
  • Example of commercially available polyethylene wax suitable for use in the present invention is Sanwax 161-P supplied by Sanyo Chemical Industries.
  • This polyethylene wax has an excellent temperature stability, it does not change its colour to yellow/yellowish and it has no influence to the colour of the final compound colour.
  • releasing agent is a polyester wax.
  • Suitable polyester waxes to be used in the present invention as releasing agents are for example polyester waxes with comb structure containing no other functional groups.
  • polyester wax suitable for use in the present invention is low molecular weight polyester, having an average molecular weight from 1800 to 2400, measured by gel permeation chromatography, preferably molecular weight from 1900 to 2100 and more preferably 2000.
  • polyester wax suitable for use in the present invention has a density from 0.94 g/cm 3 to 0.99 g/cm 3 measured according to ASTM D 792 T, preferably from 0.95 g/cm 3 to 0.985 g/cm 3 and more preferably from 0.96 g/cm 3 to 0.98 g/cm 3 .
  • polyester wax suitable for use in the present invention has a viscosity from 150 mPa ⁇ sto 200 mPa ⁇ smeasured by Brookfield viscometer with constant shear rate at 120°C, preferably from 160 mPa ⁇ sto 180 mPa ⁇ sand more preferably 170 mPa ⁇ s.
  • Preferred polyester wax has an excellent temperature stability and it does not change its colour to yellow/yellowish over the time and it does not effect on the colour of the final moulding compound.
  • polyester wax releasing agent for use in the present invention is from EuroCeras, sold under the trade mark 694.
  • This polyester wax has an excellent temperature stability, it does not change its colour to yellow/yellowish and it has no influence to the colour of the final compound colour.
  • the releasing agent can be a mixture of the polyolefin wax and polyester wax, preferably a mixture of polyethylene wax and polyester wax.
  • the ratio between polyethylene wax and polyester wax may be from 1:5 to 5:1. In one preferred embodiment releasing agent is 1:1 mixture of polyethylene wax and polyester wax.
  • releasing agent may be a carnauba wax.
  • suitable commercially available carnauba wax is TOWAX-1YL, from Toakasei Co., Ltd.
  • the releasing agent may be montan wax.
  • suitable commercially available montan wax is Licowax E FL, from Clariant.
  • a white epoxy moulding compound according to present invention comprises a releasing agent from 0.01%to 1%by weight of the total weight of the moulding compound of, preferably from 0.2%to 0.9%, more preferably from 0.4%to 0.85%and most preferably from 0.45%to 0.85%.
  • the releasing agent content is less than 0.01 %by weight of the total weight of the moulding compound, it will result in poor release-ability during moulding, while the releasing agent content is more than 1 %by weight of the total weight of the moulding compound it will cause surface contamination in the product after moulding.
  • a white epoxy moulding compound according to present invention comprises a white pigment.
  • White pigment is used to increase the brightness of the moulding compound and to provide high refractive index.
  • Suitable white pigment for use in the present invention is selected from the group consisting of TiO 2 , MgO, BaSO 4 , ZnO and mixtures thereof, preferably said white pigment is TiO 2 .
  • TiO 2 white pigment is coated with silica.
  • Uncoated TiO 2 is reactive under light and therefore, forms radicals under UV, and therefore, coated TiO2 is preferred.
  • Preferred silica coated white pigment TiO 2 increases the brightness of the composition and provides high refractive index, and furthermore is stable.
  • a white epoxy moulding compound according to the present invention comprises a white pigment from 10%to 60%by weight of the total weight of the moulding compound, preferably from 15%to 55%, more preferably from 30%to 50%and most preferably from 32%to 48%.
  • the white pigment content is less than 10 %by weight of the total weight of the moulding compound, it will result in poor reflectance. While the white pigment content is more than 60 %by weight of the total weight of the moulding compound it will cause poor dispersion of the filler.
  • a white epoxy moulding compound according to present invention comprises a curing agent.
  • the curing agent is the substance that hardens the adhesive when mixed with resin.
  • Suitable curing agent for use in the present invention is anhydride.
  • the curing agent may be a cycloaliphatic anhydride such as, hexahydrophthalic anhydride (HHPA) , methyl hexahydrophthalic anhydride (MHHPA) and mixtures thereof. Small quantities of other related anhydrides such as, but not limited to, tetrahydrophthalic anhydride and phthalic anhydride may be present with the cyclic anhydride.
  • the curing agent used in the present invention is hexahydrophthalic anhydride (HHPA) .
  • a white epoxy moulding compound according to the present invention comprises a curing agent from 2.0%to 10.0%by weight of the total weight of the moulding compound, preferably from 3.0%to 8.0%, more preferably from 5.5%to 8.0%and most preferably from 6.25%to 7.75%.
  • the curing agent content is less than 2 %by weight of the total weight of the moulding compound, it will result in poor wetting of the filler. While the curing agent content is more than 10 %by weight of the total weight of the moulding compound it will cause poor release-ability during moulding.
  • a white epoxy moulding compound according to present invention further comprises a curing agent catalyst.
  • a curing catalyst is desired (even the white epoxy moulding compound according to the present invention, and subsequently, cured product formed from it may be performed without a catalyst) .
  • a relatively small group of catalytic materials, tin soaps of fatty acids of 8 to 18 carbon atoms, zinc octoate, quaternary phosphonium compounds, imidazoles, amines and 1, 8-Diazabicyclo [5.4.0] undec-7-ene can exert a catalytic effort without impairing the clarity, colourless nature and other desirable properties of the moulding compound and the final cured product.
  • said curing agent catalyst is tetra-n-butylphosphonium-o, o-diethylphosphorodithioate.
  • a white epoxy moulding compound according to the present invention comprises a curing agent catalyst from 0.01%to 1.0%by weight of the total weight of the moulding compound, preferably from 0.05%to 0.5%, more preferably from 0.1%to 0.3%and most preferably from 0.15%to 0.25%.
  • the curing agent catalyst content is less than 0.01 %by weight of the total weight of the moulding compound, it will result in poor curability during moulding. While the curing agent catalyst content is more than 1 %by weight of the total weight of the moulding compound it will cause too short flow and/or incomplete fill during moulding.
  • a white epoxy moulding compound according to the present invention further comprises one or more coupling agents.
  • the adhesion (coupling) promoting material can be selected from any known adhesion promoters that include, but are not limited to, epoxy silanes and mercapto silanes.
  • Preferably coupling agent is epoxy silane based coupling agent. More preferably the coupling agent is trimethoxyepoxysilane.
  • Epoxysilane based coupling agent is preferred due its suitability for silica surfaces, and therefore, it improves the mixing of the components, especially mixing of silica coated TiO 2 .
  • the white epoxy moulding compound according to the present invention comprises a coupling agent from 0.01%to 2.0%by weight of the total weight of the moulding compound, preferably from 0.1%to 1.5%, more preferably from 0.65%to 1.2%and most preferably from 0.75%to 1.05%.
  • the coupling agent content is less than 0.01 %by weight of the total weight of the moulding compound, it will result in poor wetting of the filler, while the coupling agent content is more than 1 %by weight of the total weight of the moulding compound it will cause poor release-ability.
  • a white epoxy moulding compound according to the present invention further comprises a filler.
  • the filler is preferably inorganic filler, selected from the group consisting of SiO 2 , glass fiber, CaCO 3 and mixtures thereof.
  • the inorganic filler is spherical silica.
  • the average particle size of the filler is less than 120 ⁇ m. If the particle size is too small, it leads to a short spiral flow. On the other hand if the particle size is too large, dispersion of the particles is not ideal, and therefore, reflectance is affected negatively.
  • a white epoxy moulding compound according to the present invention comprises a filler from 10%to 60%by weight of the total weight of the moulding compound, preferably from 25%to 55%, more preferably from 30%to 50%and most preferably from 35%to 50%.
  • the filler content is less than 10 %by weight of the total weight of the moulding compound, it will result in poor release-ability, while the filler content is more than 60 %by weight of the total weight of the moulding compound it will cause short flow.
  • the white epoxy moulding compound according to the present invention may further include one or more antioxidant materials.
  • the antioxidant material (s) can be a material capable of enhancing the UV and/or heat resistance of the white epoxy moulding compound.
  • the antioxidant material can be selected from any known antioxidant material which can enhance the UV and/or heat resistance of the white epoxy moulding compound. Examples of suitable antioxidants include, but are not limited to, primary (phenolic) antioxidants and, desirably, esters having pendant hydroxyphenyl groups. Particularly desirable are alkyl salts of propionic acid and, more desirably, those including a sulfur bridge.
  • the antioxidant material can include a thiodialkylpropionate such as, but not limited to, thiodiethylenepropionate.
  • the antioxidant material comprises thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate] , commercially available from Ciba Specialty Chemicals under the tradename 1035.
  • Other useful antioxidants include those also commercially available from Ciba Specialty Chemicals under the tradename 1010 and 1076.
  • the white epoxy moulding compound according to the present invention has a good initial reflectance and stable reflectance for long period of time.
  • the white epoxy moulding compound according to the present invention after curing, has a reflectance of over 90%to visible light.
  • the initial reflectance (%) (460nm) test the reflectance of the material is measured.
  • initial reflectance is meant reflectance of fresh material, which is not aged.
  • Initial reflectance is measured by UV-vis spectrophotometer Perkin Elmer Lambda 3. Samples are prepared as follows: transfer mould press is used to make small plates, having a diameter of 25mm and height of 1mm. Sample material is put into the mould and the mould is placed in the press to apply a pressure of 70 kg/cm 2 at 175°C. The sample is kept in the mould for 120s. Subsequently, the prepared plate is removed from the mould and is ready to be measured. Initial reflectance test results for the examples according to the present invention and comparative example are illustrated in the table 2.
  • the white epoxy moulding compound according to the present invention after curing and after aging (for 100 hours at 150°C) , has a reflectance of over 80%to visible light.
  • reflectance after aging (%) (460nm) test the reflectance of material is measured.
  • after aging reflectance reflectance of material, which has been aged at 150°C for 1000h.
  • Reflectance after aging is measured by UV-vis spectrophotometer Perkin Elmer Lambda 3. The samples are prepared as described in Initial reflectance test described above but aged at 150°C for 1000h. Reflectance after aging test results for the examples according to the present invention and comparative example are illustrated in the table 2.
  • a process to manufacture a white epoxy moulding compound according to the present invention comprises steps of:
  • mixture is mixed with high speed mixer just before extruding to make ensure that all raw materials is homogenously mixed.
  • said aging step is done for 1000 hours.
  • the white epoxy moulding compound according to the present invention can be used as a reflector material in a LED device.
  • a white epoxy compounds have been prepared comprising steps of: (1) kneading all of the white epoxy moulding compound components to form kneaded product, or mixing all of the white epoxy moulding compound components and extruding said mixture through a extruder; and (2) aging said kneaded or extruded product at 150°C for 1000 hours.
  • thermoplastic resin In the spiral flow test the flow properties of a thermoplastic resin is determined by measuring the length and weight of resin flowing along the path of a spiral cavity. Spiral flow values over 64cm are preferred for the resins according to the present invention.
  • Samples for the spiral flow test were the powder of a thermosetting resin. No additional preparations were required.
  • the spiral flow is measured using a mould for spiral flow test according to ASTM D-3123, under the conditions of a mould temperature of 175°C, a transfer pressure of 6.8 MPa, and a curing time of 90s.
  • a hot plate is heated to the temperature of 175°C.
  • the sample is placed on the hot plate and let it stand as long as the sample is gelled.
  • stopwatch gelling time is measured (stopwatch is started immediately when the sample is placed on the hot plate and stopped when gelling is complete) .
  • the gel time test is done from the powder of a thermoplastic resin.
  • the moulding compound material can achieve a good reflectance and can provide good thermal resistance, meanwhile, the material is suitable for transfer moulding process.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Cette invention concerne une matière à mouler époxy blanche comprenant (a) une résine époxy ; (b) un pigment blanc ; (c) un agent de démoulage ; (d) un agent durcisseur ; (e) un catalyseur d'agent durcisseur ; (f) une charge ; et (g) un agent de couplage, ledit agent de démoulage étant choisi dans le groupe constitué par la cire polyoléfine, la cire polyester, un mélange de cire polyoléfine et cire polyester, la cire de lignite, la cire de carnauba et leurs mélanges. L'invention concerne également un procédé de fabrication d'une matière à mouler époxy blanche, comprenant les étapes suivantes : (1) le malaxage de tous composants constituant la matière à mouler époxy blanche pour obtenir un produit malaxé, ou le mélange de tous les composants constituant la matière à mouler époxy blanche et l'extrusion dudit mélange par passage dans une extrudeuse ; et (2) le vieillissement dudit produit extrudé ou malaxé à 150°C. Une utilisation de la matière à mouler époxy blanche à titre de matériau réflecteur dans un dispositif à LED est en outre décrite.
PCT/CN2014/091065 2014-11-14 2014-11-14 Matière à mouler époxy blanche WO2016074207A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/CN2014/091065 WO2016074207A1 (fr) 2014-11-14 2014-11-14 Matière à mouler époxy blanche
TW104136591A TWI676651B (zh) 2014-11-14 2015-11-06 白色環氧模製化合物

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2014/091065 WO2016074207A1 (fr) 2014-11-14 2014-11-14 Matière à mouler époxy blanche

Publications (1)

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WO2016074207A1 true WO2016074207A1 (fr) 2016-05-19

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Country Link
TW (1) TWI676651B (fr)
WO (1) WO2016074207A1 (fr)

Cited By (1)

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WO2018106875A1 (fr) * 2016-12-09 2018-06-14 3M Innovative Properties Company Compositions époxy basse densité résistantes à la chaleur/l'humidité

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113165223B (zh) * 2018-11-23 2024-03-05 巴斯夫涂料有限公司 涂覆部件的注射模塑的自动化方法

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US20110058776A1 (en) * 2009-09-07 2011-03-10 Ntto Denko Corporation Resin composition for optical semiconductor device, optical-semiconductor-device lead frame obtained using the same, and optical semiconductor device
US20120080705A1 (en) * 2010-10-05 2012-04-05 Nitto Denko Corporation Epoxy resin composition for optical semiconductor device, lead frame obtained using the same for optical semiconductor device, and optical semiconductor device
US20120217532A1 (en) * 2011-02-24 2012-08-30 Nitto Denko Corporation Resin composition for optical semiconductor element housing package, and optical semiconductor light-emitting device obtained using the same
US20130037840A1 (en) * 2011-08-10 2013-02-14 Nitto Denko Corporation Epoxy resin composition for optical semiconductor device and optical semiconductor device using the same
CN103641998A (zh) * 2013-12-24 2014-03-19 江苏华海诚科新材料有限公司 Led反射杯用的白色环氧树脂组合物

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Publication number Priority date Publication date Assignee Title
US20110058776A1 (en) * 2009-09-07 2011-03-10 Ntto Denko Corporation Resin composition for optical semiconductor device, optical-semiconductor-device lead frame obtained using the same, and optical semiconductor device
US20120080705A1 (en) * 2010-10-05 2012-04-05 Nitto Denko Corporation Epoxy resin composition for optical semiconductor device, lead frame obtained using the same for optical semiconductor device, and optical semiconductor device
US20120217532A1 (en) * 2011-02-24 2012-08-30 Nitto Denko Corporation Resin composition for optical semiconductor element housing package, and optical semiconductor light-emitting device obtained using the same
US20130037840A1 (en) * 2011-08-10 2013-02-14 Nitto Denko Corporation Epoxy resin composition for optical semiconductor device and optical semiconductor device using the same
CN103641998A (zh) * 2013-12-24 2014-03-19 江苏华海诚科新材料有限公司 Led反射杯用的白色环氧树脂组合物

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018106875A1 (fr) * 2016-12-09 2018-06-14 3M Innovative Properties Company Compositions époxy basse densité résistantes à la chaleur/l'humidité
US11091629B2 (en) 2016-12-09 2021-08-17 3M Innovative Properties Company Hot/wet resistant low density epoxy compositions

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TWI676651B (zh) 2019-11-11

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