WO2014119693A1 - 電子線硬化性樹脂組成物、リフレクター用樹脂フレーム、リフレクター、半導体発光装置、及び成形体の製造方法 - Google Patents
電子線硬化性樹脂組成物、リフレクター用樹脂フレーム、リフレクター、半導体発光装置、及び成形体の製造方法 Download PDFInfo
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- WO2014119693A1 WO2014119693A1 PCT/JP2014/052172 JP2014052172W WO2014119693A1 WO 2014119693 A1 WO2014119693 A1 WO 2014119693A1 JP 2014052172 W JP2014052172 W JP 2014052172W WO 2014119693 A1 WO2014119693 A1 WO 2014119693A1
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- WIPO (PCT)
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- electron beam
- resin composition
- reflector
- curable resin
- beam curable
- Prior art date
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Classifications
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- 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
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
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- H01L2924/181—Encapsulation
Definitions
- the present invention relates to an electron beam curable resin composition, a reflector resin frame, a reflector, a semiconductor light emitting device, and a method for producing a molded body.
- an LED element which is one of semiconductor light emitting devices, is widely used as a light source such as an indicator lamp because of its small size, long life, and excellent power saving.
- LED elements with higher luminance have been manufactured at a relatively low cost, and therefore, use as a light source to replace fluorescent lamps and incandescent lamps has been studied.
- a plurality of LED elements are arranged on a surface-mounted LED package, that is, a metal substrate (LED mounting substrate) such as aluminum.
- a system is often used in which a reflector (reflector) that reflects light in a predetermined direction is disposed around the.
- the LED element since the LED element generates heat at the time of light emission, in such a type of LED lighting device, the reflector deteriorates due to the temperature rise at the time of light emission of the LED element, and the reflectance decreases, and thus the brightness decreases. The life of the element will be shortened. Therefore, heat resistance is required for the reflector.
- Patent Document 1 proposes a resin composition comprising a fluororesin (A) having a carbon-hydrogen bond and titanium oxide (B).
- the resin composition described in Patent Document 1 has not been studied for heat distortion resistance.
- the present invention provides an electron beam curable resin composition that can exhibit excellent heat deformation even when formed into a molded body, a reflector resin frame using the resin composition, a reflector, a semiconductor light emitting device, and It aims at providing the shaping
- the present invention is as follows.
- An olefin resin and a crosslinking agent wherein the crosslinking agent has a saturated or unsaturated ring structure, and at least one of the atoms forming at least one ring is an allyl group or a methallyl group.
- An allyl group via a linking group, and an allyl substituent of any one of a methallyl group via a linking group, and the crosslinking agent is more than 15 parts by mass and 40 parts by mass with respect to 100 parts by mass of the olefin resin.
- the white pigment and inorganic particles other than the white pigment the total amount of which is 200 to 700 parts by mass with respect to 100 parts by mass of the olefin resin.
- An electron beam curable resin composition [7] The electron beam curable resin composition according to [6], wherein the inorganic particles other than the white pigment are silica particles and / or glass fibers. [8] The electron beam according to any one of [1] to [7], wherein the olefin resin is a resin obtained by ring-opening metathesis polymerization of a norbornene derivative or a hydrogenation thereof, polyethylene, polypropylene, or polymethylpentene. Curable resin composition.
- a reflector resin frame comprising a cured product of the electron beam curable resin composition according to any one of [1] to [8].
- the resin frame for reflectors according to [9], wherein the thickness is 0.1 to 3.0 mm.
- a reflector comprising a cured product of the electron beam curable resin composition according to any one of [1] to [8].
- An optical semiconductor element and a reflector provided around the optical semiconductor element and reflecting light from the optical semiconductor element in a predetermined direction are provided on a substrate, and at least a part of the light reflecting surface of the reflector
- a semiconductor light emitting device comprising a cured product of the electron beam curable resin composition according to any one of [1] to [8].
- an electron beam curable resin composition that can exhibit excellent heat distortion resistance even when formed into a molded body, a resin frame for a reflector using the resin composition, a reflector, a semiconductor light emitting device, and the A molding method using the resin composition can be provided.
- the electron beam curable resin composition of the present invention comprises an olefin resin and a specific crosslinking agent.
- the olefin resin include a resin obtained by ring-opening metathesis polymerization of a norbornene derivative or a hydrogenated product thereof, polyethylene, polypropylene, polymethylpentene, and the like. Of these, polymethylpentene is preferable.
- polymethylpentene has a refractive index of 1.46, which is very close to the refractive index of silica particles, so that even when mixed, it is possible to suppress inhibition of optical properties such as transmittance and reflectance. .
- it is suitable for use as a reflector of a semiconductor light emitting device.
- the heat resistance in the reflow process may not be sufficient.
- it was possible to obtain a resin composition capable of exhibiting sufficient heat resistance even in the reflow process by containing a specific crosslinking agent in polymethylpentene and irradiating it with an electron beam. Thereby, even when it is set as a reflector, deformation of the reflector due to melting of the resin can be prevented.
- Polymethylpentene has a high melting point of 232 ° C., and has a characteristic that the decomposition temperature is around 300 ° C. without being decomposed even at a processing temperature of about 280 ° C.
- the polymethylpentene is irradiated with an electron beam (for example, absorbed dose: 200 kGy)
- an electron beam for example, absorbed dose: 200 kGy
- the molecular chain breaks simultaneously with the crosslinking
- effective crosslinking hardly occurs with the resin alone.
- the crosslinking agent according to the present invention is contained, a crosslinking reaction is effectively caused by electron beam irradiation, so that deformation due to dissolution of the resin can be prevented even in the reflow process.
- Such a crosslinking agent has a saturated or unsaturated ring structure, and at least one of atoms forming at least one ring is an allyl group, a methallyl group, an allyl group via a linking group, and It has a structure formed by bonding to any allylic substituent of a methallyl group via a linking group.
- the crosslinking agent having such a structure, it is possible to obtain a resin composition that exhibits good electron beam curability and has excellent heat resistance.
- the saturated or unsaturated ring structure include a cyclo ring, a hetero ring, and an aromatic ring.
- the number of atoms forming the ring structure is preferably 3 to 12, more preferably 5 to 8, and still more preferably a 6-membered ring.
- the molecular weight of the crosslinking agent according to the present invention is preferably 1000 or less, more preferably 500 or less, and further preferably 300 or less. When the molecular weight is 1000 or less, it is possible to prevent the dispersibility in the resin composition from being lowered and to cause an effective crosslinking reaction by electron beam irradiation.
- the number of ring structures is preferably 1 to 3, more preferably 1 or 2, and further preferably 1.
- the melting point of the crosslinking agent is preferably not higher than the melting point of the olefin resin to be used, and is preferably 200 ° C. or lower, for example. Since the crosslinking agent as described above has excellent fluidity during processing, the processing temperature of the thermoplastic resin is lowered to reduce the thermal load, friction during processing is reduced, and the inorganic component filling amount is reduced. Can be increased.
- examples of the linking group in the crosslinking agent according to the present invention include an ester bond, an ether bond, an alkylene group, and a (hetero) arylene group.
- atoms forming the ring atoms that are not bonded to the allylic substituent are in a state in which hydrogen, oxygen, nitrogen, or the like is bonded, or in a state in which various substituents are bonded.
- the crosslinking agent according to the present invention it is preferable that at least two atoms among the atoms forming one ring of the crosslinking agent are independently bonded to an allylic substituent.
- the ring structure is a 6-membered ring
- at least two of the atoms forming the ring are independently bonded to an allylic substituent, and one allylic substituent is bonded to the atom.
- another allylic substituent is bonded to the atom at the meta position.
- the crosslinking agent according to the present invention is preferably represented by the following formula (1) or (2).
- R 1 to R 3 are each independently an allylic substituent of any one of an allyl group, a methallyl group, an allyl group via an ester bond, and a methallyl group via an ester bond.
- R 1 to R 3 are each independently an allylic substituent of any one of an allyl group, a methallyl group, an allyl group via an ester bond, and a methallyl group via an ester bond.
- crosslinking agent represented by the above formula (1) examples include triallyl isocyanurate, methyl diallyl isocyanurate, diallyl monoglycidyl isocyanuric acid, monoallyl diglycidyl isocyanurate, and trimethallyl isocyanurate.
- crosslinking agent represented by the above formula (2) examples include orthophthalic acid diallyl ester, isophthalic acid diallyl ester, and the like.
- the crosslinking agent according to the present invention is blended in an amount of more than 15 parts by weight and 40 parts by weight or less with respect to 100 parts by weight of polymethylpentene, preferably 15 to 30 parts by weight, and preferably 16 to 20 parts by weight. More preferably, it is blended. By blending more than 15 parts by mass and not more than 40 parts by mass, crosslinking can be effectively advanced without bleeding out.
- the polymethylpentene is preferably a homopolymer of 4-methylpentene-1, but 4-methylpentene-1 and other ⁇ -olefins such as ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1
- An ⁇ -olefin having 2 to 20 carbon atoms such as octene, 1-decene, 1-dodecene, 1-tetradecene, 1-octadecene, 1-eicocene, 3-methyl-1-butene, 3-methyl-1-pentene, etc.
- a copolymer mainly composed of 4-methylpentene-1 containing 90 mol% or more of 4-methyl-1-pentene may be used.
- the molecular weight of the homopolymer of 4-methylpentene-1 is preferably not less than 1,000, particularly preferably not less than 5,000, in terms of polystyrene as measured by gel permeation chromatography.
- the electron beam curable resin composition of the present invention preferably contains a white pigment.
- a white pigment By including a white pigment, it can be used for applications such as a reflector.
- titanium oxide, zinc sulfide, zinc oxide, barium sulfide, potassium titanate and the like can be used alone or in combination, and titanium oxide is particularly preferable.
- the content of the white pigment is preferably 200 to 500 parts by mass, more preferably 300 to 480 parts by mass, and further preferably 350 to 450 parts by mass with respect to 100 parts by mass of the olefin resin.
- the product performance eg, light reflectance of reflector, strength, molding warp
- a molding state is bad, and it can prevent that product performance (for example, the light reflectivity of a reflector) falls by a boss.
- the average particle diameter of the white pigment is preferably 0.10 to 0.50 ⁇ m in the primary particle size distribution from the viewpoint of obtaining a high reflectivity in consideration of moldability, and more preferably 0.10 to 0.40 ⁇ m.
- the thickness is preferably 0.21 to 0.25 ⁇ m.
- An average particle diameter can be calculated
- inorganic particles other than a white pigment are included.
- the inorganic particles other than the white pigment it is usually possible to use those which are blended in a thermoplastic resin composition and a thermosetting resin composition such as an epoxy resin, an acrylic resin, or a silicone resin, alone or in combination. it can.
- the shape and particle size of the inorganic particles are not particularly limited. For example, particles and fibers, irregular cross-section fibers, shapes having a large unevenness, and thin flakes can be used. Specific examples include silica particles and glass fibers.
- Such an electron beam curable resin composition is particularly suitable for a reflector.
- the inorganic particles according to the present invention can be used alone or in combination with those that are usually blended in thermoplastic resin compositions and thermosetting resin compositions such as epoxy resins, acrylic resins, and silicone resins.
- the content of the inorganic particles is preferably 10 to 300 parts by mass, more preferably 30 to 200 parts by mass, and still more preferably 50 to 120 parts by mass with respect to 100 parts by mass of the olefin resin.
- the electron beam curable resin composition of the present invention includes the olefin resin and the crosslinking agent described above, and, if necessary, at least one of inorganic particles such as silica particles and glass fibers, and a white pigment as described above. It can be produced by mixing at such a predetermined ratio.
- known means such as a two-roll or three-roll, a stirrer such as a homogenizer or a planetary mixer, or a melt kneader such as a polylab system or a lab plast mill can be applied. These may be performed at normal temperature, cooling state, heating state, normal pressure, reduced pressure state, or pressurized state.
- additives can be contained as long as the effects of the present invention are not impaired.
- various kinds of whisker, silicone powder, thermoplastic elastomer, organic synthetic rubber, fatty acid ester, glycerate ester, zinc stearate, calcium stearate, and other internal mold release agents benzophenone , Salicylic acid-based, cyanoacrylate-based, isocyanurate-based, oxalic acid anilide-based, benzoate-based, hindered amine-based, benzotriazole-based, phenol-based antioxidants, hindered amine-based, benzoate-based light stabilizers, etc.
- Additives can be blended.
- a dispersing agent like a silane coupling agent can be mix
- the silane coupling agent include disilazane such as hexamethyldisilazane; cyclic silazane; trimethylsilane, trimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, allyldimethylchlorosilane, trimethoxysilane, benzyldimethylchlorosilane, Methyltrimethoxysilane, methyltriethoxysilane, isobutyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, trimethylmethoxysilane, hydroxypropyltrimethoxysilane, phenyltrimethoxysilane, n-butyltrimethoxysilane, n-hexadecyl Trimethoxysilane, n-oct
- the electron beam curable resin composition of the present invention By using the electron beam curable resin composition of the present invention, various molded products can be molded, and a molded product (for example, a reflector) having a thinner thickness can be produced.
- a molded body is preferably produced by the molding method of the present invention. That is, the electron beam curable resin composition of the present invention is injection-molded by injection molding at a cylinder temperature of 200 to 400 ° C. and a mold temperature of 20 to 150 ° C., and before or after the injection molding process. It is preferable to produce by the shaping
- the acceleration voltage of an electron beam it can select suitably according to the resin to be used and the thickness of a layer. For example, in the case of a molded product having a thickness of about 1 mm, it is usually preferable to cure the uncured resin layer at an acceleration voltage of about 250 to 3000 kV.
- the transmission capability increases as the acceleration voltage increases. Therefore, when using a base material that deteriorates due to the electron beam as the base material, the transmission depth of the electron beam and the thickness of the resin layer are substantially equal.
- the accelerating voltage so as to be equal to each other, it is possible to suppress the irradiation of the electron beam to the base material, and to minimize the deterioration of the base material due to the excessive electron beam.
- the absorbed dose when irradiating with an electron beam is appropriately set depending on the composition of the resin composition, but is preferably an amount at which the crosslinking density of the resin layer is saturated, and the irradiated dose is preferably 50 to 600 kGy.
- the electron beam source is not particularly limited.
- various electron beam accelerators such as a cockroft Walton type, a bandegraft type, a resonant transformer type, an insulated core transformer type, a linear type, a dynamitron type, and a high frequency type. Can be used.
- the electron beam curable resin composition of the present invention as described above can be applied to various applications as a composite material applied on a substrate and cured, or as a cured product of an electron beam curable resin composition.
- it can be applied as a reflector for a light source for lighting and television such as a heat-resistant insulating film, a heat-resistant release sheet, a heat-resistant transparent substrate, a light-reflecting sheet for solar cells, and LEDs.
- the resin frame for a reflector of the present invention comprises a cured product obtained by molding the electron beam curable resin composition of the present invention described above. Specifically, the electron beam curable resin composition of the present invention is formed into pellets, and a resin frame having a desired shape is formed by injection molding, whereby the reflector resin frame of the present invention is manufactured.
- the thickness of the reflector resin frame is preferably 0.1 to 3.0 mm, more preferably 0.1 to 1.0 mm, and still more preferably 0.1 to 0.8 mm.
- a resin frame having a smaller thickness than a resin frame produced using glass fibers can be produced.
- a resin frame having a thickness of 0.1 to 3.0 mm can be produced.
- the resin frame for reflectors of the present invention formed in this way does not generate warp due to the inclusion of fillers such as glass fibers even when the thickness is reduced. Also excellent.
- the reflector resin frame of the present invention can be made into a semiconductor light-emitting device by placing an LED chip on the reflector frame and further sealing with a known sealant, followed by die bonding to obtain a desired shape.
- the resin frame for reflectors of this invention acts as a reflector, it is functioning also as a frame which supports a semiconductor light-emitting device.
- the reflector of the present invention comprises a cured product obtained by curing the electron beam curable resin composition of the present invention described above.
- the reflector may be used in combination with a semiconductor light-emitting device to be described later, or may be used in combination with a semiconductor light-emitting device (LED mounting substrate) made of another material.
- the reflector of the present invention mainly has an action of reflecting light from the LED element of the semiconductor light emitting device toward the lens (light emitting portion).
- the details of the reflector are the same as those of the reflector (reflector 12 described later) applied to the semiconductor light emitting device of the present invention, and are omitted here.
- the semiconductor light emitting device of the present invention is provided around an optical semiconductor element (for example, an LED element) 10 and the optical semiconductor element 10, and reflects light from the optical semiconductor element 10 in a predetermined direction.
- a reflector 12 is provided on the substrate 14. And at least one part (all in the case of FIG. 1) of the light reflection surface of the reflector 12 is comprised with the hardened
- the optical semiconductor element 10 emits radiated light (generally UV or blue light in a white light LED), for example, an active layer made of AlGaAs, AlGaInP, GaP or GaN sandwiched between n-type and p-type cladding layers. It is a semiconductor chip (light emitter) having a double heterostructure, and has a hexahedral shape with a side length of about 0.5 mm, for example. In the case of wire bonding mounting, it is connected to an electrode (connection terminal) (not shown) via a lead wire 16. Note that electrical insulation is maintained between the optical semiconductor element 10 and the electrode to which the lead wire 16 is connected by an insulating portion 15 formed of resin or the like.
- the shape of the reflector 12 conforms to the shape of the end portion (joint portion) of the lens 18 and is usually a cylindrical shape such as a square shape, a circular shape, or an oval shape, or an annular shape.
- the reflector 12 is a cylindrical body (annular body), and all the end faces of the reflector 12 are in contact with and fixed to the surface of the substrate 14.
- the inner surface of the reflector 12 may be expanded upward in a tapered shape (see FIG. 1).
- the reflector 12 can also function as a lens holder when the end portion on the lens 18 side is processed into a shape corresponding to the shape of the lens 18.
- the reflector 12 may have only the light reflecting surface side as a light reflecting layer 12a made of the electron beam curable resin composition of the present invention.
- the thickness of the light reflection layer 12a is preferably 500 ⁇ m or less, and more preferably 300 ⁇ m or less, from the viewpoint of reducing the thermal resistance.
- the member 12b on which the light reflecting layer 12a is formed can be made of a known heat resistant resin.
- the lens 18 is provided on the reflector 12, but this is usually made of resin, and various structures may be adopted and colored depending on the purpose and application.
- the space formed by the substrate 14, the reflector 12, and the lens 18 may be a transparent sealing portion, or may be a gap if necessary.
- This space portion is usually a transparent sealing portion filled with a light-transmitting and insulating material, and the force applied by directly contacting the lead wire 16 in wire bonding mounting and indirectly. Prevents electrical defects caused by the lead wire 16 being disconnected, cut, or short-circuited from the connection portion with the optical semiconductor element 10 and / or the connection portion with the electrode due to applied vibration, impact, etc. can do.
- the optical semiconductor element 10 can be protected from moisture, dust, etc., and the reliability can be maintained over a long period of time.
- Examples of the material (transparent sealant composition) that imparts translucency and insulation usually include silicone resins, epoxy silicone resins, epoxy resins, acrylic resins, polyimide resins, polycarbonate resins, and the like. Of these, silicone resins are preferred from the viewpoints of heat resistance, weather resistance, low shrinkage, and discoloration resistance.
- the reflector 12 having a predetermined shape is molded from the reflective resin composition of the present invention by transfer molding, compression molding, injection molding or the like using a mold having a cavity space having a predetermined shape.
- the separately prepared optical semiconductor element 10, electrodes and lead wires 16 are fixed to the substrate 14 with an adhesive or a bonding member, and the reflector 12 is further fixed onto the substrate 14.
- a transparent sealant composition containing a silicone resin or the like is poured into the recess formed by the substrate 14 and the reflector 12, and cured by heating, drying, or the like to obtain a transparent sealing portion.
- the lens 18 is disposed on the transparent sealing portion to obtain the semiconductor light emitting device shown in FIG.
- the composition may be cured.
- the insulating portion 15 is provided at any stage in each process.
- crosslinking agent is as follows. The structure of the following crosslinking agent is shown in the following Table 1 and chemical formula.
- Crosslinking agent 1 TAIC (triallyl isocyanurate) manufactured by Nippon Kasei Co., Ltd.
- Crosslinking agent 2 MeDAIC Metaldiallyl isocyanurate
- Crosslinking agent 3 DA-MGIC diallyl monoglycidyl isocyanuric acid
- Cross-linking treatment agent 4 manufactured by Shikoku Kasei Co., Ltd.
- MA-DGIC monoallyl diglycidyl isocyanurate
- Shikoku Kasei Co., Ltd. crosslinking agent 5 TMAIC (trimethallyl isocyanurate) manufactured by Nippon Kasei Co., Ltd.
- Examples 1 to 16, Comparative Examples 1 to 3 Various materials were blended and kneaded as shown in Tables 2-1 to 2-4 below to obtain resin compositions.
- a resin composition mix blends various materials and performs it using an extruder (Nippon Placon Co., Ltd. MAX30: Die diameter 3.0mm) and a pelletizer (Toyo Seiki Seisakusho MPETC1), and obtains a resin composition It was.
- These compositions were press-molded into a size of 750 mm ⁇ 750 mm ⁇ thickness 0.2 mm under the conditions of 250 ° C., 30 seconds, and 20 MPa to produce a molded body (1).
- the resin composition obtained above was used on an injection molding machine Sodick TR40ER Sodick (prep plastic type) on a silver plating frame (thickness: 250 ⁇ m), thickness: 700 ⁇ m, external dimensions: 35 mm ⁇ 35 mm, opening: 2
- a resin frame molded body (2) for a reflector was obtained by molding to a size of .9 mm ⁇ 2.9 mm.
- the injection molding machine conditions were as follows: cylinder temperature: 260 ° C., mold temperature: 70 ° C., injection speed: 200 mm / sec, holding pressure: 100 MPa, holding pressure time: 1 sec, cooling time: 15 sec.
- These compacts (1) and (2) were irradiated with an electron beam at an acceleration voltage of 800 kV and an absorbed dose of 400 kGy. The following characteristics were evaluated. The results are shown in Tables 2-1 to 2-4 below.
- MFR of the resin composition was measured by a method based on the method described in MFR of JIS K 7210: 1999 thermoplastics. Specifically, the test is performed at a test temperature of 280 ° C., a test load of 2.16 kg, and 60 seconds. As a measuring device, a melt flow tester manufactured by Thiast Co. was used.
- the composition contains an olefin resin and a predetermined crosslinking agent, and the crosslinking agent is blended in an amount of more than 15 parts by mass and less than 40 parts by mass with respect to 100 parts by mass of the olefin resin. Even in the case of a molded body, it was possible to obtain a resin composition capable of exhibiting excellent heat distortion resistance. From the above, it can be said that the resin composition of the present invention is useful for reflectors and reflectors for semiconductor light emitting devices.
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Abstract
Description
しかしながら、従来使用されてきた電子部品は耐熱性が十分とは言えず、特に赤外線加熱によるリフロー工程においては、部品表面の温度が局部的に高くなり変形が生じる等の問題があり、より耐熱性(特に、耐熱変形性)に優れた樹脂組成物及び電子部品が望まれていた。
以上から、本発明は、成形体とした場合においても優れた耐熱変形性を発揮し得る電子線硬化性樹脂組成物、当該樹脂組成物を用いたリフレクター用樹脂フレーム、リフレクター、半導体発光装置、及び当該樹脂組成物を用いた成形方法を提供することを目的とする。
[3] 前記架橋処理剤の環が6員環であり当該環を形成する原子のうちの少なくとも2つの原子が、それぞれ独立に、前記アリル系置換基と結合してなり、1つのアリル系置換基が結合した原子に対して、他のアリル系置換基がメタ位の原子に結合してなる[2]に記載の電子線硬化性樹脂組成物。
[7] 前記白色顔料以外の無機粒子がシリカ粒子及び/又はガラス繊維である[6]に記載の電子線硬化性樹脂組成物。
[8] 前記オレフィン樹脂がノルボルネン誘導体を開環メタセシス重合させた樹脂あるいはその水素添加、ポリエチレン、ポリプロピレン、及びポリメチルペンテンのいずれかである[1]~[7]のいずれかに記載の電子線硬化性樹脂組成物。
[10] 厚さが0.1~3.0mmである[9]に記載のリフレクター用樹脂フレーム。
[11] [1]~[8]のいずれかに記載の電子線硬化性樹脂組成物の硬化物からなるリフレクター。
[12] 光半導体素子と、該光半導体素子の周りに設けられ、該光半導体素子からの光を所定方向に反射させるリフレクターとを基板上に有し、前記リフレクターの光反射面の少なくとも一部が[1]~[8]のいずれかに記載の電子線硬化性樹脂組成物の硬化物からなる半導体発光装置。
[13] [1]~[8]のいずれかに記載の電子線硬化性樹脂組成物に対し、射出温度200~400℃、金型温度20~150℃で射出成形する射出成形工程と、射出成形工程の前又は後に、電子線照射処理を施す電子線照射工程を含む成形体の製造方法。
本発明の電子線硬化性樹脂組成物は、オレフィン樹脂と特定の架橋処理剤とを含んでなる。
オレフィン樹脂としては、例えば、ノルボルネン誘導体を開環メタセシス重合させた樹脂あるいはその水素添加物、ポリエチレン、ポリプロピレン、ポリメチルペンテン等が挙げられる。なかでも、ポリメチルペンテンが好ましい。
しかし、リフロー工程における耐熱性に対しては、十分でない場合があった。この問題に対し本発明では、特定の架橋処理剤をポリメチルペンテンに含有させ電子線を照射させることで、リフロー工程においても十分な耐熱性を発揮し得る樹脂組成物とすることができた。これにより、リフレクターとした際にも樹脂の融解によるリフレクターの変形を防ぐことができる。
また、ポリメチルペンテンに対して電子線を照射(例えば、吸収線量:200kGy)しても架橋と同時に分子鎖の切断が進行するため、樹脂単体では有効な架橋は起こり難い。しかし、本発明に係る架橋処理剤を含有させることにより、電子線照射によって有効に架橋反応が起こるため、リフロー工程においても樹脂の溶解による変形を防ぐことができるようになる。
飽和もしくは不飽和の環構造としては、シクロ環、ヘテロ環、芳香環等が挙げられる。環構造を形成する原子の数は、3~12であることが好ましく、5~8であることがより好ましく、6員環であることがさらに好ましい。
また、環構造の数は1~3であることが好ましく、1又は2であることがより好ましく、1であることがさらに好ましい。
上記のような架橋処理剤であれば、加工時に流動性に優れるため、熱可塑性樹脂の加工温度を低下させ熱負荷を軽減したり、加工時の摩擦を軽減したり、無機成分の充填量を増やすことができる。
さらに本発明に係る架橋処理剤は、下記式(1)又は(2)で表されることが好ましい。
上記式(2)で表される架橋処理剤としてはオルトフタル酸のジアリルエステル、イソフタル酸のジアリルエステル等が挙げられる。
4-メチルペンテン-1の単独重合体の分子量はゲルパーミッションクロマトグラフィーで測定したポリスチレン換算の重量平均分子量Mwが1,000以上、特に5,000以上が好ましい。
白色顔料の含有量は、オレフィン樹脂100質量部に対し、200~500質量部とすることが好ましく、300~480質量部であることがより好ましく、350~450質量部であることがさらに好ましい。200質量部超500質量部以下とすることで、製品性能(例、リフレクターの光反射率、強度、成形反り)が良好に維持することができる。また、無機成分が多く加工ができない、または加工できても成形状態が悪く、ボソボソで製品性能(例、リフレクターの光反射率)が低下してしまったりすることを防ぐことができる。
具体的には、シリカ粒子、ガラス繊維等が挙げられる。このような電子線硬化性樹脂組成物は、特にリフレクター用に好適である。
シランカップリング剤としては、例えば、ヘキサメチルジシラザン等のジシラザン;環状シラザン;トリメチルシラン、トリメチルクロルシラン、ジメチルジクロルシラン、メチルトリクロルシラン、アリルジメチルクロルシラン、トリメトキシシラン、ベンジルジメチルクロルシラン、メチルトリメトキシシラン、メチルトリエトキシシラン、イソブチルトリメトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシラン、トリメチルメトキシシラン、ヒドロキシプロピルトリメトキシシラン、フェニルトリメトキシシラン、n-ブチルトリメトキシシラン、n-ヘキサデシルトリメトキシシラン、n-オクタデシルトリメトキシシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、γ-メタクリルオキシプロピルトリメトキシシラン、及びビニルトリアセトキシシラン等のアルキルシラン化合物;γ-アミノプロピルトリエトキシシラン、γ-(2-アミノエチル)アミノプロピルトリメトキシシラン、γ-(2-アミノエチル)アミノプロピルメチルジメトキシシラン、N-フェニル-3-アミノプロピルトリメトキシシラン、N-(2-アミノエチル)3-アミノプロピルトリメトキシシラン、及びN-β-(N-ビニルベンジルアミノエチル)-γ-アミノプロピルトリメトキシシラン、ヘキシルトリメトキシシラン等のアミノシラン化合物;等が挙げられる。
このような成形体は、本発明の成形方法により製造することが好ましい。すなわち、本発明の電子線硬化性樹脂組成物に対し、シリンダー温度200~400℃、金型温度20~150℃で射出成形する射出成形工程と、射出成形工程の前又は後に、電子線照射処理を施す電子線照射工程を含む成形方法により作製することが好ましい。
なお、成形性を損なわない限りは、電子線照射による架橋反応は成形前に行うことができる。
さらに、電子線源としては、特に制限はなく、例えばコックロフトワルトン型、バンデグラフト型、共振変圧器型、絶縁コア変圧器型、あるいは直線型、ダイナミトロン型、高周波型などの各種電子線加速器を用いることができる。
本発明のリフレクター用樹脂フレームは既述の本発明の電子線硬化性樹脂組成物を成形した硬化物からなる。具体的には、本発明の電子線硬化性樹脂組成物をペレットとし、射出成形により所望の形状の樹脂フレームとすることで、本発明のリフレクター用樹脂フレームが製造される。リフレクター用樹脂フレームの厚さは0.1~3.0mmであることが好ましく、0.1~1.0mmであることがより好ましく、0.1~0.8mmであることがさらに好ましい。
本発明のリフレクターは、既述の本発明の電子線硬化性樹脂組成物を硬化した硬化物からなる。
当該リフレクターは、後述する半導体発光装置と組み合わせて用いてよいし、他の材料からなる半導体発光装置(LED実装用基板)と組み合わせて用いてもよい。
本発明のリフレクターは、主として、半導体発光装置のLED素子からの光をレンズ(出光部)の方へ反射させる作用を有する。リフレクターの詳細については、本発明の半導体発光装置に適用されるリフレクター(後述するリフレクター12)と同じであるためここでは省略する。
本発明の半導体発光装置は、図1に例示するように、光半導体素子(例えばLED素子)10と、この光半導体素子10の周りに設けられ、光半導体素子10からの光を所定方向に反射させるリフレクター12とを基板14上に有してなる。そして、リフレクター12の光反射面の少なくとも一部(図1の場合は全部)が既述の本発明のリフレクター組成物の硬化物で構成されてなる。
なお、光半導体素子10とリード線16が接続された上記電極とは、樹脂等で形成された絶縁部15により電気的絶縁が保たれている。
なお、リフレクター12の内面は、光半導体素子10からの光の指向性を高めるために、テーパー状に上方に広げられていてもよい(図1参照)。
また、リフレクター12は、レンズ18側の端部を、当該レンズ18の形状に応じた形に加工された場合には、レンズホルダーとしても機能させることができる。
まず、上記本発明の反射材樹脂組成物を、所定形状のキャビティ空間を備える金型を用いたトランスファー成形、圧縮成形、射出成形等により、所定形状のリフレクター12を成形する。その後、別途、準備した光半導体素子10、電極及びリード線16を、接着剤又は接合部材により基板14に固定し、さらにリフレクター12を基板14上に固定する。次いで、基板14及びリフレクター12により形成された凹部に、シリコーン樹脂等を含む透明封止剤組成物を注入し、加熱、乾燥等により硬化させて透明封止部とする。その後、透明封止部上にレンズ18を配設して、図1に示す半導体発光装置が得られる。
なお、透明封止剤組成物が未硬化の状態でレンズ18を載置してから、組成物を硬化させてもよい。また、絶縁部15は各工程のいずれかの段階で設けられる。
なお、本実施例1~16及び比較例1~3において使用した材料は下記の通りである。
・樹脂(1)
ポリメチルペンテン樹脂 :TPX RT18(三井化学(株)製)
・樹脂(2)
ポリエチレン:アドマーSF731(三井化学(株)製)
・樹脂(3)
ポリプロピレン:WF836DG3(住友化学(株)製)
・樹脂(4)
シクロオレフィンポリマー(COP):ノルボルネン重合体 ZEONOR 1600(日本ゼオン(株)製)
・樹脂(5)
フッ素樹脂:RP4020(ダイキン工業(株)製)
架橋処理剤については下記の通りである。また、下記架橋処理剤の構造ついては、下記表1及び化学式に示す。
TAIC(トリアリルイソシアヌレート) 日本化成社製
・架橋処理剤2
MeDAIC(メチルジアリルイソシアヌレート) 四国化成社製
・架橋処理剤3
DA-MGIC(ジアリルモノグリシジルイソシアヌル酸) 四国化成社製
・架橋処理剤4
MA-DGIC(モノアリルジグリシジルイソシアヌレート) 四国化成社製
・架橋処理剤5
TMAIC(トリメタリルイソシアヌレート)日本化成社製
酸化チタン粒子 :PF-691(石原産業(株)製 ルチル型構造 平均粒径0.21μm)
・ガラス繊維:PF70E-001(日東紡(株)製、繊維長70μm)
・シランカップリング剤:KBM-3063(信越化学(株)製)
・離型剤 :SZ-2000(堺化学(株)製)
・1次酸化防止剤 :IRGANOX1010(BASF・ジャパン(株)製)
・2次酸化防止剤 :PEP-36(アデカ(株)製)
下記表2-1~表2-4に示すように各種材料を配合、混練し、樹脂組成物を得た。
なお、樹脂組成物は、各種材料を配合し、押出機(日本プラコン(株) MAX30:ダイス径3.0mm)とペレタイザー((株)東洋精機製作所 MPETC1)を用いて行い、樹脂組成物を得た。
これらの組成物につき、250℃、30秒、20MPaの条件で、750mm×750mm×厚さ0.2mmにプレス成形し、成形体(1)を作製した。
また、上記で得た樹脂組成物を射出成形機ソディックTR40ERソディック(プリプラ式)を用いて、銀メッキフレーム(厚さ:250μm)上に厚み:700μm、外形寸法:35mm×35mm、開口部:2.9mm×2.9mmとなるよう成形しリフレクター用樹脂フレーム成形体(2)を得た。射出成形機条件は、シリンダー温度:260℃、金型温度:70℃、射出速度:200mm/sec、保圧力:100MPa、保圧時間:1sec、冷却時間:15secとした。
これらの成形体(1)及び(2)に、加速電圧を800kVで400kGyの吸収線量にて電子線を照射した。これらの下記諸特性を評価した。結果を下記表2-1~表2-4に示す。
・メルトフローレート(MFR)の測定
樹脂組成物のMFRはJIS K 7210:1999 熱可塑性プラスチックのMFRに記載の方法に準拠した方法により測定した。具体的には、試験温度280℃、試験荷重2.16kg、60秒で行う。測定装置としては、チアスト社製 メルトフローテスターを用いた。
・貯蔵弾性率
成形体(1)の試料を、RSAIII(TA INSTRUMENTS製)により、測定温度25~400℃、昇温速度5℃/min、Strain 0.1%の条件にて測定した。260℃での貯蔵弾性率を下記表2-1~表2-4に示す。
・リフロー耐熱
成形体(2)の試料を、表面温度265℃/320℃に設定したホットプレート上で20秒間加熱し、変形の有無を寸法変化率(縦方向の変化率と横方向の変化率の和)より評価した。結果を下記表2-1~表2-4に示す。
・反射率(長期耐熱)
成形体(1)の試料を、150℃で24時間、500時間放置する前と放置した後で、波長230~780nmにおける光反射率を反射率測定装置MCPD-9800(大塚電子(株))を使用して測定した。表2-1~表2-4には、波長450nmの結果を示す。
以上から、本発明の樹脂組成物は、リフレクターや半導体発光装置用の反射材に有用であるといえる。
12・・・リフレクター
14・・・基板
15・・・絶縁部
16・・・リード線
18・・・レンズ
Claims (13)
- オレフィン樹脂と架橋処理剤とを含み、
前記架橋処理剤が飽和もしくは不飽和の環構造を有し、少なくとも1つの環を形成する原子のうち少なくとも1つの原子が、アリル基、メタリル基、連結基を介したアリル基、及び連結基を介したメタリル基のいずれかのアリル系置換基と結合してなり、
前記架橋処理剤がオレフィン樹脂100質量部に対して15質量部超40質量部以下配合されてなる電子線硬化性樹脂組成物。 - 前記架橋処理剤の1つの環を形成する原子のうち少なくとも2つの原子が、それぞれ独立に、前記アリル系置換基と結合してなる請求項1に記載の電子線硬化性樹脂組成物。
- 前記架橋処理剤の環が6員環であり当該環を形成する原子のうちの少なくとも2つの原子が、それぞれ独立に、前記アリル系置換基と結合してなり、1つのアリル系置換基が結合した原子に対して、他のアリル系置換基がメタ位の原子に結合してなる請求項2に記載の電子線硬化性樹脂組成物。
- 白色顔料と前記白色顔料以外の無機粒子とを含み、これらの合計量がオレフィン樹脂100質量部に対して200~700質量部である請求項1~5のいずれか1項に記載の電子線硬化性樹脂組成物。
- 前記白色顔料以外の無機粒子がシリカ粒子及び/又はガラス繊維である請求項6に記載の電子線硬化性樹脂組成物。
- 前記オレフィン樹脂がノルボルネン誘導体を開環メタセシス重合させた樹脂あるいはその水素添加、ポリエチレン、ポリプロピレン、及びポリメチルペンテンのいずれかである請求項1~7のいずれか1項に記載の電子線硬化性樹脂組成物。
- 請求項1~8のいずれか1項に記載の電子線硬化性樹脂組成物の硬化物からなるリフレクター用樹脂フレーム。
- 厚さが0.1~3.0mmである請求項9に記載のリフレクター用樹脂フレーム。
- 請求項1~8のいずれか1項に記載の電子線硬化性樹脂組成物の硬化物からなるリフレクター。
- 光半導体素子と、該光半導体素子の周りに設けられ、該光半導体素子からの光を所定方向に反射させるリフレクターとを基板上に有し、
前記リフレクターの光反射面の少なくとも一部が請求項1~8のいずれか1項に記載の電子線硬化性樹脂組成物の硬化物からなる半導体発光装置。 - 請求項1~8のいずれか1項に記載の電子線硬化性樹脂組成物に対し、射出温度200~400℃、金型温度20~150℃で射出成形する射出成形工程と、射出成形工程の前又は後に、電子線照射処理を施す電子線照射工程を含む成形体の製造方法。
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