WO2011118108A1 - シリコーン樹脂製反射基材、その製造方法、及びその反射基材に用いる原材料組成物 - Google Patents
シリコーン樹脂製反射基材、その製造方法、及びその反射基材に用いる原材料組成物 Download PDFInfo
- Publication number
- WO2011118108A1 WO2011118108A1 PCT/JP2010/073445 JP2010073445W WO2011118108A1 WO 2011118108 A1 WO2011118108 A1 WO 2011118108A1 JP 2010073445 W JP2010073445 W JP 2010073445W WO 2011118108 A1 WO2011118108 A1 WO 2011118108A1
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- WIPO (PCT)
- Prior art keywords
- silicone resin
- reflective
- raw material
- inorganic filler
- reflective substrate
- Prior art date
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- 239000000758 substrate Substances 0.000 title claims abstract description 110
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 51
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- 239000000203 mixture Substances 0.000 title claims description 89
- 239000000843 powder Substances 0.000 claims abstract description 89
- 229910052751 metal Inorganic materials 0.000 claims abstract description 86
- 239000002184 metal Substances 0.000 claims abstract description 86
- 239000011256 inorganic filler Substances 0.000 claims abstract description 79
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 79
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 134
- 239000002994 raw material Substances 0.000 claims description 120
- -1 polysiloxane Polymers 0.000 claims description 110
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 102
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- 235000012211 aluminium silicate Nutrition 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
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- 239000010931 gold Substances 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
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- 238000007650 screen-printing Methods 0.000 description 15
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- 239000006087 Silane Coupling Agent Substances 0.000 description 13
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- 229920006136 organohydrogenpolysiloxane Polymers 0.000 description 13
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Definitions
- the present invention is incorporated in a light-emitting device such as a lighting fixture and reflects light from the light source to the side to be irradiated, or is incorporated in a solar cell assembly and reflects incident light on the photoelectric conversion element.
- the present invention relates to a reflective base made of silicone resin, a method for producing the same, and a raw material composition used for forming the reflective base.
- a light-emitting element that emits light of a desired wavelength such as a light-emitting diode (LED) is used as a light source of various light-emitting devices such as lighting fixtures, traffic lights, and backlights of liquid crystal displays.
- LED light-emitting diode
- Such light-emitting diodes, particularly high-intensity light-emitting diodes, are brighter, consume less power, and have a longer lifetime than white-type lighting fixtures such as incandescent bulbs, halogen lamps, mercury lamps, and fluorescent lamps.
- a photoelectric conversion element made of P-type silicon and N-type silicon that performs photoelectric conversion upon incidence of sunlight is incorporated in the solar cell assembly.
- a wiring board that mounts an element that receives and emits light such as a light emitting element or a photoelectric conversion element, and a package case that encloses and accommodates these elements reflect light from the light emitting element to the side to be irradiated.
- a reflective base made of ceramic or resin that can reflect these lights.
- the reflective base material of the wiring board or package case is made of ceramics, sufficient reflection efficiency cannot be obtained due to leakage of emitted light.
- Patent Document 1 an epoxy resin containing an alicyclic epoxy resin, a glycidyl (meth) acrylate polymer, a white pigment, and a resin composition containing a curing agent as essential components are disclosed.
- a white prepreg impregnated and dried on a substrate which is a support such as a sheet-like glass fiber is disclosed.
- Such resins and resin compositions such as liquid crystal polymers, polyamides, and bismaleimide / triazine (BT) resins are too low in viscosity to be applied only a few ⁇ m at a time, and the base of the support can be seen through. In addition, sufficient reflection efficiency cannot be obtained. Forcibly, even if it is applied in large amounts, dripping may occur, or only the surface will cause solvent volatilization and hardening preferentially, resulting in wrinkles. It becomes uniform. Therefore, the coating and drying of such a composition on the support are repeated to form a two-dimensional resin in several layers, and finally a thickness of about several tens of ⁇ m that shows the desired reflectance is sufficient. A whitened reflective layer was formed.
- a reflective non-silicone varnish containing a reflective component was cured to form a reflective substrate.
- these resin and varnish reflective base materials generally lack heat resistance such as yellowing and light resistance, and absorb light in a wavelength region of 400 nm or less, and thus are difficult to reflect.
- these resin and varnish reflective bases have the advantage of being inexpensive and easy to mold, they are heated to around 300 ° C. in the reflow process for lead flow soldering in recent years, so the heat causes yellowing. Initial deterioration, and with recent performance improvements such as shortening of the emission wavelength and higher output, etc. The surface gradually becomes dull, leading to a decrease in reflection efficiency. As a result, there is a problem in that the illumination characteristics of the initial design gradually change and become insufficient and dark.
- a versatile and simple reflective base material that is excellent in heat resistance and light resistance, does not deteriorate in reflectance over long periods of use, and has excellent thermal conductivity.
- the present invention has been made in order to solve the above-described problems, and includes a short wavelength of about 340 to 500 nm of the light emission wavelength of the LED light source including a wavelength of about 380 to 400 nm near the lower limit of the visible region, and a long wavelength in the near infrared region.
- An object of the present invention is to provide a reflective base made of silicone resin that is high in cost and can be manufactured at low cost.
- the present invention provides a raw material composition for a reflective layer in which a reflective layer can be formed by thick coating once on a support having various shapes, and a film shape having a thickness that provides sufficient reflectivity using the raw material composition.
- Another object of the present invention is to provide a method for producing a simple silicone resin reflective base material that can be molded into a three-dimensional shape or a plate shape.
- the reflective base made of silicone resin according to claim 1, which has been made to achieve the above object, has a white inorganic filler powder having a higher refractive index dispersed in a three-dimensionally crosslinked silicone resin.
- the reflective layer contained in the film is formed into a film shape, a three-dimensional shape or a plate shape on the support.
- the reflective base material made of silicone resin according to claim 2 is the one described in claim 1, wherein the silicone resin contains an acyclic dimethylsiloxy repeating unit as a main component.
- the reflective base material made of silicone resin according to claim 3 is the reflective base material according to claim 1, wherein the low molecular weight polysiloxane having a siloxy group repeating unit of 4 to 10 contained in the silicone resin is a maximum. However, it is characterized by 300 ppm.
- the reflective substrate made of silicone resin according to claim 4 is the reflective substrate according to claim 1, characterized in that the reflective layer is formed with a thickness of 1 to 2000 ⁇ m.
- the reflective substrate made of silicone resin according to claim 5 is the reflective substrate according to claim 1, wherein the silicone resin has a refractive index of 1.35 or more and less than 1.65.
- the reflective base material made of silicone resin according to claim 6 is the one described in claim 1, wherein the white inorganic filler powder is titanium oxide, alumina, barium sulfate, magnesia, aluminum nitride, boron nitride, titanium. It is at least one light reflecting agent selected from barium acid, kaolin, talc, calcium carbonate, zinc oxide, silica, mica powder, powdered glass, powdered nickel and powdered aluminum.
- the reflective base material made of silicone resin according to claim 7 is the reflective base material according to claim 1, wherein the white inorganic filler powder is a silane coupling treatment and dispersed in the silicone resin.
- the reflective base material made of silicone resin according to claim 8 is the reflective base material according to claim 6, wherein the white inorganic filler powder is anatase type or rutile type titanium oxide, alumina, or barium sulfate. It is characterized by that.
- the reflective substrate made of silicone resin according to claim 9 is the reflective base material according to claim 8, wherein the titanium oxide is surface-treated with Al, Al 2 O 3 , ZnO, ZrO 2 , and / or SiO 2. It is characterized by being coated.
- the reflective base material made of silicone resin according to claim 10 is the reflective base material according to claim 1, wherein the white inorganic filler powder has an average particle size of 0.05 to 50 ⁇ m, and 2 in the silicone resin. It is characterized by containing ⁇ 80% by mass.
- the reflective base material made of silicone resin according to claim 11 is the reflective base material according to claim 1, characterized in that the white inorganic filler powder and the phosphor are contained in the reflective layer while being dispersed. To do.
- the reflective base material made of silicone resin according to claim 12 is the reflective base material according to claim 11, wherein at least one of the white inorganic filler powder and the phosphor is exposed on the surface of the reflective layer. It is characterized by that.
- the reflective base material made of silicone resin according to claim 13 is the reflective base material according to claim 1, wherein the surface of the reflective layer is continuous, and has a concave-convex shape of nanometer to micrometer order, a prism shape, and / or It is characterized by a non-mirror surface having a pear ground shape.
- the reflective substrate made of silicone resin according to claim 14 is the reflective base material according to claim 1, wherein at least a part of the surface of the silicone resin is polished, roughened, molded by a rough mold or stamped. A part of the white inorganic filler powder is exposed from the surface by molding and / or chemical etching.
- the reflective substrate made of silicone resin according to claim 15 is the reflective substrate made of silicone resin according to claim 1, wherein the reflective layer covering the support with the conductive pattern attached is polished, and the conductive pattern is exposed. It is characterized by that.
- the reflective substrate made of silicone resin according to claim 16 is the one according to claim 15, characterized in that a metal film is attached on the surface.
- the reflective substrate made of silicone resin according to claim 17 is the reflective base material according to claim 16, wherein the metal film is formed of at least one metal selected from copper, silver, gold, nickel, and palladium. It is characterized by.
- the reflective substrate made of silicone resin according to claim 18 is the reflective substrate according to claim 16, wherein the metal film is a plating film, a metal vapor-deposited film, a metal sprayed film, or a bonded metal foil film. It is characterized by.
- the method for producing a reflective base made of silicone resin according to claim 19 is the method according to claim 1, wherein the back surface, outer periphery and / or light guide material reflection of any one of the light emitting element, the light emitting device and the photoelectric conversion element. It is arranged on the surface.
- the method for producing a reflective base made of a silicone resin according to claim 20 of the present invention comprises the step of forming the silicone resin into a polymerizable silicone resin raw material that is polymerized into a three-dimensionally crosslinked silicone resin. After dispersing the white inorganic filler powder having a higher refractive index than the raw material composition, the raw material composition is applied to the support in the form of a film, three-dimensionally crosslinked, and polymerized to the silicone resin, The reflective layer is formed in a film shape, a three-dimensional shape or a plate shape on the support.
- the method for producing a reflective substrate made of a silicone resin according to claim 21 is the method according to claim 20, wherein the polymerization is performed by at least one of humidification, pressurization, and ultraviolet irradiation. To do.
- the method for producing a reflective substrate made of a silicone resin according to claim 22 is the method according to claim 20, wherein the polymerization is performed during injection molding in a mold or pressure molding in a mold. And / or by pressurization.
- the method for producing a reflective base made of silicone resin according to claim 23 is the method according to claim 22, wherein the surface of the mold is coated with a fluororesin.
- the method for producing a reflective substrate made of silicone resin according to claim 24 is the method according to claim 20, wherein the polymerizable silicone resin raw material is cross-linked with a three-dimensional crosslinking agent for the silicone resin, and heated. Inactive or volatilized reaction inhibitor is dispersed and contained, and after dispersing white inorganic filler powder having a refractive index higher than that of the silicone resin to obtain the raw material composition, the heating causes the Polymerization is performed.
- the raw material composition according to claim 25 of the present invention made to achieve the above object comprises: a raw material for a polymerizable silicone resin; a cross-linking agent for three-dimensionally cross-linking the raw material for the silicone resin; and the silicone resin.
- the raw material composition according to claim 26 is the raw material composition according to claim 25, and is characterized by containing a reaction inhibitor that is deactivated or volatilized by heating.
- a raw material composition according to a twenty-seventh aspect is the one according to the twenty-fifth aspect, characterized in that it contains an organic solvent and / or a reactive diluent for viscosity adjustment.
- the reflective base made of silicone resin of the present invention contains a white inorganic filler powder having a refractive index higher than that of the silicone resin while being dispersed. Therefore, from the emission wavelength of the LED light source of about 340 to 500 nm, the near infrared region, for example, 1000 nm. High reflection efficiency of high-intensity light in a wide range of wavelengths up to long wavelengths, especially high reflection efficiency even in the short wavelength region such as blue light and near ultraviolet rays, which were difficult to reflect in the past, and excellent heat conductivity and easy heat dissipation Is. Moreover, this silicone resin reflective base material is excellent in concealing property and does not cause light leakage.
- the reflective layer in the reflective base made of silicone resin is formed of a stable three-dimensional cross-linked silicone resin that is unlikely to be decomposed or altered by light or heat, and preferably has an acyclic dimethylsiloxy repeating unit in the main chain. It is made of a silicone resin containing as a main component. Therefore, it is far more stable than light and heat-resistant epoxy resin, and is stable to light and heat. It is not only reflective efficiency but also light resistance over time, especially UV light resistance or high brightness light resistance, and heat resistance. Property, durability such as weather resistance, flame retardancy, and workability are excellent, and yellowing does not occur over a long period of time and hardly deteriorates.
- the reflective base made of silicone resin can maintain high reflectivity because the reflective layer remains white even after a long period of time.
- This reflective base made of silicone resin is a high-intensity light-emitting diode, even if it contains white inorganic filler powder, especially titanium oxide with extremely high decomposition catalytic activity, due to heat and light stable siloxy repeating units. Even when exposed to direct sunlight or high temperatures for a long period of time, neither yellowing nor deterioration occurs.
- This silicone resin reflective base material improves the reflectivity when white inorganic filler powder and phosphor are dispersed in the reflective layer and the particles are exposed from the surface, so the irradiation efficiency when mounted on a light emitting device Can be improved.
- the difference in refractive index between the white inorganic filler powder and the low refractive index silicone rubber raw material in contact with the phosphor surface is desirable because the reflection of light is more efficiently reflected and the light is reflected and emitted more efficiently from the surface of the exposed white inorganic filler powder or phosphor.
- the surface of the reflective layer of the reflective base made of silicone resin may be a mirror surface that reflects the surface.
- the surface is a non-mirror surface, it is easy to diffuse and diffuse reflectance is improved, and light reflection unevenness can be reduced.
- the reflective layer having the silicone resin has a film-like, three-dimensional structure on the support. It can be formed in a shape or plate shape.
- a liquid composition containing a white inorganic filler powder and a polymerizable silicone resin raw material or a grease-like or plastic raw material composition is coated to a thickness of 2000 ⁇ m at the maximum, and is then three-dimensionally cross-linked and cured to produce a reflective layer Can be formed.
- the reflective base made of silicone resin is highly versatile because the reflective layer can be shaped freely according to the wiring board, assembly or package case of the optical element.
- the raw material composition can also be used to form a reflective material that also serves as an adhesive for bonding a component such as a package case to a support.
- the polymerizable silicone resin raw material composition is formed so as to have a high viscosity and can be applied thickly.
- the metal such as a conductive pattern and the conductor of an element such as a light-emitting diode can be reduced. It is easy to perform wiring processing such as soldering.
- the surface of the reflective base made of silicone resin itself is on the order of nanometer to micrometer by surface treatment such as physical polishing / roughening, rough metal mold, or chemical chemical etching.
- surface treatment such as physical polishing / roughening, rough metal mold, or chemical chemical etching.
- the polishing may be mirror polishing, rough surface polishing, or cutting polishing.
- This reflective base made of silicone resin is highly productive because it can be manufactured easily, homogeneously and with high quality precisely, reliably and in large quantities at a low cost in a simple process.
- the reflective base made of silicone resin is not only a light emitting element such as a light emitting diode, but also various optical elements such as a photoelectric conversion element such as a solar cell element, a wiring case, a package case, a back sheet, and other lighting fixture members. It can be used for general purposes as a reflective base material for devices in various fields such as electrical members.
- a thick coating of 2000 ⁇ m can be made without dripping. For this reason, it is polymerized into a three-dimensionally crosslinked silicone resin by injection molding (LIMS), stamp molding using a pressing mold / roller, spraying or coating, and from a thin film of 1 to 10 ⁇ m.
- the reflective layer can be formed in a thick film or plate having a thickness of 2000 ⁇ m or a three-dimensional shape.
- the silicone resin raw material composition is directly or after adjusting to an appropriate viscosity, followed by screen printing, bar coater, roll coater, reverse coater, gravure coater.
- an air knife coater, a spray coater, or a curtain coater may be used, and a thin film may be applied by a known application method such as a high-precision offset coater or a multi-stage roll coater. Since this thick coating can form the desired shape even once, it is not necessary to repeat coating and drying.
- molds are preferably coated with a release agent such as a fluororesin such as polytetrafluoroethylene.
- the polymerizable silicone resin raw material composition does not cause deformation during heating because it does not cause a decrease in viscosity when heated as in the case of a raw material composition such as an epoxy resin, even if diluted with a suitable solvent. In this way, a reflective layer having a desired shape and thickness can be formed.
- Such polymerization is simply completed by heating, humidification, ultraviolet irradiation, or if necessary under pressure, to form a reflective layer having excellent adhesion to the support. Therefore, this manufacturing method is excellent in processing characteristics, high in production efficiency, and can be manufactured in any shape of a reflective base material. Therefore, it is excellent in versatility and suitable for mass industrial production.
- the manufacturing method of the reflective base made of silicone resin makes it easy to release using a mold which is vapor-deposited with fluorine resin or spray-coated and coated to about 0.1 mm, and has any desired shape, arbitrary A reflective layer having a surface roughness of 5 mm can be formed accurately and with good reproducibility, and the yield and production efficiency can be further improved.
- This method for producing a reflective base made of silicone resin includes a raw material for a silicone resin in which a polymerizable silicone resin raw material contains a three-dimensional crosslinking agent, a reaction inhibitor deactivated or volatilized by heating, and a white inorganic filler.
- a polymerizable silicone resin raw material contains a three-dimensional crosslinking agent, a reaction inhibitor deactivated or volatilized by heating, and a white inorganic filler.
- 1 is a light emitting device
- 2 is a solar cell assembly
- 10 is a package case of a reflective base made of silicone resin
- 11 is an inner wall
- 12a and 12b are white inorganic filler powders
- 13 is a light emitting diode
- 14a and 14b are lead wires
- 15a 15b is a copper film
- 16 is a support
- 17 is a solar cell element
- 17a is a p-type silicon semiconductor
- 17b is an n-type silicon semiconductor
- 18a and 18b are copper films
- 20 and 21 are substrates of a silicone resin reflective base material
- 22 is a glass cloth
- 31 is a mold
- 32 is a hole
- 33 is a dicing saw
- 34 is a coating nozzle
- 35 is a roller
- 36 is a grinder.
- the reflective base made of silicone resin of the present invention is incorporated in a lighting fixture 1 that is a kind of light emitting device, and copper foils 15 a and 15 b that are wiring patterns for mounting a light emitting diode 13 as a light emitting element. Is used for a wiring board provided with a reflective base material 20 made of silicone resin and a package case 10 surrounding the light emitting element 13.
- the reflective base material 10/20 made of silicone resin which is such a package case or wiring board, has a reflective layer containing a white inorganic filler powder having a higher refractive index dispersed in a silicone resin on the support. It is formed in a film shape, a three-dimensional shape or a plate shape.
- the silicone resin reflective base materials 10 and 20 are exposed with a silicone resin, and a portion of, for example, anatase-type titanium oxide particles that are white inorganic filler powders 12a and 12b are exposed.
- the reflective base materials 10 and 20 made of silicone resin are white and have an excellent concealing property so that light is not leaked. Furthermore, the reflectance of light from the short wavelength region of 380 to 420 nm to the long-wavelength near infrared ray is extremely high at that portion.
- the reflective base materials 10 and 20 made of silicone resin have high reflectivity, can maintain a white color without being yellowed even when exposed to high luminance light for a long period of time, and have high mechanical strength and are excellent. Since it shows light resistance, heat resistance, and weather resistance, it has excellent durability.
- the reflective layer of the reflective base material 10 or 20 made of silicone resin is a silicone resin containing a non-cyclic dimethylsiloxy repeating unit [—Si (—CH 3 ) 2 —O—] as a main component in the main chain, for example, refraction.
- a white inorganic material composed of a silicone resin comprising polydimethylsiloxane having a refractive index of 1.41, a silicone resin having a polydimethylsiloxane main chain and three-dimensionally cross-linked main chains, and a titanium oxide having a higher refractive index.
- Filler powders 12a and 12b are contained.
- the silicone resin containing an acyclic dimethylsiloxy repeating unit as a main component in the main chain is not particularly limited, and includes a hard silicone resin, a soft silicone resin, and a silicone rubber. Silicone resin should be used properly according to the application. For example, when it is used in a three-dimensional shape such as a casing, it is preferably a hard or soft silicone resin from the viewpoint of shape stability. When the support is a flexible material, it is preferably silicone rubber. When manufactured by grinding as shown in FIGS. 6 and 7 described later, a hard silicone resin or a soft silicone resin is preferable because it can be adjusted to a desired thickness with high accuracy.
- the rubber is generally 90 or less in Shore A hardness as measured with a JIS A type hardness meter, and according to a JIS D type hardness meter.
- Shore D hardness in the measurement is 30 or less, it is a feeling that it is a rubber when touched.
- a Shore D hardness of 50 or less can be regarded as a rubber region.
- the Shore D hardness is from 40 to 60, it is a soft resin reflective layer, and when it exceeds 60, the rubber property is lost and it can be said to be a hard reflective layer having high resin properties.
- Such a silicone resin is bonded to the Si atom of the next repeating unit of the same main chain or the repeating unit of another main chain via an oxygen atom and / or a crosslinkable functional group and three-dimensionally cross-linked.
- examples of the silicone resin include the following substances.
- the silicone resin is hard or soft and exhibits inelasticity or rubber elasticity.
- the silicone resin raw material composition used to form the silicone resin reflective substrate of the present invention includes various curable types such as addition reaction curable type, organic peroxide curable type, and condensation curable type.
- curable types such as addition reaction curable type, organic peroxide curable type, and condensation curable type.
- an addition reaction curing type is preferable.
- the addition reaction curable type is small in curing shrinkage at the time of curing and can prevent generation of wrinkles on the film when cured.
- a silicone resin containing an acyclic dimethylsiloxy repeating unit as a main component in the main chain is more specifically a polymer having a degree of polymerization of about 5000 to 10,000 and an average molecular weight of about 400,000 to 800,000. It is.
- This silicone resin may be polydimethylsiloxane composed of only the dimethylsiloxy repeating unit [—Si (—CH 3 ) 2 —O—], so-called dimethyl silicone, and may be [—Si (—CH 3 ) 2 —.
- the silicone resin raw material in such a silicone resin raw material composition has, as a main component, an organopolysiloxane having one or more alkenyl groups in the molecule, and one or more silicon-bonded hydrogen atoms in the molecule.
- Organohydrogenpolysiloxane and platinum group metal catalyst-containing polysiloxane can be mentioned.
- it contains fine powder silica of 0.2% or more by mass ratio with respect to the organopolysiloxane in order to surely express non-conductivity while preventing the decrease in volume resistivity due to the metal powder content. Good.
- this silicone resin raw material composition is provided with an adhesive property having a reactive functional group such as an epoxy group, an alkoxysilyl group, a carbonyl group, and a phenyl group in order to improve adhesion and adhesion to the support. It may contain components.
- the silicone resin used to form the reflective substrate of the present invention may be three-dimensionally cross-linked with another cross-linkable functional group.
- the intermediate Si group may be an alkyloxysilyl group, a dialkyloxysilyl group, a vinylsilyl group, a divinylsilyl group, a hydrosilyl group, a dihydrosilyl group, or a plurality of such groups.
- the main chain of the acyclic dimethylsiloxy repeating unit is three-dimensionally crosslinked in a network form through the presence of these functional groups.
- the main chains may be three-dimensionally crosslinked directly by these crosslinkable functional groups and / or indirectly via a silane coupling agent.
- the main chains are condensed between each crosslinkable functional group or between a crosslinkable functional group and a silane coupling agent by a dealcoholization reaction between each alkyloxysilyl group or dialkyloxysilyl group.
- a platinum catalyst such as a platinum complex
- a vinylsilyl group or divinylsilyl group and a hydrosilyl group or dihydrosilyl group are added and crosslinked by heating or light irradiation in the absence of a solvent.
- the silicone resin is preferably added and crosslinked.
- the silicone resin has a repeating unit such as a repeating unit of a dimethylsiloxy group (—Si (CH 3 ) 2 —O—) forming a main chain and a diphenylsiloxy group (—Si (C 6 H 5 ) 2 —O—). It may have a unit.
- the silicone resin has a repeating unit of a dimethylsiloxy group in the main chain and is crosslinked with an alkyloxysilyl group, a dialkyloxysilyl group, a vinylsilyl group, a divinylsilyl group, a hydrosilyl group, or a dihydrosilyl group. preferable.
- the three-dimensionally cross-linked silicone resin is obtained, for example, when a polymerizable silicone resin raw material is three-dimensionally cross-linked and cured. More specifically, the raw material of an addition reaction curable type silicone resin will be described as an example.
- a silicone resin is formed by thermosetting.
- an organopolysiloxane is used as a base polymer, and an organohydrogenpolysiloxane and a platinum-based material are used.
- the thing containing heavy metal type catalysts, such as a catalyst, is mentioned.
- organopolysiloxane examples include the following average unit formula R 1 a SiO (4-a) / 2 Wherein R 1 is an unsubstituted or substituted monovalent hydrocarbon group, preferably having 1 to 10 carbon atoms, especially 1 to 8. a is 0.8 to 2, especially 1 to 1.8. (It is a positive number.) The thing shown by is mentioned.
- R is an alkyl group such as a methyl group, an ethyl group, a propyl group or a butyl group, an alkenyl group such as a vinyl group, an allyl group or a butenyl group, an aryl group such as a phenyl group or a tolyl group, or an aralkyl such as a benzyl group.
- a halogen-substituted hydrocarbon group such as a chloromethyl group, a chloropropyl group, or a 3,3,3-trifluoropropyl group in which some or all of the hydrogen atoms bonded to these carbon atoms are substituted with a halogen atom
- a cyano group-substituted hydrocarbon group such as a 2-cyanoethyl group substituted with a cyano group may be mentioned, and R 1 may be the same or different, but R 1 may be a methyl group, particularly a dimethylsiloxy group. What is a methyl group which becomes a main component is preferable from the viewpoints of reflectivity, heat resistance and durability.
- R 1 containing an alkenyl group having 2 to 8 carbon atoms such as a vinyl group, particularly 1 to 20 mol% of all R is preferably an alkenyl group. Those having at least one are preferably used.
- organopolysiloxane include dimethylpolysiloxane having a alkenyl group such as a vinyl group and / or a dimethylsiloxane / methylphenylsiloxane copolymer at the terminal and / or in the middle of the main chain, and / or Alternatively, an alkenyl group-containing diorganopolysiloxane may be mentioned in the middle of the main chain, and in particular, those which are liquid at normal temperature are preferably used.
- alkenyl group-containing organopolysiloxane is R 2 — [Si (R 3 ) 2 —O] b — [Si (R 3 ) (R 4 ) —O] c —R 2
- R 2 is the same or different, saturated hydrocarbon group such as methyl group exemplified by R 1 or aromatic hydrocarbon group such as phenyl group or alkenyl group exemplified by R 1
- R 3 is the same or different
- R 1 is a saturated hydrocarbon group or aromatic hydrocarbon group exemplified by R 1
- R 4 is an alkenyl group exemplified by R 1
- b and c are positive numbers). Or random copolymerization.
- Such an alkenyl group-containing organopolysiloxane may be linear, may include a branched structure in a part of the molecular structure, or may be a cyclic body.
- a linear diorganopolysiloxane is preferred from the viewpoint of physical properties such as mechanical strength, elasticity, and resistance to repeated bending of a reflective substrate containing a three-dimensionally crosslinked silicone resin.
- the number of repeating units is preferably 10 to 10,000.
- Such alkenyl group-containing diorganopolysiloxane preferably has a viscosity at 25 ° C. of about 10 to 1,000,000 cSt.
- the organohydrogenpolysiloxane is linear, branched, cyclic, or three-dimensional network, and is singular or plural, preferably trifunctional or more (that is, hydrogen atoms bonded to silicon atoms in one molecule). (Having three or more (Si—H groups)) is preferable, and it is not particularly limited as long as it has Si—H groups at the ends and / or in the middle of the main chain.
- Si—H groups Si—H groups
- methyl hydrogen polysiloxane Methylphenyl hydrogen polysiloxane, and the like, and liquids at room temperature are particularly preferable.
- the catalyst examples include platinum, platinum compounds, organometallic compounds such as dibutyltin diacetate and dibutyltin dilaurate, and metal fatty acid salts such as tin octenoate.
- organometallic compounds such as dibutyltin diacetate and dibutyltin dilaurate
- metal fatty acid salts such as tin octenoate.
- the types and amounts of these organohydrogenpolysiloxanes and catalysts may be appropriately determined in consideration of the degree of crosslinking and the curing rate.
- organohydrogenpolysiloxane examples include the following average unit formula H d R 5 e SiO (4-de) / 2 (Wherein R 5 is a group exemplified by R 1 , particularly a saturated hydrocarbon group, and d and e are numbers satisfying 0 ⁇ d ⁇ 2, 0.8 ⁇ e ⁇ 2). .
- organohydrogenpolysiloxane examples include 1,1,3,3-tetramethyldisiloxane, 1,3,5,7-tetramethyltetracyclosiloxane, 1,3,5 , 7,8-pentamethylpentacyclosiloxane, etc., a siloxane oligomer having a Si—H group at its terminal; trimethylsiloxy end group-containing methylhydrogen polysiloxane, trimethylsiloxy end group-containing dimethylsiloxane / methylhydrogensiloxane copolymer, Silanol terminal group-containing methyl hydrogen polysiloxane, Silanol terminal group-containing dimethyl siloxane-methyl hydrogen siloxane copolymer, dimethyl hydrogen siloxy terminal group-containing dimethyl polysiloxane, dimethyl hydrogen siloxy terminal group-containing methyl Hydrogen polysiloxane, dimethyl hydrogen siloxy terminal groups containing homopolymer or copoly
- Such organohydrogenpolysiloxanes contain R 5 2 (H) SiO 1/2 units and SiO 4/2 units, R 5 3 SiO 1/2 units, R 5 2 SiO 2/2 units, R 5 It may contain (H) SiO 2/2 units, (H) SiO 3/2 units or R 5 SiO 3/2 units.
- This organohydrogenpolysiloxane can be obtained by, for example, cohydrolyzing a chlorosilane compound such as R 5 SiHCl 2 or R 5 2 SiHCl (where R 5 is the same as described above), or these chlorosilane compound and R 5 3 SiCl or the like. It may be prepared by cohydrolyzing another chlorosilane compound such as R 5 2 SiCl 2 (wherein R 5 is the same as described above), or may be prepared by equilibrating it.
- This organohydrogenpolysiloxane is used together with an alkenyl group-containing organopolysiloxane. Both are preferably blended so that the SiH group of the organohydrogenpolysiloxane is 0.5 to 4 molar equivalents relative to 1 molar equivalent of the alkenyl groups of the alkenyl group-containing organopolysiloxane.
- a platinum group metal catalyst used for a platinum group metal catalyst-containing polysiloxane is a hydrosilylation reaction catalyst for promoting an addition reaction between an alkenyl group of an alkenyl group-containing organopolysiloxane and an SiH group of an organohydrogenpolysiloxane. It is.
- the catalyst include various metal catalysts.
- platinum group metal simple substance such as platinum, platinum black, rhodium and palladium; H 2 PtCl 4 ⁇ mH 2 O, H 2 PtCl 6 ⁇ mH 2 O, NaHPtCl 6 ⁇ mH 2 O, KHPtCl 6 ⁇ mH 2 O, Na 2 PtCl 6 ⁇ mH 2 O, K 2 PtCl 4 ⁇ mH 2 O, PtCl 4 ⁇ mH 2 O, PtCl 2 , Na 2 HPtCl 4 ⁇ mH 2 O (Where m is a number from 0 to 6), such as platinum chloride complex, chloroplatinic acid complex and chloroplatinic acid complex salt; alcohol-modified chloroplatinic acid; chloroplatinic acid-olefin complex; platinum group metals such as platinum and palladium Support metal supported on a support such as alumina, silica, carbon, etc .; rhodium-olefin complex;
- the platinum group metal catalyst may be used in the presence of an alkenyl group-containing organopolysiloxane or organohydrogenpolysiloxane, and may be used in a catalyst amount of about 0.1 to 500 ppm relative to them. Good.
- Silicone resins include, for example, triorganosiloxy units (R 3 SiO 1/2 units: M units), diorganosiloxy units (R 2 SiO units: D units), monoorganosiloxy units (RSiO 3/2 units: T units). Unit) and siloxy units (SiO 2 unit: Q unit) arbitrarily combined resin (however, the organo groups R are the same or different and are crosslinkable such as alkyl groups such as methyl groups, phenyl groups, or vinyl groups) A group derived from a functional group). With these combinations, any combination of resins such as MQ resin, MDQ resin, MTQ resin, MDTQ resin, TD resin, TQ resin, and TDQ resin in which three-dimensional crosslinking is formed can be used as the silicone resin.
- the Si atom of the repeating unit is bonded to the Si atom of the next repeating unit via an oxygen atom or a crosslinkable functional group, and is three-dimensionally crosslinked.
- the reflective base made of silicone resin is attached to an electrical component, it causes electric contact obstruction and cloudiness, and low molecular siloxane contained in the silicone resin, for example, 4 to 10 repeating units of siloxy group It is even more preferable that the low molecular weight siloxane (D4 to D10) is formed of a silicone resin from which 300 ppm, preferably less than 50 ppm, has been previously removed.
- a commercially available low molecular weight siloxane-reducing grade polymerizable silicone resin raw material is used, or as a low molecular weight siloxane removal treatment, a heating oven treatment (eg, heat treatment at 200 ° C.
- a vacuum heat treatment eg, under vacuum
- a silicone resin raw material that has been subjected to a heat treatment such as heating at 200 ° C. for 2 hours can be used.
- low molecular siloxane can be removed from the molded article by means such as ultrasonic solvent extraction. Although the low molecular siloxane can be removed from the silicone resin raw material, it is preferable to remove the low molecular siloxane from the molded product because it can be removed to a lower level.
- the silicone resin raw material composition may be a so-called two-component composition in which the two components are mixed and cured at the time of use, as in the case of a normal curable silicone resin composition. It is preferable to use a one-pack type from the viewpoint of workability and the like.
- This silicone resin raw material composition can be cured under normal conditions.
- the silicone resin raw material composition can be crosslinked and cured by heating or irradiation with ultraviolet rays to develop hard or soft inelasticity or rubber elasticity.
- Such a reflective base material 10/20 made of silicone resin may have a reflective layer formed on an untreated support.
- the adhesive strength and adhesion of the silicone resin are excellent, and thus the adhesive strength between the support and the reflective layer is high.
- the coated surface side of the support is previously subjected to corona discharge treatment, plasma treatment, ultraviolet treatment, flame treatment, and intro treatment.
- a reflective layer is formed on a surface-treated support such as a roughened surface because the reflective base material is more firmly adhered and adhered to the surface-treated support.
- these supports and the reflective material layer are firmly bonded by corona discharge treatment, plasma treatment, ultraviolet irradiation treatment, flame treatment or itro treatment, and the reactive group-containing polysiloxane which becomes an adhesive body. It may be surface-treated with a solution.
- a functional silane compound such as a silane coupling agent may be used on the surface to be either or one of the adhesive bodies.
- functional silane compounds include polysiloxanes containing reactive groups that are highly reactive with OH groups.
- n is a number of 3 to 4, and at least one of the reactive groups —OCH 3 reacts with a functional group such as an OH group on the surface of the reflective layer and the metal foil layer
- the repeating unit may be one obtained by block copolymerization or random copolymerization.
- a platinum catalyst may be held on a vinyl group.
- Table 1 shows the bending strength and hardness of the silicone resin reflective base material with and without the silane coupling treatment.
- the composition of the silicone resin raw material containing the white inorganic filler powder in the silicone resin raw material adjusts the addition amount of the white inorganic filler powder and silicone rubber powder or the addition amount of organic solvent and reactive diluent to the polymerizable silicone resin raw material as appropriate.
- it can be appropriately adjusted so as to be plastic, which is a liquid, a grease, or a plastic as defined by plasticity.
- the resist ink used for spraying, dispenser, or screen printing is preferably liquid and has a viscosity of 0.5 to 500 Pa ⁇ s, more preferably 10 to 200 Pa ⁇ s.
- the plasticity based on international standard ISO 7323 is preferably used as a raw material composition as a millable type or plastic material of 100 to 500 mm / 100.
- silicone rubber powder and white inorganic filler When silicone rubber powder and white inorganic filler are used, 3 to 400 parts by weight, preferably 50 to 300 parts by weight are added to 100 parts by weight of the silicone resin raw material in order to adjust viscosity and hardness. Is preferred. If the addition amount of the white inorganic filler is less than this range, sufficient reflection cannot be obtained, and conversely, if the addition amount of the white inorganic filler is more than this range, the workability deteriorates. When the silicone resin raw material composition is applied thinly, the greater the amount of white inorganic filler added, the higher the reflectivity, whereas when it is applied thickly, it is sufficient that the amount added is small. Reflectance is obtained. The silicone rubber powder is added with the white inorganic filler within the above range.
- the organic solvent may be added for storage stability, coating property improvement, coating amount control, viscosity adjustment and the like.
- an organic solvent it is preferably added in an amount of 100 to 10,000 parts by mass with respect to 100 parts by mass of the silicone resin raw material. If the amount of the organic solvent is less than this range, stringing and clogging may occur during application and printing, resulting in decreased productivity. On the other hand, when the organic solvent is larger than this range, thick coating cannot be performed, or sufficient reflectance cannot be obtained once coating.
- the organic solvent is appropriately adjusted and used in accordance with various coating methods and required reflectance, film thickness, and viscosity. As the organic solvent, those that do not react with the silicone resin raw material, the crosslinking agent, and the reaction inhibitor are appropriately used.
- the addition concentration of the organic solvent relatively decreases the filling concentration of the white inorganic filler powder.
- the organic solvent evaporates after curing, the filling concentration of the white inorganic filler powder is increased before the viscosity adjustment. Since the density is restored, the coating thickness is thin and high density printing is possible.
- the reactive diluent is used especially for adjusting the viscosity of the one-pack type adhesive, and unlike an organic solvent, it does not volatilize and is cured as it is as a silicone resin.
- the reactive diluent include a reactive diluent for liquid silicone resin (trade name: ME91, manufactured by Momentive Materials Performance).
- the reactive diluent is used by adding 0.1 to 30 parts by weight, preferably 1 to 20 parts by weight, based on 100 parts by weight of the silicone resin raw material. If the amount added is too small, the viscosity cannot be adjusted. If the amount added is too large, the physical properties of the silicone resin will be weak. Since the reactive diluent is cured into a silicone resin, it does not cause volatilization and thinning after curing as in the case where a large amount of an organic solvent is used. Therefore, it is useful for forming a thick reflective layer.
- the amount of the organic solvent and the reactive diluent is appropriately adjusted according to the thickness of the reflective layer and the coating method such as printing / coating.
- a liquid or grease-like or plastic raw material composition containing a white inorganic filler powder in a polymerizable silicone resin raw material is a cross-linking agent for three-dimensional cross-linking to a silicone resin such as hydrogen organopolysiloxane or platinum group metal as described above.
- Cross-linking agents such as system catalyst-containing polysiloxanes and peroxides may be contained.
- the liquid, grease-like or plastic raw material composition containing the white inorganic filler powder in the polymerizable silicone resin raw material may contain a reaction inhibitor that is deactivated or volatilized by heating.
- the reaction inhibitor does not lower the activity of the catalyst added as necessary during storage of the raw material composition, and can perform addition reaction of a silicone resin raw material such as an alkenyl group-containing organopolysiloxane or organohydrogenpolysiloxane. It suppresses and enhances storage stability.
- Reaction inhibitors include, for example, methylvinylcyclotetrasiloxanes; 3-methyl-1-butyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, 3-methyl-1-pentene-3
- Acetylene alcohols such as ol and phenylbutynol
- acetylene compounds such as 3-methyl-3-penten-1-yne and 3,5-dimethyl-1-hexyne-3-yne
- these acetylene compounds and alkoxy Examples include siloxane-modified acetylene alcohols obtained by reacting silane, alkoxysiloxane, hydrogensilane, or hydrogensiloxane; nitrogen-containing organic compounds such as benzotriazole; organic phosphorus compounds; oxime compounds;
- this raw material composition can be stored for a long period of time because the three-dimensional crosslinking does not start before heating, while the three-dimensional crosslinking is quickly completed by heating, and the three-dimensional crosslinking is quickly completed and cured.
- a reflective layer is formed.
- the liquid or grease-like or plastic composition is diluted with an organic solvent, a uniform coating film is formed even if it is applied not only when the organic solvent is not volatilized but also when it is volatilized. Therefore, the reflective layer cannot be uneven.
- the crosslinking agent and reaction inhibitor are preferably contained in an amount of 0.01 to 10 parts by mass with respect to 100 parts by mass of the polymerizable silicone resin raw material.
- Such a raw material composition is also used as a resist.
- This raw material is a thermosetting resist, and is cured when heated to, for example, 100 ° C. or higher.
- the curing temperature can be appropriately adjusted by appropriately selecting a reaction inhibitor depending on its temperature dependency and crosslink initiation temperature controllability.
- the raw material composition may contain a crosslinking agent, a platinum catalyst, a reaction inhibitor, a reinforcing agent, and other various additives depending on the use in addition to the main component.
- This raw material composition may contain an adhesion-imparting component as an adhesive component.
- Adhesion imparting components include vinyl groups, phenyl groups, alkoxy groups, epoxy ring-containing groups such as 2,3-epoxypropyl groups (C 2 H 3 O—), and reactive functional groups such as (meth) acryloyl groups. Examples thereof include silane compounds and siloxane compounds having a group.
- the reflective base made of silicone resin formed using this it is preferable that 3 to 400 parts by mass of white inorganic filler powders 12a and 12b are contained with respect to 100 parts by mass of the silicone resin. It is more preferable that the white inorganic filler powder has an average particle size of 0.1 to 10 ⁇ m.
- Examples of the white inorganic filler powders 12a and 12b include titanium oxide, and more specifically, anatase type titanium oxide and rutile type titanium oxide. With or instead of titanium oxide, alumina, barium sulfate, magnesia, aluminum nitride, boron nitride (hexagonal and cubic), barium titanate, kaolin, silica, talc, powdered mica, powdered glass, powdered aluminum, Inorganic white pigments such as powdered nickel and calcium carbonate may be used in combination or may be used alone.
- the silicone resin contains a maximum amount capable of dispersing only an inorganic white pigment such as alumina or barium sulfate, there is a risk of light leakage, but with such an inorganic white pigment, titanium oxide has particularly high hiding power. Coexistence of rutile type titanium oxide is more preferable because light leakage is eliminated.
- heat conductive materials may be dispersed and filled in a silicone resin and laminated or placed as a part of the reflective base material of the present invention as a separate heat conductive layer or heat conductive member.
- the thermal conductivity was 1.2 W / m ⁇ ° C.
- the reflectance was 95% or more in the region of 450 to 1000 nm.
- A-42-6 100 parts by mass of alumina 100 parts by weight of silicone raw material 100
- a test piece having a size of 70 ⁇ 70 mm and a thickness of 0.8 mm was prepared by mixing with the mass part, and the thermal conductivity and the reflectance were measured.
- the thermal conductivity was 1.4 W / m ⁇ ° C.
- the reflectance was 450. It was 85 to 90% in the region of ⁇ 1000 nm.
- a test piece having a size of 70 ⁇ 70 mm and a thickness of 0.8 mm was prepared by mixing 200 parts by mass of alumina with 100 parts by mass of a silicone raw material, manufactured by Showa Denko Co., Ltd.
- the thermal conductivity was 1.9 W / m ⁇ ° C., and the reflectance was 75 to 80% in the region of 450 to 1000 nm. From this result, it was possible to improve the thermal conductivity while maintaining the reflectance of 90%. Moreover, it turned out that a reflectance and thermal conductivity can be adjusted by laminating
- the phosphor is included in the reflective layer to expose the particles from the surface and reflect the light directly or light.
- fluorescence or phosphorescence emitted when returning from the ground state to the ground state via the excited state may be emitted.
- an inorganic phosphor or an organic phosphor such as a halogenated phosphate phosphor, a rare earth metal-containing phosphor such as Eu, or a YAG (yttrium-aluminum-garnet) phosphor is used.
- reinforcing inorganic fillers such as silica, kaolin calcium carbonate, and zinc carbonate; reinforcing organic fillers such as silicone resin powder may be blended.
- Non-reinforcing inorganic fillers such as calcium silicate and titanium dioxide may be blended.
- the white inorganic filler powders 12a and 12b in the reflective base materials 10 and 20 made of silicone resin are more preferably titanium oxide, especially anatase-type titanium oxide, because the wavelengths of near-ultraviolet LEDs and blue LEDs are reflected.
- titanium oxide especially anatase-type titanium oxide
- the anatase-type titanium oxide is less than 3 parts by mass with respect to 100 parts by mass of the silicone resin, sufficient reflectivity cannot be obtained.
- it exceeds 400 parts by mass workability becomes difficult and productivity is lowered.
- the anatase type titanium oxide is contained in an amount of 30 to 300 parts by mass with respect to 100 parts by mass of the silicone resin.
- the anatase-type titanium oxide is not limited in shape, and may be any particle shape, for example, flaky, indeterminate or spherical particles, but the particle size is 0.05 to 50 ⁇ m, preferably 0.05 to
- the photocatalyst of titanium oxide is 30 ⁇ m, more preferably 0.1 to 10 ⁇ m. Since the organic oxidative decomposition reaction due to can be suppressed, it can withstand long-term use.
- the white titanium oxide powder particularly the anatase type titanium oxide powder, contained in the reflective base material 10 or 20 made of silicone resin has a much larger decomposition catalytic activity than the rutile type titanium oxide.
- Anatase-type titanium oxide powder is added to building materials such as tiles made of inorganic materials and outer wall materials, and acts as a powerful photolysis catalyst that decomposes adhering foreign matter such as dust adhering to the surface of the building material.
- polymer compounds such as thermoplastics such as polycarbonate, polyphthalamide, polyetheretherketone, it will decompose and yellow, or it will deteriorate and cause cracks. End up.
- silicone resins particularly silicone resins containing dimethylsiloxy repeating units as the main component
- the silicone resin reflective substrates 10 and 20 can be used for a long time. It does not change or deform like crossover yellowing.
- the surface of the anatase-type titanium oxide powder is treated with Al, Al 2 O 3 , ZnO, ZrO 2 , and / or SiO 2 , the decomposition catalytic activity is suppressed and yellowing occurs for a longer period of time. Such a change can be prevented, or the dispersibility in the silicone resin is improved and the reflectance of the reflective layer is further improved.
- the surface treatment is performed by kneading with titanium oxide and a raw powder of these surface treatment agents, or by dipping or spraying in a suspension containing the raw powder of these surface treatment agents.
- Commercially available surface-treated titanium oxide may be used. When titanium oxide is surface-treated, whiteness is enhanced and the reflectance of the reflective layer is further improved.
- the surface of the reflective layer of the reflective base made of silicone resin has an irregular shape of the order of 100 nm to 10 ⁇ m, a prismatic shape such as a pyramidal or prismatic shape, an etching treatment or a sandblast treatment, and the like. If the surface is non-specular, the incident light diffuses in all directions, improving the diffuse reflectance compared to reflection in a specific direction like a mirror surface, reducing light reflection unevenness, and increasing whiteness. The reflection efficiency is further improved.
- FIG. 11 shows anatase-type titanium oxide, Al 2 O 3 surface-treated with silane-coupled Al 2 O 3 in 100 parts by mass of silicone resin composed of only polydimethylsiloxane and only polyphenylsiloxane.
- silicone resin composed of only polydimethylsiloxane and only polyphenylsiloxane.
- the reflection base made of silicone resin in which 200 parts by mass of surface-treated rutile type titanium oxide and alumina (Al 2 O 3 ) are dispersed respectively the correlation between the irradiation wavelength and the reflectance thereof is FIG.
- the silicone resin reflective substrate made of polydimethylsiloxane having a low refractive index is any one containing anatase-type titanium oxide and rutile-type titanium oxide than those made of polyphenylsiloxane having a high refractive index.
- the reflectance is 3% higher over a wide range of wavelengths of 200 to 1000 nm, particularly 350 to 1000 nm.
- the reflective base made of silicone resin of either polydimethylsiloxane or polyphenylsiloxane has a wavelength of 400 nm and the reflectance of rutile-type titanium oxide-containing material is only about 30%, whereas it contains anatase-type titanium oxide.
- the reflectivity of the product is over 80%.
- those containing anatase-type titanium oxide have a reflectance as high as 40%, particularly at wavelengths of 380 to 420 nm, compared with those containing rutile-type titanium oxide.
- the reflectance of rutile titanium oxide is 6% higher.
- the refractive index of anatase type titanium oxide is 2.45 to 2.55, while the refractive index of rutile type titanium oxide is 2.61 to 2.90.
- the refractive index of alumina is about 1.76.
- Anatase-type titanium oxide has a higher refractive index than alumina, as does rutile-type titanium oxide, and thus exhibits a whiter color.
- Alumina has a lower refractive index than titanium oxide, but has high thermal conductivity and excellent heat dissipation.
- the reflective substrate made of alumina containing polydimethylsiloxane and silicone resin has a reflectance of 6 to 9% higher at a wavelength of 340 to 1000 nm than that of polyphenylsiloxane containing alumina.
- a conventional silicone resin composed only of polyphenylsiloxane containing alumina has a reflectance of about 80% at a wavelength of 400 nm or more and is not suitable as a reflective base material.
- the base polymer is a dimethyl such as polydimethylsiloxane.
- the reflectance becomes 90% or more at a wavelength of 400 nm or more, which is suitable as a reflective substrate.
- a white inorganic filler powder while using a silicone resin containing a dimethylsiloxy repeating unit as a main component, it is possible to have reflectivity and heat dissipation, but titanium was selected as the white inorganic filler powder.
- the improvement in reflectivity is emphasized, and in the case of selecting alumina, the improvement in heat dissipation is emphasized, and the reflective base material 10 made of silicone resin according to the intended use of adjusting the reflectivity and heat radiation by using in combination. 20 can be obtained.
- FIG. 12 shows a silicone resin reflective base material in which 200 parts by mass of anatase-type titanium oxide and rutile-type titanium oxide are dispersed and contained in 100 parts by mass of a silicone resin composed only of polyphenylsiloxane at 150 ° C. It is a figure which shows the correlation with an irradiation wavelength and its reflectance before and after heating for 1000 hours.
- the reflectance of the silicone resin composed only of the rutile titanium oxide-containing polyphenylsiloxane at a wavelength of 460 nm is 97%, whereas the silicone composed only of the rutile titanium oxide-containing polydimethylsiloxane.
- the reflectance of the resin is over 100%.
- the silicone resin composed only of polydimethylsiloxane has higher reflectance in the entire wavelength region than the silicone resin composed only of polyphenylsiloxane.
- the reflectance of the silicone resin consisting only of polydimethylsiloxane containing rutile-type titanium oxide also exceeded 100%.
- Reflective base materials 10 and 20 made of silicone resin are added using a liquid or grease-like or plastic raw material composition containing a silicone resin raw material, white inorganic filler powders 12a and 12b and, if necessary, a silane coupling agent. It is heat-cured in the absence of a solvent by reaction, and is formed on a support using a mold by a method such as compression molding, injection molding, transfer molding, injection molding (LIMS), extrusion molding, or calendar molding. . Such a liquid or grease-like or plastic composition may be applied while adjusting to an appropriate thickness of 1 to 2000 ⁇ m using a coater. In the case of a chip-on-board in which an electronic circuit is mounted by combining a chip and a device, this raw material composition is applied by a method such as screen printing, leaving a portion where the chip is mounted.
- a liquid or grease-like or plastic raw material composition containing a silicone resin raw material, white inorganic filler powders 12a and 12b and, if necessary, a silane
- silane coupling agent examples include those having an alkyloxy group, a vinyl group, an amino group, or an epoxy group as a reactive functional group.
- the coupling agent may be a titanate or aluminate coupling agent in addition to the silane coupling agent.
- the silicone resin takes in the white inorganic filler powder, for example, anatase-type titanium oxide, into the network structure more securely than when the silane coupling agent is not included. The strength of is significantly increased.
- the reflective substrate made of silicone resin containing white inorganic filler powder treated with silane coupling agent is cross-linked with silicone via silane coupling agent, so that the bending strength, wettability and dispersion The quality is improved and the quality is improved.
- a silane coupling treatment for example, 1% by mass of a silane coupling agent is added to anatase-type titanium oxide, and the surface treatment is performed by stirring with a Henschel mixer at 100 to 130 ° C. for 30 to 90 minutes. It is to dry.
- polishing is performed with abrasive cloths having a roughness of 500 to 10,000, for example, rubbing with a sandpaper, polishing with a fine particle-containing abrasive, polishing with a grindstone, or rubbing with a soft material such as cloth.
- the white inorganic filler is exposed on the surface of the silicone resin by performing buffing or by contacting the surface with embossed surfaces with irregularities such as a file while rotating at high speed.
- the roughening is performed by sandblasting or finishing with metal coarse particles, sand or abrasives, wet blasting by spraying a liquid in which abrasives are suspended, or scratching with a metal file.
- the reflection efficiency is further improved. Physical polishing is more preferred.
- FIG. 13 shows a silicone resin reflective group in which 100 parts by mass of anatase-type titanium oxide and rutile-type titanium oxide as a white inorganic filler powder are dispersed in 100 parts by mass of a silicone resin composed only of polydimethylsiloxane. It is a figure which shows the correlation with the irradiation wavelength before and behind grind
- these roughened silicone resin reflective base materials are either polydimethylsiloxane or polyphenylsiloxane, and whether the white inorganic filler powder is anatase-type titanium oxide or rutile-type titanium oxide. Regardless, the reflectance is as high as about 3% over a wide range of wavelengths from 200 to 1000 nm.
- the reflective base made of silicone resin conforms to JIS K7375, and when the standard white plate is 100, it also shows a relative reflectance value of about 100, indicating that the reflection efficiency is high.
- the reflective base made of silicone resin made only of polydimethylsiloxane containing rutile-type titanium oxide had a reflectance exceeding 100% and a very high reflection efficiency.
- the surface-roughened silicone resin reflecting base material is easy to adhere to a metal, and the metal film is easily attached to the surface of the silicone resin.
- the silicone resin reflective base material using the white inorganic filler subjected to the coupling treatment is easy to adhere to the metal, and the metal film is easily attached to the surface of the silicone resin.
- the metal film include plating films such as copper, silver, gold, nickel, and palladium, metal vapor-deposited films, adhesives, and metal foil films bonded by metal spraying.
- Silicon resin is usually difficult to adhere, so it is difficult to attach a metal film. However, if this silicone resin reflective substrate is used, the adhesion to the metal film is good.
- the metal film may be formed by directly plating on a reflective base made of silicone resin, vapor-depositing metal, or bonding a metal foil film with an adhesive.
- a reflective base made of silicone resin may be pre-corona-treated, plasma-treated, UV-treated, flame-treated, itro-treated, or coated with polyparaxylylene, and then coated with a metal film by vapor deposition or the like. Good.
- An example of the method for forming the metal film is as follows. A film is affixed as a masking material to a silicone resin reflective base material containing a white inorganic filler powder and formed into a plate shape.
- “Parylene C” which is a polyparaxylylene (trade name manufactured by Japan Parylene Co., Ltd .; “Parylene” is a registered trademark; — [(CH 2 ) —C 6 H 3 Cl— (CH 2 )] n ⁇ ),
- the powdered monochloroparaxylylene dimer that is the raw material dimer of “Parylene C” is placed in the vaporization chamber and heated under reduced pressure, and the evaporated dimer is induced in the thermal decomposition chamber and reacted.
- a radical of highly functional paraxylylene monomer After forming a radical of highly functional paraxylylene monomer, it is vapor-deposited on a reflective substrate and coated with a polyparaxylylene coating of 0.5 to 5 microns, preferably 1 to 2 microns to form an undercoat layer. To do. On the undercoat layer, a silver layer having a thickness of several microns is formed as a metal layer by vacuum deposition. Thereafter, when the masking material is peeled off, a reflective base made of silicone resin having a metal film attached and a small gas permeability coefficient and insulation resistance is obtained.
- metal plating or adhesion of a metal foil film may be used, and the preparation method thereof is not particularly limited.
- a reflective surface made of a silicone resin containing a white inorganic filler powder and formed into a plate shape is roughened using an acid or alkali, and then nickel plating is performed by electroless nickel plating. Then, copper plating is performed by electrolytic plating. Furthermore, gold or silver is plated according to the application.
- an adhesive layer is formed on the back surface of the copper foil, and the adhesive layer side is bonded to a reflective substrate made of a silicone resin containing a white inorganic filler powder and formed into a plate shape. It is heat-cured with a combined hydraulic press and cross-linked.
- the copper foil may be a roll-like continuous sheet or an individual sheet obtained by cutting it. The copper foil wound in the shape of a rolled roll may be pulled out and bonded to the reflective base made of silicone resin, and then rolled up again in a roll shape.
- a metal layer is provided on the support, a circuit is formed on the metal layer by etching, and the silicone resin raw material composition is applied by silk printing, except for the portion where the light emitting diode chip is connected and the portion where it is mounted.
- a gas barrier layer may be provided between the circuit and the silicone resin reflective substrate.
- the reflective base made of silicone resin consists of a three-dimensionally crosslinked silicone resin and inorganic filler powder, and therefore has higher gas permeability than ordinary resins such as epoxy resins, so that the metal layer of the circuit is corroded to form an oxide film. Therefore, peeling may occur between the reflective base made of silicone resin and the metal layer.
- a film having gas barrier properties may be formed between the reflective base made of silicone resin and the metal layer.
- the gas barrier layer may be flexible or inflexible.
- the thickness of the gas barrier layer is preferably 1 to 30 ⁇ m, and any material can be selected and used as long as it has a lower gas permeability than that of a silicone resin. Examples include ren coat, polyimide resin, polyparaxylylene, urethane resin, acrylic resin, and polyamide.
- Silicone resin is highly gas permeable and easily penetrates corrosive gas, so that the metal layer is corroded. Therefore, in order to prevent this, it is preferable to coat a gas barrier resin as a gas barrier layer and to provide a reflective base made of silicone resin thereon.
- Metal foil or metal plating may be applied on the silicone resin reflective base material.
- a silicone resin raw material composition may be applied to a copper foil and bonded to a substrate and etched to produce a pattern, or a silicone resin may be applied to a substrate and then plated.
- This silicone resin reflective base material has non-adhesiveness because the reflective layer uses a silicone resin. Therefore, if dust or foreign matter such as dust or dirt adheres to it, using an adhesive roller, the dust and foreign matter can easily adhere to the adhesive roll without sticking to the silicone resin reflective substrate. And removed. Moreover, although this silicone resin reflective base material is non-adhesive, it has high insulating properties, so that dust and foreign matters such as dust and dust are easily adsorbed and adhered by static electricity. Therefore, by coating a silicone hard coat layer on the reflective surface of the silicone resin reflective base material, it is possible to prevent these dusts and foreign substances from adhering. Moreover, even if dust / foreign matter adheres, it can be easily removed by blowing air. As a silicone hard coating agent that can be used for this silicone resin reflective substrate, a silicone hard agent in which silica or fluorine powder is dispersed, or a silicone coating agent used for air bag surface treatment can be used.
- a package case 10 which is a silicone resin reflective base material and a silicone resin reflective base material 20 include a silicone resin containing a dimethylsiloxy repeating unit as a main component in the main chain.
- the lighting fixture which is a light emitting device of an example containing anatase type titanium oxide particles will be specifically described.
- the reflective base material 20 made of silicone resin that forms a part of the wiring board is formed of a silicone resin containing anatase-type titanium oxide particles 12b. A part of the titanium oxide particles 12b is exposed from the surface on the mounting surface side to the light emitting diode 13 on the reflective base material 20 made of silicone resin. Copper films 15a and 15b, which are conductive metal films, are attached to the surface of the reflective base material 20 made of silicone resin to form a conductive pattern connected to a power source (not shown). Two lead wires 14a and 14b extending from the light emitting diode 13 are connected to the copper film 15a and the copper film 15b, respectively.
- the portions other than the conductive pattern portion on the surface of the reflective base material 20 made of silicone resin are exposed to the silicone resin, and a part of the anatase-type titanium oxide particles 12b is exposed there, and thus white color is exhibited. Moreover, since it has an excellent concealing property, light is not leaked and leaked. In addition, the reflectance of light, particularly not only in the wavelength region of 380 to 420 nm but also in the visible region longer than that, and heat rays such as infrared rays having longer wavelengths is extremely high.
- the package case 10 is also molded from a raw material composition containing the same kind of anatase-type titanium oxide particles 12a in a silicone resin.
- the package case 10 surrounds the light emitting diode 13 and is opened toward the emission direction by an inclined inner wall 11, and is disposed on the mounting surface side of the light emitting diode 13 on the silicone resin reflective base material 20 of the wiring board.
- the surface is integrally bonded via an adhesive layer (not shown).
- This package case body 10 also exhibits white color due to the anatase-type titanium oxide particles 12a and has excellent concealing properties, so that light does not leak, and light, particularly light having a wavelength of 380 nm or more, particularly 400 nm or more.
- the reflectivity is extremely high.
- Both the silicone resin reflective substrate 20 and the package case 10 are three-dimensionally cross-linked while containing an acyclic dimethylsiloxy repeating unit as a main component in a main chain such as polydimethylsiloxane which is chemically stable and hardly discolored. Because it is made of silicone resin, it has high reflectivity, can remain white even when exposed to high-intensity light for a long time, has a high mechanical strength, and has excellent light and heat resistance. Because of its durability and weather resistance, it has excellent durability.
- a support 16 is attached to the surface on the non-mounting surface side of the light emitting diode 13 on the reflective base material 20 made of silicone resin, and the lighting fixture 1 is formed.
- a lighting fixture in which a plurality of sets of the silicone resin reflective base material 20 to which the light emitting diodes 13 are mounted and the package case 10 are arranged in an orderly manner may be used.
- the opening on the emission direction side of the package case 10 may be covered with a transparent plate or transparent film made of glass or resin.
- the transparent plate or transparent film may contain a pigment, a dye, a fluorescent agent, or a phosphorescent agent that converts the wavelength of the transmitted light to a desired wavelength.
- the opening on the emission direction side of the package case 10 may be covered with a lens such as a convex lens, a concave lens, or a Fresnel lens (not shown).
- the silicone resin reflective base material 20 is formed on the support 16 by various printing such as screen printing, spraying, brush coating, coating, and the like.
- Such a support 16 may have any shape such as a non-deformable hard or rigid film shape, a plate shape, a cylindrical shape such as a cylinder, a spherical shape, or a three-dimensional shape such as a bowl. It may be a flexible and flexible sheet such as a circuit (FPC), a hard sheet that is energized when bent, or a roll that can be wound, and can be used for various elements. It may be a small working chip that is built in and does not take up much area.
- the support may be conductive, or may have thermal conductivity and heat dissipation.
- the front surface may have a reflective layer, and if necessary, the back surface may have an adhesive layer / adhesive layer.
- the support 16 may be an organic material or an inorganic material. Silicone resin, imide resin, bismaleimide / triazine resin, glass fiber-containing epoxy resin (glass epoxy), paper phenol resin, bakelite, polyethylene terephthalate resin, polybutylene terephthalate resin Polyacrylonitrile resins, plastic films include polycarbonate resins, fluorine resins, polyimide resins, polyphenylene sulfide resins, aramid resins, polyether ether resins, polyether imide resins, liquid crystal polymers, polyether sulfone resins, cycloolefin resins, silicone resins , And silicone rubber, aluminum foil, copper foil, nickel foil and the like molded as raw materials, but are not limited thereto.
- the reflective base material 20 made of silicone resin that forms a part of the wiring board contains an expensive silicone resin containing a dimethylsiloxy repeating unit as a main component in the main chain, but is only thinly attached to the inexpensive support 16. And because it has a sufficient reflection effect, it contributes to the reduction of production costs.
- the film-shaped silicone reflective substrate is applied on the support 16 as a 10-200 ⁇ m film by applying the raw material-containing composition.
- the wiring board having the package case 10 and the silicone resin reflective base material 20 is used as follows.
- the cathode side copper film 15a and the lead wire 14a, and the anode side copper film 15b and the lead wire 14b are applied to the light emitting diode 13
- the light emitting diode 13 emits light.
- Part of the emitted light is directly irradiated to the outside through the opening on the emission direction side of the package case 10.
- Another part of the emitted light is reflected from the inner wall 11 of the package case 10 or the portion of the reflective base material 20 made of silicone resin other than the conductive pattern on the surface of the wiring board, and from the opening on the emission direction side to the outside Is irradiated.
- the wiring substrate 21 is made of titanium oxide particles 12 c that are white inorganic filler powder having a high refractive index.
- the silicone resin contained is molded with the glass cloth 22 inside, and the conductive patterns of the copper films 15a and 15b, which are conductive metal films, are formed on the surface, and the lead wires 14a and 14b of the light emitting diode 13 are formed.
- the copper film 15a and the copper film 15b are connected to each other.
- Another embodiment of the reflective base material 1 made of silicone resin is used by being mounted on another lighting fixture as shown in FIG. 3 (d), and conductive metal films 15a and 15b, such as a copper film, forming a conductive line pattern,
- a package case 10 serving as a reflective layer formed of a silicone resin containing titanium oxide particles 12 which is a white inorganic filler powder having a high refractive index is attached on a support 16 formed of a suitable material such as rigid plastic.
- the support 15 and the copper films 15a and 15b are covered as a reflective base made of silicone resin.
- a conductive metal film 15a that forms a conductor pattern of a desired shape by printing, chemical etching, or the like on a support 16 such as a glass epoxy substrate in which a glass fiber cloth is impregnated with an epoxy resin.
- a support 16 such as a glass epoxy substrate in which a glass fiber cloth is impregnated with an epoxy resin.
- -Form 15b Next, a liquid or grease-like or plastic composition of the polymerizable silicone resin raw material is applied so as to cover the support 16 and the conductive metal films 15a and 15b, and the mold 31 having a large number of substantially hemispherical protrusions is used.
- the polymerizable silicone resin raw material When heated so that the thick part is 100 to 1000 ⁇ m and the thinnest part is 10 to 100 ⁇ m, the polymerizable silicone resin raw material is cured while being three-dimensionally cross-linked, and the package case 10 also serving as a reflective layer is obtained.
- the support 16 and the conductive metal films 15a and 15b are formed in close contact with each other.
- the mold 31 is released from the package case 10, the inner wall 11 formed in the released part becomes a reflective surface.
- a hole 32 is formed in the thinnest part of the package case 10 until reaching the conductive metal films 15a and 15b. As shown in FIG.
- a light emitting diode is inserted therein, and the negative and positive terminals are appropriately connected to the conductive metal films 15a and 15b with a connecting material such as solder. If necessary, a light emitting diode chip for a lighting fixture is formed by cutting the dicing saw 33 into a predetermined size.
- a sandblast surface treatment is performed.
- the mold 31 is heated while being pressed, the raw material for the polymerizable silicone resin is cured while being three-dimensionally crosslinked, and the reflective base material 20 made of a silicone resin that also serves as a reflective layer is formed.
- the support sheet is pulled out from the flexible support sheet raw material roll provided with the conductive metal film 15a / 15b having a conductor pattern of a desired shape, and applied to the surface on the conductive metal film 15a / 15b side.
- the polymerizable silicone resin raw material was cured while being three-dimensionally cross-linked by heating while being pressed with a roller 35 subjected to sandblasting, and also served as a reflective layer A reflective base material 20 made of silicone resin is formed. If necessary, it may be cut into a desired size with a dicing saw 33.
- the reflective base material 20 made of silicone resin as shown in FIGS. 4 to 5 has a slightly tapered grinder 36 as shown in FIG. 6A or a substantially hemispherical grinder 36 as shown in FIG. While rotating, until the conductive metal films 15a and 15b are exposed, they are cut in the thickness direction so as to form a recess in the package case, and then, if necessary, to a lighting fixture (not shown) by mounting a light emitting diode or the like. You may lead. As shown in FIG. 6C, while rotating the disc-shaped grinder 36, the conductive metal films 15a and 15b may be cut along a groove shape until they are exposed.
- the reflective base material 20 made of silicone resin is cut and polished until the conductive metal films 15 a and 15 b are reached while rotating the roller-shaped grinder 36 at a high speed, and the conductive metal is formed on the support 16.
- the films 15a and 15b and the reflective base 20 made of a silicone resin to be a reflective layer may be exposed without being spaced apart.
- the reflective base material 1 made of silicone resin has the light emitting diodes 13 as light emitting elements connected to the conductive metal films 15 a and 15 b of the conductor pattern having a desired shape attached to the support 16.
- the raw material of the polymerizable silicone resin that has flowed out from the nozzle 34 may be dropped and molded so as to surround and swell it.
- the silicone resin reflective base material 1 is spray-coated with a polymerizable silicone resin raw material on the surface of the support 16 that also serves as a package case having a depression, and then heated, You may form the reflective base material 20 made from a silicone resin.
- a mold release agent for example, die-free (manufactured by Daikin Industries, Ltd.) every time the mold is released from these molds when the reflective substrate 1 made of a silicone resin is formed, or every several to 10 times. May be applied to the mold to further improve the releasability.
- the reflective base made of silicone resin is incorporated as an assembly of the solar cell 2 as shown in FIG. 10, and is used in the package case 10 to which the photoelectric conversion element as the solar cell element 17 is attached.
- the package case 10 is a silicone resin containing anatase-type titanium oxide particles 12a, and is formed by arranging a plurality of rows that are recessed in a bowl shape.
- the solar cell element 17 includes a substantially spherical p-type silicon semiconductor 17a inside and an n-type silicon semiconductor 17b covering the periphery thereof and PN-junctioned. The lower end of the n-type silicon semiconductor 17b is missing due to polishing, and the p-type silicon semiconductor 17a is exposed therefrom.
- the n-type silicon semiconductor 17b is connected only to the copper film 18b that is the negative electrode element layer, while the p-type silicon semiconductor 17a is connected only to the copper film 18a that is the positive electrode element layer.
- the copper films 18a and 18b, which are both electrodes, are isolated and insulated by an insulator layer 19 stacked between them.
- the package case 10 surrounds the solar cell element 17 and opens toward the emission direction by the inner wall 11 that is recessed in a bowl shape, and is integrated with the copper film 18b through an adhesive layer (not shown). It is glued.
- the silicone resin reflective base material that is the package case 10 is used as follows. As shown in FIG. 10, light, for example, sunlight is incident on the solar cell element 17 of the solar cell assembly 2. For example, incident sunlight from directly above enters the top of the solar cell element 17 perpendicularly and perpendicularly. Incident sunlight slightly off from directly above is reflected by the inner wall 11 of the package case 10 and enters the side surface of the solar cell element 17 substantially perpendicularly. In this way, the light incident on the solar cell assembly 2 efficiently reaches the PN junction interface between the n-type silicon semiconductor 17b and the p-type silicon semiconductor 17a to generate a photovoltaic force. Flowing.
- the surface of the silicone resin of the silicone reflective substrate 20 as shown in FIGS. 1 to 10, that is, the surface on the side of the mounting surface to the light emitting diode 13 on the wiring board, and the surface of the inner wall 11 of the package case 10 are polished.
- Surface treatment is performed by roughening and / or chemical etching, and some of the white inorganic filler particles may be exposed from the surface of the silicone resin.
- the package case 10 and the surface on the mounting surface side of the light emitting diode 13 on the reflective base material 20 made of silicone resin of the wiring board are integrally bonded via an adhesive layer.
- the silicone resin adhesive include low molecular siloxane cut product SE-9186L (manufactured by Toray Dow Corning Co., Ltd .; trade name).
- the reflective base made of silicone resin is used to reflect light like a solar cell in addition to various light emitting devices such as lighting fixtures such as desk lamps with general incandescent bulbs, halogen lamps and LEDs. Alternatively, it may be applied to a wall or a fixture near a heat source such as an electric stove or a combustion stove to reflect infrared rays to increase the heating efficiency or to protect the wall or fixture against heat.
- the following shows an example in which the silicone resin reflective substrate of the present invention is prototyped and incorporated in the apparatus.
- Example 1 Comparison of initial reflectance (comparison between polyphenylsiloxane resin and polydimethylsiloxane resin) Anatase-type titanium oxide (trade name A-) using polyphenylsiloxane resin (trade name XE14-C2508: Momentive Performance Materials) and polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials) 950: Sakai Chemical Industry Co., Ltd.), rutile type titanium oxide (trade name GTR-100; Sakai Chemical Industry Co., Ltd.) and alumina (trade name AES12: Sumitomo Chemical Co., Ltd.) were added in an amount of 200 parts by mass, respectively, and 25 ⁇ m.
- a reflective base made of a silicone resin which is a white silicone reflector having a length of 70 mm, a width of 70 mm, and a thickness of 0.3 mm, was prepared on a support using a heating press at 150 ° C. for 10 minutes.
- Each reflectance was measured using a spectrophotometer UV-3150 (manufactured by Shimadzu Corporation). From FIG. 11 showing the results, in all cases, when polydimethylsiloxane was used as the base polymer, the reflectance was improved by 3 to 5%.
- Example 2 Reflectance after aging at high temperature Polyphenylsiloxane resin (trade name XE14-C2508: Momentive Performance Materials) and polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials) anatase titanium oxide (Trade name A-950: manufactured by Sakai Chemical Industry Co., Ltd.) and rutile-type titanium oxide (trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd.) were added in an amount of 200 parts by mass, respectively. A reflective layer was formed on the support under curing conditions at 150 ° C.
- a reflective base made of silicone resin which was a silicone white reflective plate having a length of 70 mm, a width of 70 mm, and a thickness of 0.3 mm, was produced.
- the reflectance after heating for 1000 hours at 150 ° C. was measured using a spectrophotometer UV-3150 (manufactured by Shimadzu Corporation). From FIG. 12, which shows the result, the silicone white reflector made of polyphenylsiloxane resin shows a decrease in reflectance on the short wavelength side, whereas the silicone white reflector made of polydimethylsiloxane resin shows a decrease in reflectance. Absent.
- Example 3 Polydimethylsiloxane resin (trade name: IVSM4500: manufactured by Momentive Performance Materials), anatase type titanium oxide (trade name: A-950: manufactured by Sakai Chemical Industry Co., Ltd.) and rutile type titanium oxide (trade name: GTR-100; 100 parts by mass of each (made by Chemical Industry Co., Ltd.) was added, and a reflective layer was formed by heating press at 150 ° C. for 10 minutes under a curing condition, and a silicone white reflector having a length of 70 mm, a width of 70 mm, and a thickness of 0.3 mm A silicone resin reflective substrate was prepared.
- IVSM4500 manufactured by Momentive Performance Materials
- anatase type titanium oxide trade name: A-950: manufactured by Sakai Chemical Industry Co., Ltd.
- rutile type titanium oxide trade name: GTR-100; 100 parts by mass of each (made by Chemical Industry Co., Ltd.
- each silicone white reflector After measuring the initial reflectivity of each reflectivity using a spectrophotometer (trade name UV-3150; manufactured by Shimadzu Corporation), the surface of each silicone white reflector is polished with # 1500 sandpaper, Measure the reflectance again. From FIG. 13 showing the result, the reflectance was improved by 2 to 3% by performing surface processing by polishing or the like.
- the polyphenylsiloxane resin reflector has a sufficient reflectance. Further, when polydimethylsiloxane is used as a base polymer, the reflectance is higher than when polyphenylsiloxane is used as a base, and further, no reduction in reflectance is observed even after 1000 hours. Since it does not yellow or deteriorate from this, it has been found that it is excellent in light resistance, heat resistance and weather resistance, and is a useful reflective material. Moreover, it turned out that a reflectance improves by surface-treating.
- Example 4 100 parts by mass of rutile titanium oxide (trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd.) is added to 100 parts by mass of silicone resin in polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials). Then, a reflective layer was formed on a 25 ⁇ m polyimide support under a heating condition at 150 ° C. for 10 minutes by a heating press, and a white silicone resin reflective substrate having a length of 70 mm, a width of 70 mm, and a thickness of 50 ⁇ m was produced. .
- rutile titanium oxide trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd.
- silicone resin in polydimethylsiloxane resin trade name IVSM4500: manufactured by Momentive Performance Materials
- Comparative Example 1 Except having used the epoxy resin composition which added 100 mass parts of rutile type titanium oxide (brand name GTR-100; Sakai Chemical Industry Co., Ltd.) with respect to 100 mass parts of epoxy resins, it carried out similarly to Example 4, and using. An epoxy resin white reflective sheet was prepared.
- rutile type titanium oxide brand name GTR-100; Sakai Chemical Industry Co., Ltd.
- the heat resistance test was performed on the silicone resin reflective substrate of Example 4 and the reflective sheet of Comparative Example 1 in the same manner as in Example 2.
- the reflectance before heating and after 1000 hours of heating at 150 ° C. was measured using a spectrophotometer UV-3150 (manufactured by Shimadzu Corporation).
- the result is shown in FIG.
- the epoxy resin white reflective sheet has a lower reflectance than the reflective substrate made of polydimethylsiloxane resin in the entire wavelength region.
- the epoxy resin white reflective sheet subjected to heating has a significant decrease in reflectance on the short wavelength side, whereas the polydimethylsiloxane resin reflective substrate does not have a decrease in reflectance.
- Example 5 As a support, a 15 ⁇ m copper plating was applied to a 25 ⁇ m polyimide film. A circuit was formed by etching using a photoresist. Next, the composition of anatase-type titanium oxide is changed in the range of 150 to 200 parts by mass with respect to 100 parts by mass of the silicone resin, and if necessary, silicone rubber powder is added in an appropriate amount to each raw material for the white reflector containing anatase-type titanium oxide. This is a composition, and this is applied to the surface of the circuit except for the portion where the LED chip and the wiring are to be applied, using screen printing to a thickness of 30 ⁇ m, and heated at 150 ° C.
- the reflective base material made of silicone resin had a reflective layer hardness of 80 with a JIS A type hardness meter and 70 with a JIS D type hardness meter.
- Example 6 As a support, a 15 ⁇ m copper plating was applied to a 25 ⁇ m polyimide film. A circuit was formed by etching using a photoresist. On the entire surface of the circuit, including the LED chip and the copper plating part for wiring thereof, the composition of anatase-type titanium oxide is changed in the range of 150 to 200 parts by mass with respect to 100 parts by mass of the silicone resin, and silicone rubber powder is added if necessary. An appropriate amount of each was added to form a raw material composition for anatase-type titanium oxide-containing white reflective material, which was applied at a thickness of 30 ⁇ m using screen printing, and heated at 150 ° C. for 1 hour to form a reflective layer.
- the hardness of the reflective layer was 70 according to JIS D type hardness tester.
- the reflective layer was ground until the copper plating was exposed, and a white reflective base made of silicone resin in which the copper plating portion and the silicone resin portion were separated was produced.
- Example 7 As a support, a 15 ⁇ m copper plating was applied to a 25 ⁇ m polyimide film. A circuit was formed by etching using a photoresist for the copper plating. Except for the part where the LED chip and the wiring are connected to the surface of this circuit, polyimide varnish (trade name; FC-114 fine polyimide varnish: manufactured by Fine Chemical Japan Co., Ltd.) is applied twice and cured by heating to form a gas barrier with a film thickness of 4 ⁇ m. A layer was provided. Thereafter, a white reflective base material made of silicone resin (the hardness of the reflective layer was the same) was produced in the same manner as in Example 5.
- FC-114 fine polyimide varnish manufactured by Fine Chemical Japan Co., Ltd.
- Example 8 100 parts by mass of rutile titanium oxide (trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd.) is added to a silicone adhesive (trade name X-32-1964, manufactured by Shin-Etsu Chemical Co., Ltd.), and acetylene is used as a reaction inhibitor. 0.01 parts of alcohol was added to obtain a liquid raw material composition (viscosity 600 Pa ⁇ s) used for a silicone resin reflective substrate. After the storage can was opened, it was left at room temperature for 7 days and the viscosity was measured. As a result, no change was observed, no precipitation of titanium oxide was observed, and even in heat curing at 150 ° C. for 1 hour, both reflectivity and hardness were initial. It showed the same characteristics as those of the raw material composition, showed long-term storability, was able to mount LEDs as shown in FIG. 1, and was found to be excellent in productivity in mass production.
- Example 9 As a chip-on film (hereinafter referred to as COF), a circuit is formed on a conductor (copper foil) having a thickness of 8 ⁇ m on a polyimide film having a thickness of 38 ⁇ m, and a polyimide varnish (trade name; FC-) is formed as a gas barrier layer excluding the land pattern portion.
- FC- polyimide varnish
- 114 fine polyimide varnish (made by Fine Chemical Japan Co., Ltd.) was applied twice and heat-cured to provide a gas barrier layer having a film thickness of 4 ⁇ m, and then screen printing was used to remove the land pattern portion and the white inorganic filler-containing raw material composition to 30 ⁇ m. It was applied and cured at 150 ° C.
- the white inorganic filler-containing raw material composition is composed of 100 parts by mass of polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials) and anatase-type titanium oxide (trade name A-950: manufactured by Sakai Chemical Industry Co., Ltd.) and rutile. 80 parts by mass of type titanium oxide (trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd.) is added.
- a white LED package NSSW064 made by Nichia Chemical was directly mounted on the land portion on the reflective base made of silicone resin, and was soldered through lead-free reflow to obtain a flexible LED lighting substrate of a high reflection COF substrate.
- This substrate was thin and could be inserted into a narrow part, and was not yellowed by heat, resulting in a COF with a reflectance of 98%. Also, no peeling between the metal and the reflective layer was observed.
- Example 10 After preparing the silicone resin raw material composition, low molecular weight polysiloxane having a siloxy group repeating unit of 4 to 10 was maintained under reduced pressure and / or 200 ° C. until it became less than 300 ppm, and then returned to normal pressure and used. Except for the above, a silicone resin reflective base material was produced in the same manner as in Examples 1 to 10, and each LED was mounted to manufacture an LED lighting board. As a result, electrical contact failure, illuminance reduction due to clouding, etc. The phenomenon was not observed.
- Example 11 A reflective substrate made of silicone resin was prepared in the same manner as in Example 1 except that titanium oxide was immersed in the reactive group-containing polysiloxane represented by the chemical formula (1) as a silane coupling agent and surface-treated. As a result, the bending strength and hardness of the resin-made reflective base material were improved as in the case shown in Table 1 above, compared with the case where the surface treatment was not performed.
- Example 12 After the circuit was formed in the same manner as in Example 9, the titanium oxide-containing dimethyl silicone resin raw material composition was applied by screen printing except for the land pattern portion that fits in ⁇ 1 mm, cured at 150 ° C. ⁇ 1 hour, and finer with ⁇ 1 mm It was possible to form a reflective layer without sagging into a land pattern.
- Example 13 After the circuit was formed in the same manner as in Example 9, the titanium oxide-containing dimethyl silicone resin raw material composition was applied by screen printing except for the land pattern portion that fits in ⁇ 1 mm, cured at 150 ° C. ⁇ 1 hour, and finer with ⁇ 1 mm It was possible to form a reflective layer without sagging into a land pattern. Further, when the reflectance of the substrate on which the surface was polished with sandpaper # 1000 and the titanium oxide powder was exposed was measured, an improvement in reflectance of 3% was observed.
- Example 14 After the circuit was formed in the same manner as in Example 9, the raw material composition of dimethyl silicone resin containing 100 parts by mass of anatase titanium oxide and 3 parts by mass of YAG phosphor as an inorganic white filler powder except for the land pattern part that fits within 1 mm.
- the product was applied by screen printing, cured at 150 ° C. for 1 hour, and a reflective layer could be formed without sagging into a fine land pattern of ⁇ 1 mm.
- the reflectance of the substrate on which the surface was polished with sandpaper # 1000 and the inorganic white filler powder was exposed was 90%. Absorption at 400 to 500 nm was confirmed and the reflectivity was reduced accordingly, but sufficient reflectivity could be maintained and excitation light at 550 nm was confirmed.
- Example 15 As a support, a 25 ⁇ m polyimide film is subjected to a plasma treatment, a primer treatment is performed, and 200 parts by mass of anatase-type titanium oxide subjected to a surface treatment with alumina with respect to 100 parts by mass of a silicone resin is mixed and dispersed as 30 ⁇ m. On the opposite side of the support, a silicone adhesive was applied at 30 ⁇ m, a release sheet was laminated, heated at 150 ° C. for 1 hour, and a cover layer having a reflective layer and an adhesive layer. A film was obtained. The coverlay film was bonded to the FR-4 substrate provided with a circuit by making a hole so as to allow the land pattern to escape.
- Example 16 After preparing the silicone resin raw material composition, low molecular weight polysiloxane having a siloxy group repeating unit of 4 to 10 was maintained under reduced pressure and / or 200 ° C. until it became less than 300 ppm, and then returned to normal pressure and used. Except for the above, a reflective base made of silicone resin was prepared in the same manner as in Examples 1 to 15, and LED lighting substrates were manufactured by mounting LEDs, respectively. Such a phenomenon was not recognized.
- Example 17 A reflective substrate made of silicone resin was prepared in the same manner as in Example 1 except that titanium oxide was immersed in the reactive group-containing polysiloxane represented by the chemical formula (1) as a silane coupling agent and surface-treated. As a result, the bending strength and hardness of the resin-made reflective base material were improved as in the case shown in Table 1 above, compared with the case where the surface treatment was not performed.
- COB chip-on-board
- a circuit is formed on a glass epoxy substrate (FR-4 substrate) with a conductor thickness of 8 ⁇ m (copper foil), the land pattern portion is removed, and a gas barrier layer is coated with an epoxy resin at 150 ° C.
- the titanium resin-containing silicone resin raw material composition by screen printing (the silicone resin raw material composition is polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials) 100 parts by mass of anatase type Titanium oxide (trade name A-950: manufactured by Sakai Chemical Industry Co., Ltd.) and rutile type titanium oxide (trade name GTR-100; manufactured by Sakai Chemical Industry Co., Ltd., 80 parts by mass) were applied, and 150 ° C. ⁇ It was cured in 1 hour to obtain a reflective substrate having a COF silicone resin reflective layer. A white LED package NSSW064 made by Nichia was directly mounted on the film and soldered through lead-free reflow to obtain a highly reflective COB substrate.
- the silicone resin raw material composition is polydimethylsiloxane resin (trade name IVSM4500: manufactured by Momentive Performance Materials) 100 parts by mass of anatase type Titanium oxide (trade name A-950: manufactured by Sakai Chemical Industry Co., Ltd.
- a titanium oxide-containing silicone resin raw material composition is discharged as a reflective frame so as to surround the resin-enclosed bare chip by a dispenser at a height of 0.5 mm, and then cured at 150 ° C. for 1 hour to form a thick material.
- a highly reflective COB with a resin reflective frame was obtained.
- Example 8 A silicone resin raw material composition was formed in the same manner as in Example 7, and this was soldered to a conductive circuit on a 25 ⁇ m polyimide film support as a casing with an outermost diameter of 3 mm around a bare chip, in a donut shape with a height of 1 mm. Potting was provided to provide a highly reflective frame, and the corresponding portion of the chip was sealed with a transparent silicone resin to produce a reflective substrate. Although this reflective substrate was bent to a radius of curvature of 20 mm, no abnormal reflection occurred.
- the hardness of the potted portion was Shore D hardness of 70 according to JIS D type hardness tester.
- a liquid or plastic raw material composition made of a silicone resin containing a white inorganic filler powder having a higher refractive index than that of a silicone resin such as a silicone resin and titanium oxide is a support.
- a silicone resin containing a white inorganic filler powder having a higher refractive index than that of a silicone resin such as a silicone resin and titanium oxide is a support.
- it can be combined with a plate-like support.
- a liquid or plastic raw material composition made of silicone resin containing a white inorganic filler powder having a refractive index higher than that of a silicone resin such as titanium oxide is used as a bare chip casing, and the diameter is 4 mm or less. Even if it is used by potting in such a way that it does not take up an area, if the curvature radius of bending of the support is as large as 20 mm or more, it can be used for the substrate.
- the reflective substrate made of silicone resin of the present invention is mounted on a light emitting device such as a light emitting diode, a light emitting device such as an incandescent bulb, a halogen lamp, a mercury lamp, or a fluorescent lamp, and reflects the emitted light in a desired direction. In order to emit light to the light source, it is used for a wiring board or a package case mounted on the light emitting source.
- this silicone resin reflective substrate is mounted on a photoelectric conversion element such as a solar cell element, and is mounted on these photoelectric conversion elements in order to reflect incident light and collect it on the photoelectric conversion elements. Used for printed circuit boards and package cases.
- the method for producing a reflective substrate made of a silicone resin of the present invention is useful for producing these light emitting devices.
- the raw material composition of the present invention is useful for easily forming a reflective base made of silicone resin by coating, spraying, dipping, molding or the like.
- the raw material composition of the present invention can be stored stably at room temperature, it is put into a can and becomes a product as a resist ink. Moreover, it is useful for adjusting a viscosity suitably and forming a reflective layer.
Abstract
Description
R1 aSiO(4-a)/2
(式中、R1は非置換又は置換一価炭化水素基で、好ましくは炭素数1~10、特に1~8のものである。aは0.8~2、特に1~1.8の正数である。)
で示されるものが挙げられる。ここで、Rとしてはメチル基、エチル基、プロピル基、ブチル基等のアルキル基、ビニル基、アリル基、ブテニル基等のアルケニル基、フェニル基、トリル基等のアリール基、ベンジル基等のアラルキル基や、これらの炭素原子に結合した水素原子の一部又は全部がハロゲン原子で置換されたクロロメチル基、クロロプロピル基、3,3,3-トリフルオロプロピル基等のハロゲン置換炭化水素基、或いはシアノ基で置換された2-シアノエチル基等のシアノ基置換炭化水素基などが挙げられ、R1は同一であっても異なっていてもよいが、R1としてメチル基、特にジメチルシロキシ基を主成分となるようなメチル基であるものが、反射性発現、耐熱性・耐久性等の観点から好ましい。
R2-[Si(R3)2-O]b-[Si(R3)(R4)-O]c-R2
(R2は同一又は異なり前記R1で例示されたメチル基等の飽和炭化水素基若しくはフェニル基等の芳香族炭化水素基又は前記R1で例示されたアルケニル基、R3は同一又は異なり前記R1で例示された飽和炭化水素基若しくは芳香族炭化水素基、R4は前記R1で例示されたアルケニル基、b、cは正数)で模式的に示されるもので、ブロック共重合であってもランダム共重合であってもよいものである。
HdR5 eSiO(4-d-e)/2
(式中、R5はR1で例示された基、特に飽和炭化水素基、d及びeは、0<d<2、0.8≦e≦2となる数)で表されるものである。
具体的には、このようなオルガノハイドロジェンポリシロキサンの例としては、1,1,3,3-テトラメチルジシロキサン、1,3,5,7-テトラメチルテトラシクロシロキサン、1,3,5,7,8-ペンタメチルペンタシクロシロキサン等の末端にSi-H基を有するシロキサンオリゴマー;トリメチルシロキシ末端基含有メチルハイドロジェンポリシロキサン、トリメチルシロキシ末端基含有ジメチルシロキサン・メチルハイドロジェンシロキサン共重合体、シラノール末端基含有メチルハイドロジェンポリシロキサン、シラノール末端基含有ジメチルシロキサン・メチルハイドロジェンシロキサン共重合体、ジメチルハイドロジェンシロキシ末端基含有ジメチルポリシロキサン、ジメチルハイドロジェンシロキシ末端基含有メチルハイドロジェンポリシロキサン、ジメチルハイドロジェンシロキシ末端基含有ジメチルシロキサン・メチルハイドロジェンシロキサン共重合体のような主鎖の途中にSi-H基を有するホモポリマー又はコポリマーのハイドロジェンポリシロキサンが挙げられる。このようなオルガノハイドロジェンポリシロキサンは、R5 2(H)SiO1/2単位とSiO4/2単位とを含み、R5 3SiO1/2単位、R5 2SiO2/2単位、R5(H)SiO2/2単位、(H)SiO3/2単位又はR5SiO3/2単位を含んでいてもよいものである。
初期反射率の比較
(ポリフェニルシロキサン樹脂とポリジメチルシロキサン樹脂との比較)
ポリフェニルシロキサン樹脂(商品名XE14-C2508:モメンティブ・パフォーマンス・マテリアルズ)とポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)を用いて、アナターゼ型酸化チタン(商品名A-950:堺化学工業株式会社製)とルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)とアルミナ(商品名AES12:住友化学株式会社製)を各々200質量部添加し、25μmのポリイミドを支持体に加熱プレスにて、150℃で10分間の硬化条件によって、縦70mm、横70mm、厚さ0.3mmのシリコーン白色反射板であるシリコーン樹脂製反射基材を作製した。それぞれの反射率を、分光光度計UV-3150(株式会社島津製作所製)を用いて測定した。その結果を示す図11よりすべてにおいてポリジメチルシロキサンをベースポリマーとした場合3~5%の反射率の向上が見られた。
高温での経時後の反射率
ポリフェニルシロキサン樹脂(商品名XE14-C2508:モメンティブ・パフォーマンス・マテリアルズ)とポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)にアナターゼ型酸化チタン(商品名A-950:堺化学工業株式会社製)とルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)をそれぞれ200質量部添加し、加熱プレスにて、25μmのポリイミドの支持体に150℃で10分間の硬化条件によって反射層を形成し、縦70mm、横70mm、厚さ0.3mmのシリコーン白色反射板であるシリコーン樹脂製反射基材を作製した。150℃で1000時間、加熱経過後の反射率を、分光光度計UV-3150(株式会社島津製作所製)を用いて測定した。その結果を示す図12より、ポリフェニルシロキサン樹脂のシリコーン白色反射板は短波長側で反射率の低下が見られるのに対し、ポリジメチルシロキサン樹脂のシリコーン白色反射板は反射率の低下が見られない。
ポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)にアナターゼ型酸化チタン(商品名A-950:堺化学工業株式会社製)とルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)をそれぞれ100質量部添加し、加熱プレスにて、150℃で10分間の硬化条件によって反射層を形成し、縦70mm、横70mm、厚さ0.3mmのシリコーン白色反射板であるシリコーン樹脂製反射基材を作製した。それぞれの反射率を、分光光度計(商品名UV-3150;株式会社島津製作所製)を用いて初期反射率を測定した後、#1500のサンドペーパーでシリコーン白色反射板の表面をそれぞれ研磨し、再度反射率を測定する。その結果を示す図13より、研磨などで表面加工を行うことにより2~3%反射率が向上した。
ポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)にシリコーン樹脂100質量部に対してルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)を100質量部添加し、加熱プレスにて、25μmのポリイミドの支持体に150℃で10分間の硬化条件によって反射層を形成し、縦70mm、横70mm、厚さ50μmの白色のシリコーン樹脂製反射基材を作製した。
エポキシ樹脂100質量部に対してルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)を100質量部添加したエポキシ樹脂組成物を用いたこと以外は、実施例4と同様にして、エポキシ樹脂白色反射シートを作製した。
支持体として、25μmのポリイミドフィルムに15μmの銅めっきを施した。これにフォトレジストを用いて、エッチング加工により回路を形成した。次に、アナターゼ型酸化チタンをシリコーン樹脂100質量部に対して150~200質量部の範囲で配合を変え、必要によりシリコーンゴムパウダーを夫々適量ずつ加えてアナターゼ型酸化チタン含有白色反射材用の原材料組成物となし、これを回路の表面にLEDチップ及び配線を行う部分を除いて、スクリーン印刷を用いて30μmの厚みで塗布し、150℃×1時間加熱し、反射層を形成し、シリコーン樹脂製反射基材を作製した。このときシリコーン樹脂製反射基材は、反射層の硬度はJIS A型硬度計で80と、JIS D型硬度計で70の硬度とであった。
支持体として、25μmのポリイミドフィルムに15μmの銅めっきを施した。これにフォトレジストを用いて、エッチング加工により回路を形成した。回路の表面にLEDチップ及びその配線を行う銅めっき部分を含む全面に、アナターゼ型酸化チタンをシリコーン樹脂100質量部に対して150~200質量部の範囲で配合を変え、必要によりシリコーンゴムパウダーを夫々適量加えてアナターゼ型酸化チタン含有白色反射材用の原材料組成物となし、これを、スクリーン印刷を用いて30μmの厚みで塗布し、150℃×1時間加熱し、反射層を形成した。このとき反射層の硬さはJIS D型硬度計で70の硬度を有していた。次いで、図7に示すように、銅めっきが露出するまで反射層を研削し、銅めっき部分とシリコーン樹脂部分とが区分けされたシリコーン樹脂製白色反射基材を作製した。
支持体として、25μmのポリイミドフィルムに15μmの銅めっきを施した。この銅めっきにフォトレジストを用いて、エッチング加工により回路を形成した。この回路の表面にLEDチップ及びその配線を行う部分を除いてポリイミドワニス(商品名;FC-114 ファイン・ポリイミドワニス:ファインケミカルジャパン社製)を2回塗りして加熱硬化し膜厚4μmのガスバリアー層を設けた。しかる後、実施例5と同様にしてシリコーン樹脂製白色反射基材(反射層の硬度は同値)を作製した。
シリコーン接着剤(商品名X-32-1964:信越化学工業株式会社製)にルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)を100質量部添加しさらに反応抑制剤としてアセチレンアルコールを0.01部添加しシリコーン樹脂製反射基材に用いる液状の原材料組成物(粘度600Pa・s)を得た。この保存缶を開封後、室温において7日間放置し粘度を測定した結果変化が見られず、酸化チタンの沈降が見られず、150℃1時間の加熱硬化においても反射率、硬さとも初期の原材料組成物のものと同じ特性を示し、長期の保管性を示し、図1のようにLEDを実装でき、量産において生産性に優れていることが分かった。
一液型エポキシ樹脂性レジストインクにおいては、その保存缶の開封後、室温において24時間放置し確認した結果、外周が硬化し内部がゲル化し使用ができない状況であった。
チップオンフィルム(以下COFとする)として、厚さ38μmのポリイミドフィルムに厚さ8μmの導体(銅箔)に回路を形成し、ランドパターン部を除いてガスバリア層としてポリイミドワニス(商品名;FC-114 ファイン・ポリイミドワニス:ファインケミカルジャパン社製)を2回塗りして加熱硬化し膜厚4μmのガスバリアー層を設けたのち、スクリーン印刷により、ランドパターン部を除き白色無機フィラー含有原材料組成物を30μm塗布し、150℃×1時間で硬化させ、反射層を形成し、COFのシリコーン樹脂製反射基材を得た。白色無機フィラー含有原材料組成物はポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)100質量部にアナターゼ型酸化チタン(商品名A-950:堺化学工業株式会社製)とルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)を80質量部添加したものである。このシリコーン樹脂製反射基材に日亜化学製白色LEDパッケージNSSW064を直接ランド部の上にマウントし、鉛フリーリフローに通しハンダを行い、高反射COF基板のフレキシブルLED照明基板を得た。この基板は厚みが薄く狭い箇所に挿入可能であり、熱による黄変がなく反射率98%のCOFとなった。また、金属と反射層との剥離も認めれなかった。
シリコーン樹脂原材料組成物を調製後、シロキシ基繰返単位を4~10とする低分子量ポリシロキサンを300ppm未満になるまで、減圧下及び/又は200℃で維持した後、常圧に戻して用いたこと以外は、実施例1~10と同様にして、シリコーン樹脂製反射基材を作製し、夫々LEDを実装してLED照明基板を製造したところ、電気接点障害、くもりの発生による照度低下などの現象は、認められなかった。
酸化チタンを、前記化学式(1)で示される反応性基含有ポリシロキサンをシランカップリング剤として浸漬し、表面処理したこと以外は、実施例1と同様にして、シリコーン樹脂製反射基材を作製したところ、表面処理しない場合よりも、前記表1で示す場合と同様に、樹脂製反射基材の曲げ強度と硬度とが、向上していた。
(実施例12)
実施例9と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて酸化チタン含有ジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。
実施例9と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて酸化チタン含有ジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。更に、サンドペーパー#1000を用い表面を研磨し、酸化チタン粉末を露出させた基板の反射率を測定したところ、3%の反射率向上が見られた。
実施例9と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて無機白色フィラー粉末としてアナターゼ酸化チタンを100質量部、YAG蛍光体を3質量部含有させたジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。サンドペーパー#1000を用い表面を研磨し、無機白色フィラー粉末を露出させた基板の反射率を測定したところ90%であった。400~500nmの吸収が確認されその分反射率が低下したものの十分な反射率を維持できるとともに、550nmの励起光が確認された。
支持体として、25μmのポリイミドフィルムにプラズマ処理を行い、プライマー処理を行い反射層として、シリコーン樹脂100質量部に対してアルミナで表面処理を行ったアナターゼ型酸化チタン200質量部を配合し分散させ30μmの厚みで塗布し、その支持体の反対の面にはシリコーン粘着剤を30μmで塗工し、離型シートを積層し、150℃×1時間加熱し、反射層と粘着層を有したカバーレイフィルムを得た。このカバーレイフィルムを、回路を設けてあるFR-4基板にランドパターンを逃がすように穴を開け、位置を合わせて、貼り合わせた。
シリコーン樹脂原材料組成物を調製後、シロキシ基繰返単位を4~10とする低分子量ポリシロキサンを300ppm未満になるまで、減圧下及び/又は200℃で維持した後、常圧に戻して用いたこと以外は、実施例1~15と同様にして、シリコーン樹脂製反射基材を作製し、夫々LEDを実装してLED照明基板を製造したところ、何れも電気接点障害、くもりの発生による照度低下などの現象は、認められなかった。
酸化チタンを、前記化学式(1)で示される反応性基含有ポリシロキサンをシランカップリング剤として浸漬し、表面処理したこと以外は、実施例1と同様にして、シリコーン樹脂製反射基材を作製したところ、表面処理しない場合よりも、前記表1で示す場合と同様に、樹脂製反射基材の曲げ強度と硬度とが、向上していた。
チップオンボード(以下COBとする)として、ガラエポ基板(FR-4基板)に導体厚み8μm(銅箔)に回路を形成しランドパターン部を除き、ガスバリア層としてエポキシ樹脂でコーティングし150℃×4時間で硬化させたのち、スクリーン印刷により酸化チタン含有のシリコーン樹脂原材料組成物(シリコーン樹脂原材料組成物はポリジメチルシロキサン樹脂(商品名IVSM4500:モメンティブ・パフォーマンス・マテリアルズ社製)100質量部にアナターゼ型酸化チタン(商品名A-950:堺化学工業株式会社製)とルチル型酸化チタン(商品名GTR-100;堺化学工業株式会社製)を80質量部添加したもの)を塗布し、150℃×1時間で硬化させ、COFのシリコーン樹脂製反射層を有する反射基材を得た。そこに日亜化学製白色LEDパッケージNSSW064を直接フィルム上にマウントし、鉛フリーリフローに通しハンダを行い、高反射COB基板を得た。
製造例1と同様にしてCOBのシリコーン樹脂製反射層を有する基材を得た。そこにベアチップ(LED素子自体)を直接基板上のランドパターンに実装しワイヤー(金線)ボンディングし、シリコーン透明樹脂で封止を行い、ガラスエポキシLED照明基板を得た。この基板は熱による黄変もなく反射率98%のCOBとなった。
COBとしてBTレジン製基板(三菱ガス化学株式会社製)に導体厚み8μm(銅箔)を形成しランドパターン部を除き、ガスバリア層としてエポキシ樹脂を20μmコーティングし150℃×4時間で硬化させたのち、反射層をスクリーン印刷により塗布し、150℃×1時間で硬化させ、COBのシリコーン樹脂製反射層を有する基材を得た。そこにベアチップ(LED素子自体)を直接基板上のパターンに実装しワイヤー(金線)ボンディングしシリコーン透明樹脂で封止を行った。さらに、樹脂封止されたベアチップ周辺を囲むようにして反射枠として酸化チタン含有シリコーン樹脂原材料組成物をディスペンサーにより、高さ0.5mmで吐出したのち150℃×1時間で硬化させ厚物成形を行いシリコーン樹脂製反射枠付高反射COBを得た。
製造例1と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて酸化チタン含有ジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。
製造例1と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて酸化チタンジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。更に、サンドペーパー#1000を用い表面を研磨し、酸化チタン粉末を露出させた基板の反射率を測定したところ、3%の反射率向上が見られた。
製造例1と同様にして回路を形成した後、φ1mmに収まるランドパターン部を除いて無機白色フィラー粉末としてアナターゼ酸化チタンを100質量部、YAG蛍光体を3質量部含有させたジメチルシリコーン樹脂原材料組成物をスクリーン印刷により塗布し、150℃×1時間で硬化させ、φ1mmの微細なランドパターンにダレることなく反射層を形成することができた。サンドペーパー#1000を用い表面を研磨し、無機白色フィラー粉末を露出させた基板の反射率を測定したところ90%であった。400~500nmの吸収が確認されその分反射率が低下したものの十分な反射率を維持できるとともに、550nmの励起光が確認された。
支持体として、25μmのポリイミドフィルムにプラズマ処理を行い、プライマー処理を行い反射層としてシリコーン樹脂100質量部に対してアルミナで表面処理を行ったアナターゼ型酸化チタン200質量部を配合し分散させ30μmの厚みで塗布し、その支持体の反対の面にはシリコーン粘着剤を10μmで塗工し、熱伝導層として、50μmのアルミ箔を積層し、更に粘着剤を10μmで塗工し離型シートを積層し、150℃×1時間加熱し、反射層と粘着層を有したカバーレイフィルムを得た。このカバーレイフィルムを、回路を設けてあるFR-4基板にランドパターンを逃がすように穴を開け、位置を合わせて、貼り合わせた。
実施例7と同様にシリコーン樹脂原材料組成物となし、これを25μmのポリイミドフィルムの支持体上の導電回路に半田付けしたベアチップの周りに最外直径3mmのケーシングとして、高さ1mmでドーナッツ状にポッティングして高反射枠を設け、チップ該当箇所を透明シリコーン樹脂で封止し、反射基材を作製した。この反射基材を曲率半径20mmに撓ませたが反射異常は起きなかった。このポッティングした箇所の硬度は、JIS D型硬度計により、ショアD硬度で70であった
Claims (27)
- 三次元架橋したシリコーン樹脂に、それよりも高屈折率の白色無機フィラー粉末が分散されつつ含有された反射層が、支持体上で膜状、立体状又は板状に形成されていることを特徴とするシリコーン樹脂製反射基材。
- 前記シリコーン樹脂が、非環状のジメチルシロキシ繰返単位を主成分として含んでいることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記シリコーン樹脂中に含まれる、シロキシ基繰返単位を4~10とする低分子量ポリシロキサンが、最大でも300ppmであることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記反射層が、1~2000μmの厚さで形成されていることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記シリコーン樹脂が、屈折率を1.35以上、1.65未満とすることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記白色無機フィラー粉末が、酸化チタン、アルミナ、硫酸バリウム、マグネシア、チッ化アルミニウム、チッ化ホウ素、チタン酸バリウム、カオリン、タルク、炭酸カルシウム、酸化亜鉛、シリカ、マイカ粉、粉末ガラス、粉末ニッケル及び粉末アルミニウムから選ばれる少なくとも1種の光反射剤であることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記白色無機フィラー粉末が、シランカップリング処理されてシリコーン樹脂中に分散されたものであることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記白色無機フィラー粉末が、アナターゼ型若しくはルチル型の前記酸化チタン、前記アルミナ、又は前記硫酸バリウムであることを特徴とする請求項6に記載のシリコーン樹脂製反射基材。
- 前記酸化チタンが、Al、Al2O3、ZnO、ZrO2、及び/又はSiO2で表面処理されて被覆されていることを特徴とする請求項8に記載のシリコーン樹脂製反射基材。
- 前記白色無機フィラー粉末が、平均粒径0.05~50μmであって、前記シリコーン樹脂中に、2~80質量%含有されていることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記反射層に、前記白色無機フィラー粉末と蛍光体とが分散されつつ含有されていることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記反射層の表面に、前記白色無機フィラー粉末と前記蛍光体との少なくとも何れかが露出していることを特徴とする請求項11に記載のシリコーン樹脂製反射基材。
- 前記反射層の表面が連続して、ナノメートル乃至マイクロメートルオーダーの凹凸形状、プリズム形状、及び/又は梨地面形状の何れかの非鏡面となっていることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記シリコーン樹脂の少なくとも一部の表面の研磨、粗面化、ざらついた金型による金型成形若しくはスタンプ成形、及び/又はケミカルエッチングによって、前記白色無機フィラー粉末の一部が、前記表面から露出していることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 導電パターンの付された前記支持体を覆う前記反射層が研磨され、前記導電パターンが露出していることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 前記表面の上に、金属膜が付されていることを特徴とする請求項15に記載のシリコーン樹脂製反射基材。
- 前記金属膜が、銅、銀、金、ニッケル、及びパラジウムから選ばれる少なくとも何れかの金属で形成されていることを特徴とする請求項16に記載のシリコーン樹脂製反射基材。
- 前記金属膜が、めっき被膜、金属蒸着被膜、金属溶射膜、又は接着された金属箔膜であることを特徴とする請求項16に記載のシリコーン樹脂製反射基材。
- 発光素子、発光装置及び光電変換素子の何れかの背面、外周及び/又は導光材反射面に、配置されていることを特徴とする請求項1に記載のシリコーン樹脂製反射基材。
- 三次元架橋したシリコーン樹脂へと重合させる重合性シリコーン樹脂原材料に、前記シリコーン樹脂よりも高屈折率の白色無機フィラー粉末を分散させて原材料組成物とした後、前記原材料組成物を膜状に支持体上に付し、三次元架橋させて前記シリコーン樹脂へ重合させることにより、反射層を前記支持体上で膜状、立体状又は板状に形成することを特徴とするシリコーン樹脂製反射基材の製造方法。
- 前記重合が、加湿、加圧及び紫外線照射の少なくとも何れかにより、なされることを特徴とする請求項20に記載のシリコーン樹脂製反射基材の製造方法。
- 前記重合が、金型内での射出成形、又は金型での押圧成形の際加熱及び/又は加圧により、なされることを特徴とする請求項20に記載のシリコーン樹脂製反射基材の製造方法。
- 前記金型の表面が、フッ素樹脂でコーティングされていることを特徴とする請求項22に記載のシリコーン樹脂製反射基材の製造方法。
- 前記重合性シリコーン樹脂原材料に、前記シリコーン樹脂への三次元架橋の架橋剤と、加熱によって失活又は揮発する反応抑制剤とが、分散して含有されており、前記シリコーン樹脂よりも高屈折率の白色無機フィラー粉末を分散させて、前記原材料組成物となした後、前記加熱によって前記重合がなされることを特徴とする請求項20に記載のシリコーン樹脂製反射基材の製造方法。
- 重合性シリコーン樹脂の原材料と、前記シリコーン樹脂の原材料を三次元架橋させる架橋剤と、前記シリコーン樹脂よりも高屈折率の白色無機フィラー粉末とが含まれた液状又は塑性の原材料組成物であって、請求項1に記載のシリコーン樹脂製反射基材を形成するために用いられる原材料組成物。
- 加熱によって失活又は揮発する反応抑制剤が含まれていることを特徴とする請求項25に記載の原材料組成物。
- 粘度調整のための有機溶剤及び/又は反応性希釈剤が含まれていることを特徴とする請求項25に記載の原材料組成物。
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CN115418164A (zh) * | 2022-09-16 | 2022-12-02 | 南京奥创先进材料科技有限公司 | 一种高温热反射材料及其施工工艺 |
CN115418164B (zh) * | 2022-09-16 | 2024-03-26 | 奥创特新(苏州)科技有限公司 | 一种高温热反射材料及其施工工艺 |
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US20170114226A1 (en) | 2017-04-27 |
JP5770502B2 (ja) | 2015-08-26 |
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CN106025053B (zh) | 2020-01-10 |
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CN102893417B (zh) | 2016-06-15 |
US9574050B2 (en) | 2017-02-21 |
JP2017124632A (ja) | 2017-07-20 |
KR20130038847A (ko) | 2013-04-18 |
KR20170066684A (ko) | 2017-06-14 |
JP2020013142A (ja) | 2020-01-23 |
JP5836420B2 (ja) | 2015-12-24 |
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EP3490015A1 (en) | 2019-05-29 |
KR101853598B1 (ko) | 2018-04-30 |
JP6581695B2 (ja) | 2019-09-25 |
CN102893417A (zh) | 2013-01-23 |
JP5519774B2 (ja) | 2014-06-11 |
US10533094B2 (en) | 2020-01-14 |
JP6717512B2 (ja) | 2020-07-01 |
CN106025053A (zh) | 2016-10-12 |
WO2011118109A1 (ja) | 2011-09-29 |
JPWO2011118109A1 (ja) | 2013-07-04 |
JP2018180551A (ja) | 2018-11-15 |
JP2011221518A (ja) | 2011-11-04 |
HK1179048A1 (zh) | 2013-09-19 |
JP6157118B2 (ja) | 2017-07-05 |
US20200095430A1 (en) | 2020-03-26 |
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