CN101278213A - Reflecting material and reflector for light emitting diode - Google Patents
Reflecting material and reflector for light emitting diode Download PDFInfo
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- CN101278213A CN101278213A CNA2006800355125A CN200680035512A CN101278213A CN 101278213 A CN101278213 A CN 101278213A CN A2006800355125 A CNA2006800355125 A CN A2006800355125A CN 200680035512 A CN200680035512 A CN 200680035512A CN 101278213 A CN101278213 A CN 101278213A
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- reflecting material
- particle
- compound
- hollow
- resin
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Abstract
The invention provides a reflecting material having high reflectivity to ultraviolet rays and also having high reflectivity after heat treatment, and a reflector for LED. Which is composed of a polymer starting from a composition comprising the following and (b): 95-30% by mass of a thermally or photopolymerizable compound; (b) 5 to 70% by mass of hollow particles made of a material having an ultraviolet transmittance at a wavelength of 350nm of 50% or more.
Description
Technical field
The present invention relates to reflecting material and reflector for light-emitting diode.
Background technology
After nineteen ninety generation, the progress of light emitting diode (LED) is obvious, has made progress high outputization and multicolor.Wherein, White LED as an alternative in the past white electric ball, Halogen lamp LED, the follow-on light source of HID lamp be worth expectation.In fact, LED be evaluated as have the long-life, economize electric power, specialities such as temperature stability, low voltage drive, and be applied in display, destination display board, vehicle-mounted illumination, signal lamp, emergency condition lamp, mobile phone, the video camera etc.Described light-emitting device is usually by fixed L ED on the reflecting body that forms that synthetic resin and lead frame are shaped integratedly, and with seal, sealing materials sealing-ins such as epoxy resin or silicone resins and make.
Take out the luminous light of LED well for efficient, need LED reflection body material to have the high light reflectivity rate.In recent years, use the LED of blue outside line gradually, high reflectivity is also sought in ultraviolet ray.In addition, also there are sealing-in operation or solder operation etc. to be exposed to occasion under the high temperature sometimes.Therefore, even seek to be exposed under the high temperature, reflectivity does not reduce yet.
In polyamide-based resin, add the resin combination (for example, patent documentation 1) of titanium dioxide through being commonly used for the LED reflecting body.This material has high reflectivity in the visible region.Yet therefore the ultraviolet ray that the easy absorbing wavelength 400nm of titanium dioxide is following, contains the described material following ultraviolet ray of reflection wavelength 400nm hardly of titanium dioxide.Use potassium titanate fibre (patent documentation 2) if replace titanium dioxide, then improve ultraviolet reflection characteristic, but this also not enough (reflectivity under 350nm is about 30%)
On the other hand, in patent documentation 3, disclose when making the LED lamp, had the technology of the resin bed that contains the light reflective filler at the periphery of light-emitting component.As the light reflective filler, disclose the compound that titanium dioxide or potassium titanate etc. contain titanium and oxygen.Yet these fillers have the ultraviolet character of absorption, and are therefore, still extremely low to ultraviolet reflectivity.
In patent documentation 4, disclose and comprising the stacked light reflective film that contains the superficial layer of hollow-particle on the vibrin sheet of bubble.Disclose the reflectivity height of this film, and then group goes under the situation of LCD backlight lamp to improve brightness, but the ultraviolet reflection characteristic is not related to.For example, polyester has been selected as benchmark in the aspect that does not almost have with the absorption in the visible region.In addition, the size of LED lamp is the square degree of 5mm usually, and is very little, is difficult to described laminate film is gone in the LED lamp as the reflecting body group.And then, not open for the variation of the reflectivity in the heat treatment step that requires in the manufacturing of LED lamp, also not discussion.
Patent documentation 1: the spy opens flat 2-288274 communique
Patent documentation 3: the spy opens the 2000-150969 communique
Patent documentation 4: the spy opens the 2004-101601 communique
Summary of the invention
The object of the present invention is to provide ultraviolet ray is had high reflectivity, and after thermal treatment, also have the reflecting material and the LED reflecting body of high reflectivity.
According to the present invention as can be known, provide following reflecting material and LED reflecting body.
1. reflecting material, it is that the polymkeric substance of raw material constitutes by following to comprise (a) and composition (b):
(a) heat or optical polymerism compound 95～30 quality %;
(b) be hollow-particle 5～70 quality % that the material more than 50% constitutes by the ultraviolet ray transmissivity under the wavelength 350nm.
2. according to 1 described reflecting material, wherein,
Ultraviolet ray transmissivity under the wavelength 350nm of described heat or optical polymerism compound is more than 50%.
3. according to 1 or 2 described reflecting materials, wherein,
Described heat or optical polymerism compound are by one or more compounds that constitute that are selected from acrylic acid series compound, epoxy based compound, silicone compound.
4. according to each described reflecting material in 1～3, wherein,
Described hollow-particle is cross-linked resin or mineral compound.
5. according to each described reflecting material in 1～4, wherein,
Described hollow-particle is that cross-linked styrene is that resin, cross-linked acrylic acid are resin, unorganic glass or silica.
6. according to each described reflecting material in 1～5, wherein,
Also comprise: the luminous ray reflectivity under the wavelength 550nm is the matrix more than 80%, and is laminated with described to comprise (a) and (b) composition is the polymkeric substance of raw material on this matrix.
7. according to 6 described reflecting materials, wherein,
Described matrix is that to comprise entity particle (filled particles) be the resin combination of Chinese white.
8. according to 6 described reflecting materials, wherein,
Described matrix is by one or more metals that constitute that are selected from aluminium, gold, silver, copper, nickel or palladium.
9. reflector for light-emitting diode, it has each described reflecting material in 1～8 at reflecting surface at least.
10. according to 9 described reflector for light-emitting diode, wherein,
It is on the formed body that constitutes of the resin combination of Chinese white that described reflecting material is layered in by comprising the entity particle.
11. according to 9 described reflector for light-emitting diode, wherein,
Described reflecting material is layered on the formed body that is made of one or more metals that constitute that are selected from aluminium, gold, silver, copper, nickel or palladium.
According to the present invention as can be known, can provide ultraviolet ray is had high reflectivity, and after thermal treatment, also have the reflecting material and the LED reflecting body of high reflectivity.
Description of drawings
Fig. 1 is the chart that is illustrated in the reflectivity of the reflecting plate that obtains among the embodiment 2.
Fig. 2 is illustrated in the figure that the LED that makes among the embodiment 9 uses reflecting body, (a) be to contain the sputtering forming of resin combination that the entity particle is a Chinese white and the sectional view of the formed body that obtains, (b) be on the formed body of (a), LED to be installed, containing the polymerizable compound of hollow-particle and sectional view during polymerization in the inner coating of formed body, (c) is to drop into the sealing-in agent and sectional view when solidifying in recess.
Embodiment
Reflecting material of the present invention comprises: with the composition that contains heat and optical polymerism compound and hollow-particle is the polymkeric substance of raw material.
Heat or optical polymerism compound also can be one or more potpourri.When heat or optical polymerism compound preferred thickness are 250 μ m one by one is more than 50% to the ultraviolet ray transmissivity under the wavelength 350nm, more preferably 60%～100%.Also have, this ultraviolet ray transmissivity is the value to utilizing heat or photopolymerisable resin to measure.If the ultraviolet ray transmissivity height, the ultraviolet ratio that then sees through resin bed and arrive the gas blanket that forms on hollow-particle uprises, and is also uprised by the ultraviolet ratio of this gas blanket reflection.Like this, form the high reflecting material of ultraviolet reflection rate.
Ultraviolet ray transmissivity under the wavelength 350nm during as thickness 250 μ m is heat or the optical polymerism compound more than 50%, can enumerate acrylic acid series compound, epoxy based compound, silicone compound, polystyrene compound, phenol based compound, unsaturated polyester (UP) based compound etc., one or more that contain them also can.
Also have, heat of the present invention or optical polymerism compound are meant and utilize heat or photopolymerisable compound.Such compound can be any of monomer, oligomer or resin.Oligomer or resin are under the effect of heat or light and then carry out polymerization.
Wherein, preferably give acrylic acid series compound, epoxy based compound, the silicone compound of high-fire resistance polymkeric substance.And then, preferred acrylic acid series compound and silicone compound.Especially, clicyclic hydrocarbon (methyl) acrylate compounds of carbon atom quantity more than 7 give aspect the superior polymkeric substance of glass temperature height and photostability preferred.
As the clicyclic hydrocarbon of carbon number more than 7, can enumerate adamantyl, norborneol alkyl or two cyclopentane bases etc.Heat or optical polymerism compound are liquid before polymerization, also can be solid, but at room temperature operate easily under the situation of liquid, and because of this, Eng is preferred.
On the other hand, the glass temperature of the polymkeric substance (silicone-based resin) that is obtained by silicone compound is low, but flexibility is superior.Therefore, the thermal stress that the silicone-based resin can relax when the LED lamp is made or produce when using, can make it be difficult for causing and sealing-in agent or lead frame between peel off.In addition, the silicone-based resin is the also superior resin of photostability.Above preferred reason as the silicone-based resin is enumerated.
The content of heat or optical polymerism compound is 95～30 quality % with respect to containing the composition that heat or optical polymerism compound and hollow-particle form, preferred 90～50 weight %.
When hollow-particle comprises thickness 250 μ m is 50% above material to the ultraviolet ray transmissivity under the wavelength 350nm.More preferably 60%～100%.The ultraviolet ray that has seen through the shell of hollow-particle is reflected by hollow bulb, therefore, needs the high material of ultraviolet ray transmissivity.
In order to improve the reflectivity on the hollow bulb, preferably make the part that constitutes hollow-particle and be present in the difference of refractive index of hollow-particle gas inside big.Be present in the hollow-particle gas inside and be generally air, but can be inert gases such as nitrogen or argon, also can be vacuum.
Hollow-particle is the particle of an above separated foam of bag in particle inside preferably, but also can be for being formed with the offspring of hollow bulb.The composition that constitutes hollow-particle can be organism, also can be inorganics.But if the shell of hollow-particle absorbs ultraviolet ray, the ultraviolet ray that then arrives hollow-particle inside reduces, and the reflectivity on hollow bulb reduces, and therefore, preferably less absorbs ultraviolet hollow-particle.In addition, owing to causing hollow bulb, thermal treatment destroys sometimes.If hollow bulb disappears, then lose reflection characteristic, therefore, the preferred high hollow-particle of thermotolerance.
As such material, in inorganics, can suitably use slaines such as metal oxides such as beaded glass, silica, aluminium oxide, lime carbonate, barium carbonate, calcium silicate, nickelous carbonate etc.Can suitably use phenylethylene resin series, acrylic resin, and these crosslinked body etc. in organism, one or both that contain them all can.Wherein, preferred glass pearl, silica, cross-linked acrylic acid are that resin, cross-linked styrene are resin.
The external diameter of hollow-particle does not limit especially.From the viewpoint of light reflective, the property handled, preferred 0.01～500 μ m, more preferably 0.1～100 μ m.If less than 0.01 μ m, the preceding viscosity of polymerization that then contains the composition of heat or optical polymerism compound and hollow-particle uprises, and has the trouble that is difficult to figuration.If greater than 500 μ m, then the generation of the surface of reflecting body is coarse, has the trouble of reflectivity reduction.
The internal diameter of hollow-particle also limits especially.From the viewpoint of light reflective, preferred 0.005～100 μ m, more preferably 0.1～50 μ m.If come off this scope, then there is the trouble of reflection efficiency variation.
The content of hollow-particle is 5～70 quality % with respect to the composition that contains heat or optical polymerism compound or hollow-particle, preferred 10～50 weight %.If less than 5 weight %, then there is the trouble of reflectivity reduction, if greater than 70 quality %, the preceding viscosity of polymerization that then contains the composition of heat or optical polymerism compound and hollow-particle uprises, and has the trouble that is difficult to figuration.
The polymkeric substance that is used in reflecting material of the present invention contains thermoplastic resin and also can in order to improve thermotolerance.As thermoplastic resin, the preferably clear height, glass temperature is the resin more than 120 ℃.Glass temperature less than 120 ℃ situation under, the trouble that exists stable on heating raising effect to diminish.Usually, thermoplastic resin is used the composition before polymerization.
As such thermoplastic resin, can enumerate acrylic resin, phenylethylene resin series, polycarbonate-based, the polyarylate class, polyether sulfone, the epoxy acrylate class, alkene-maleic amide multipolymer, Qi Aonike (ZEONEX, Japan strange (Co., Ltd.) difficult to understand system, the cyclic olefine polymkeric substance), strange Noah (ZEONOR difficult to understand, Japan strange (Co., Ltd.) difficult to understand system, the cyclic olefine polymkeric substance), logical (the ARTO of peace, JSR (Co., Ltd.) system, the cyclic olefine polymkeric substance), broken plucked instrument (the TOPAS of holder, the Ticona corporate system, the cyclic olefine polymkeric substance), transparent ABS, transparent propene, the metering system styrene resin, polyarylate, polysulfones, transparent nylon, transparent polybutylene terephthalate, transparent fluororesin, poly--4-methylpentene-1, transparent phenoxy resin etc.
Under the situation of adding thermoplastic resin, its addition preferably contains 0.5～20 quality % in reflecting material of the present invention.If less than 0.5 quality %, then can not get improving thermotolerance and improve effect, if greater than 20 quality %, then make the mobile variation of the preceding composition of polymerization easily.
In addition, in the polymkeric substance that in reflecting material of the present invention, uses,, can also use known oxidation inhibitor and light stabilizer etc. as adjuvant.As oxidation inhibitor, can be that oxidation inhibitor, phosphorus are that oxidation inhibitor, sulphur are that oxidation inhibitor, lactone are that oxidation inhibitor, amine are oxidation inhibitor etc. for phenol.
The use amount of these oxidation inhibitor is generally 0.005～5 mass parts with respect to polymkeric substance total amount 100 mass parts, preferred 0.02～2 mass parts.Can also make up the two or more of these adjuvants.
It is light stabilizer that light stabilizer can suitably use hindered amine.
The addition of light stabilizer is generally 0.005～5 mass parts with respect to polymkeric substance total amount 100 mass parts, preferred 0.02～2 mass parts.Also can make up the two or more of these adjuvants.
In order further to reduce light-emitting device, the layer of preferred above-mentioned polymkeric substance is thin, but layer is thin more, and the summary that light and hollow-particle collide is high more, and therefore, reflectivity uprises.
By reflecting material cambium layer of the present invention the time, the preferred 0.05～2mm of thickness of the layer of above-mentioned polymkeric substance, more preferably 0.25～2mm.
Reflecting material of the present invention not only has high reflectivity to ultraviolet ray, even and also keep high reflectivity through bakingout process when light-emitting device is made.For example, even pass through the thermal treatment of sealing-in operation (100～200 ℃ were descended several hours), the so-called cruelty of solder reflow operation (260 ℃ of several seconds), also can keep reflectivity more than 50% to the light of wavelength 350nm.
Above-mentioned polymkeric substance preferably uses with the state that is laminated with polymkeric substance on the matrix that constitutes at the material high to the reflectivity of visible light.Thus, can access not only ultraviolet ray, and to the high reflectance of visible light.At this, " material high to the reflectivity of visible light " is meant that the visible reflectance under wavelength 550nm is the material more than 80%.
As the material of such matrix, can enumerate and contain the resin combination that the entity particle is a Chinese white.Comprise that entity particles such as containing titanium dioxide is that the ultraviolet reflection ability of matrix of resin combination of Chinese white is low, but the reflectivity of visible light is very high.
If comprising on the matrix of this resin combination, stacked is the polymkeric substance of raw material with the composition that contains heat of the present invention or optical polymerism compound and hollow-particle, then shine under the situation of visible light, even the light that is seen through by the polymeric layer reflection that with the composition that contains heat or optical polymerism compound and hollow-particle is raw material is not reflected by matrix yet on top from this duplexer.Thereby, stacked as described above, can access not only ultraviolet ray, and to the high reflectivity of visible light.
As the entity particle is Chinese white, for example, can enumerate titanium dioxide, silica, potassium titanate, barium sulphate, aluminium oxide, zinc paste, lime carbonate, talcum, mica etc.
The entity particle is that the content of Chinese white does not limit especially, but is that Chinese white is preferably 1～50 weight % with respect to containing the entity particle, more preferably 5～40 weight %.
As containing the resin that the entity particle is a Chinese white, for example, can enumerate polyamide, liquid crystal polymer, polyethers is resin, syndiotactic polytyrene, polyester based resin etc.
The content that contains the entity particle and be the resin of Chinese white does not limit especially, but is that the resin combination of Chinese white is preferably 40～95 weight % with respect to containing the entity particle, more preferably 50～90 weight %.
The resin combination that contains the entity particle and be Chinese white can also contain glass fibre etc.
In addition, matrix preferably uses by one or more metals that constitute that are selected from aluminium, gold, silver, copper, nickel or palladium.The matrix that such metal constitutes even serve as reasons also can obtain high reflectivity in ultraviolet ray and visible light.
The shape of matrix may not be for plane, can be shape arbitrarily.
The present invention is being applicable under the situation of LED reflecting body, for example, can use be configured as Fig. 2 (a) 10 the matrix of concavity shape.In this case, the thickness of the polymeric layer that constitutes by the composition that contains heat or optical polymerism compound and hollow-particle according to circumstances and different (with reference to Fig. 2 (b) 24).Preferred 0.05～the 3mm of the maximum ga(u)ge of this layer, more preferably 0.25～2mm.
Reflecting material of the present invention can be by mixing hollow-particle in heat or optical polymerism compound, utilize light or photopolymerization then and make.In addition, in order to promote polyreaction, add polymerization initiator and also can.Polymerization initiator does not limit especially.For example, can use radical polymerization initiator etc.As radical polymerization initiator, can enumerate ketone peroxide classes such as butanone peroxide, methyl-isobutyl ketone peroxide, acetyl acetone peroxide, cyclohexanone superoxide, methyl cyclohexanone peroxide; 1,1,3, hydroperoxide type such as 3-tetramethyl butyl hydroperoxides, cumene hydroperoxide, tert butyl hydroperoxide; And isobutyryl superoxide, two-3,5, diacyl peroxide classes such as 5-trimethyl hexanone superoxide, lauroyl superoxide, benzoyl peroxide, Zhong Jia (base) benzoyl benzoyl superoxide; Dicumyl peroxide, 2,5-dimethyl-2,5-two (tert-butyl hydroperoxide isopropyl) hexane, tert-butyl group cumyl peroxide, di-tert-butyl peroxide, 2,5-dimethyl-2, dialkyl peroxide classes such as 5-two (tert-butyl hydroperoxide) hexene; 1,1-two (tert-butyl hydroperoxide-3,5,5-trimethyl) cyclohexane, 1,1-two-tert-butyl hydroperoxide cyclohexane, 2, ketal peroxide classes such as 2-two (tert-butyl hydroperoxide) butane; 1,1,3, new two carbonic esters of 3-tetramethyl butyl peroxidating, new two carbonic esters of α-cumyl peroxidating, new two carbonic esters of tert-butyl hydroperoxide, uncle's hexyl peroxidating pivalate, t-butylperoxy pivarate, 1,1,3,3-tetramethyl butyl peroxidating-2-ethyl hexanone ester, the amino peroxidating of uncle-2-ethyl hexanone ester, tert-butyl hydroperoxide-2-ethyl hexanone ester, the tert-butyl hydroperoxide isobutyl ester, di-tert-butyl peroxide six hydrogen terephalic acid esters, 1,1,3, the peroxidating-3 of 3-tetramethyl butyl, 5,5-tri-methyl hexanoic acid ester, the amino peroxidating 3 of uncle, 5,5-trimethyl hexanone ester, tert-butyl hydroperoxide 3,5,5-trimethyl hexanone ester, the tert-butyl hydroperoxide acetic acid esters, tert butyl peroxy benzoate, alkyl such as dibutyl peroxidating trimethyladipic acid ester are crossed the ester class, two-3-methoxyl butyl peroxyization, two carbonic esters, two-2-ethylhexyl peroxy dicarbonate, two (1,1-butyl hexamethylene oxygen two carbonic esters), diisopropyl oxygen two carbonic esters, the amino peroxidating isopropyl of uncle carbonic ester, tert-butyl hydroperoxide isopropyl carbonic ester, tert-butyl hydroperoxide-2-ethylhexyl carbonic ester, 1, peroxycarbonates classes such as two (tert-butyl hydroperoxide carboxyl) hexanes of 6-etc.In addition, can enumerate Po Haise 3M-95 (Japanese grease (Co., Ltd.) or the azobis isobutyronitrile etc. that in embodiment described later, use.The use amount of radical polymerization initiator is generally 0.01～5 mass parts with respect to described heat or optical polymerism total amount of compound 100 mass parts, preferred 0.05～1.0 mass parts.Use respectively separately above-mentioned radical polymerization initiator also can, in addition, share and a plurality ofly also can.
Reflecting material of the present invention can suitably be used in the LED reflecting body, but also goes for other reflecting body purposes.Especially, be fit to the purposes of needs ultraviolet reflection ability or require purposes to the stability of heat.
It is the polymeric layer of raw material that LED of the present invention has with the composition that contains heat or optical polymerism compound and hollow-particle with reflecting body at reflecting surface at least.
With in the reflecting body, described polymkeric substance is preferably to contain the upward stacked state use of formed body (matrix) that the entity particle is the resin combination formation of Chinese white at LED of the present invention.In addition, with in the reflecting body, described polymkeric substance preferably uses to go up stacked state at the formed body that is made of specific metal (matrix) at LED of the present invention.
[embodiment]
Shown in the thermoplastic resins that use in embodiment and comparative example etc. are following.
(1) thermoplastic resin
Semiconductor aromatic polyamide: carry your (ザ イ テ Le) HTN501 (Du Pont (Co., Ltd.)) assortedly
(2) polymerizable compound
The acrylic acid series compound:
(a) the Order Man Dike AM (ultraviolet ray transmissivity 92% (wavelength 350nm, thickness 250 μ m) of the emerging product of bright dipping (Co., Ltd.) system, 1-adamantyl methacrylate/Po Haise 3M-95 (Japanese grease (Co., Ltd.))=100/0.1 (mass ratio), polymkeric substance
(b) can lira FM-513 (Hitachi changes into industry (Co., Ltd.) system, two cyclopentane ylmethyl acrylate)/azobis isobutyronitrile (Tokyo changes into industry (Co., Ltd.))=100/0.1 (mass ratio), the ultraviolet ray transmissivity 92% (wavelength 350nm, thickness 250 μ m) of polymkeric substance
(c) ultraviolet ray transmissivity 92% (wavelength 350nm, thickness 250 μ m) of norborny methacrylate (with the pure pharmaceutical worker's industry of light (Co., Ltd.))/Po Haise 3M-95 (Japanese grease (Co., Ltd.))=100/0.1 (mass ratio), polymkeric substance
The epoxy based compound
Ai Pukete (エ ピ コ one ト) 828 (japan epoxy resin (Co., Ltd.))/methyl hexahydroxy anhydride phthalic acids (hardening agent) (with the pure medicine of light (Co., Ltd.))/1,8-diazabicyclo (ジ ア ザ PVC シ Network ロ) [5,4,0] ultraviolet ray transmissivity 90% (wavelength 350nm, thickness 250 μ m) of undecane-7-alkene (Qi Gemaalede Japan (シ グ マ ア Le De リ Star チ ジ ヤ パ Application) (Co., Ltd.))=50/50/0.1 (mass ratio), polymkeric substance.
Silicone compound:
(a) ultraviolet ray transmissivity 93% (wavelength 350nm, thickness 250 μ m) of XJL-0012A (Japan sends happy nox (ペ Le ノ Star Network ス) (Co., Ltd.))/XJL-0012B (Japan sends happy nox (Co., Ltd.))=100/5 (mass ratio), polymkeric substance
(b) ultraviolet ray transmissivity 91% of SCR-1011A (SHIN-ETSU HANTOTAI's silicone (Co., Ltd.))/SCR-1011B (SHIN-ETSU HANTOTAI's silicone (Co., Ltd.))=100/100 (mass ratio), polymkeric substance (wavelength 350nm, thickness 250 μ m)
(3) hollow packing (hollow-particle)
Hollow Glass Sphere: HSC-110C (Pa Dezi Paro base of a fruit Buddhist nun (Co., Ltd.), mean grain size 13 μ m, average pore size 9 μ m, (ultraviolet ray transmissivity 90% of glass (wavelength 350nm, thickness 250 μ m))
Cross-linked acrylic acid is a hollow-particle: (ponding changes into product industry (Co., Ltd.), mean grain size 5 μ m, average pore size 1-2 μ m, (ultraviolet ray transmissivity 84% of cross-linked acrylic acid (wavelength 350nm, thickness 250 μ m)) to XX06BZ
(4) entity filler (the entity particle is a Chinese white)
Silica beads: FB201SX (clear and electrician (Co., Ltd.), mean grain size 7.8 μ m)
Titanium dioxide: pik ( イ ペ one Network) R680 (the former industry of stone (Co., Ltd.), mean grain size 0.21 μ m) too
(5) other
Glass fibre: rising sun fiber Ge Lesi (Co., Ltd.), JAFT164G
Embodiment 1～5, comparative example 1～2
In acrylic acid series compound (a) (liquid), add filler,, fully disperse filler at 15 minutes ultrasound wave of supersonic wave cleaning machine internal radiation in the ratio shown in the table 1.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃, make acrylic acid series compound (a) thermal polymerization.After the polymerization, from aluminium practise usury from, obtain the plectane of diameter 5cm, the about 1mm of thickness.This plectane is implemented following processing and estimated.
(1) thermal treatment
Under two following conditions, heat-treat.Following i) being the condition of the imagination hot resume that reflecting material is subjected in the sealing-in operation, ii) is the condition of the hot resume that reflecting material is subjected in the imaginary solder reflow operation.
I) 160 ℃, 3 hours.Ii) 260 ℃, 10 seconds.
(2) ultraviolet ray irradiation
(lucky skot Na Suoer (ジ ヤ ス コ イ Application one Na シ ヨ Na Le) system, solarbox1500e0 are with 500W/m to use the light fastness test machine
2Output irradiation 100 hours.
(3) mensuration of reflectivity
By the following method, measure after initial reflectance, the thermal treatment and ultraviolet postradiation reflectivity.Dividing spectrum photometer UV-2400PC to go up in the system self-recording of (Co., Ltd.) Shimadzu Seisakusho Ltd. installs the large-scale test portion chamber unit of (Co., Ltd.) Shimadzu Seisakusho Ltd. system multi-usage MPC-2200, measure reflectivity (%) in the scope of wavelength 700～300nm.Also have, as a reference, use barium sulphate.
Fig. 1 illustrates the measurement result of embodiment 2.Table 2 illustrates the reflectivity under 550nm and the 350nm.
(4) glass temperature
Use differential scanning type calorimeter (eight Jin Ailuma (パ one キ Application エ Le マ one) corporate system, DSC-7), with test portion 10mg under the blanket of nitrogen-50 ℃ down keep 5 minutes after, with 20 ℃ of/minute intensifications, hot-fluid speed curve thus, with the point of discontinuity of this hot-fluid speed curve of observing as glass temperature.The results are shown in the table 2.
Embodiment 6, comparative example 3
In epoxy based compound (liquid), add filler,, fully disperse filler at 15 minutes ultrasound waves of supersonic wave cleaning machine internal radiation in the ratio shown in the table 1.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 3 hours with 130 ℃, make the thermal polymerization of epoxy based compound, obtain the plectane of diameter 5cm, the about 1mm of thickness.Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 2.
Embodiment 7
In silicone compound (liquid), add filler,, fully disperse filler at 15 minutes ultrasound waves of supersonic wave cleaning machine internal radiation in the ratio shown in the table 1.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 3 hours with 160 ℃, make the silicone compound thermal polymerization, obtain the plectane of diameter 5cm, the about 1mm of thickness.Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.The results are shown in the table 2.
Comparative example 4
Cooperate semiaromatic polyamide composition, titanium dioxide, glass fibre in the ratio shown in the table 1, do mix after, it is dropped in the funnel of biaxial extruder of internal diameter 30mm, like for 330 ℃ forming particle by melting mixing at barrel temperature.The particle that obtains at 100 ℃ down behind the dry diel, with 330 ℃ of barrel temperatures, 120 ℃ of sputtering formings of metal pattern temperature, is obtained the thick square plate of the square 1mm of 3cm.Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.The results are shown in the table 2.
[table 1]
| Raw material (weight %) | Embodiment 1 | |
Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Acrylic acid series compound (a) | 90 | 80 | 70 | 50 | 80 | 80 | 80 | ||||
| The epoxy based compound | 80 | 80 | |||||||||
| Silicone-based resin (a) | 80 | ||||||||||
| Semiaromatic polyamide composition | 70 | ||||||||||
| Hollow Glass Sphere | 10 | 20 | 30 | 50 | 20 | 20 | |||||
| Cross-linked acrylic acid is a hollow-particle | 20 | ||||||||||
| The entity silica beads | 20 | ||||||||||
| Titanium dioxide | 20 | 20 | 10 | ||||||||
| Glass fibre | 20 |
The Hollow Glass Sphere that the last coating of the square plate that obtains in comparative example 4 (the luminous ray reflectivity 90.6% under the 550nm) will be used in embodiment 2 is scattered in the fillers dispersed liquid 1g in the acrylic acid series compound (a), carries out thermal polymerization with 110 ℃ of 3 hours, 160 ℃ conditions of 1 hour.Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.The results are shown in the table 2.
Comparative example 5
Open the embodiment 1 of 2004-101601 according to the spy, make the light reflective film of the about 200 μ m of thickness.
Promptly, supply with intrinsic viscosity 0.63dl/g to main extruder, the polyethylene terephthalate that fusing point is 256 ℃ (following is PET) 89 weight %, the polymethylpentene 10 weight % that fusing point is 235 ℃, molecular weight 4, the particle that 000 polyglycol 1 weight % mixes, in addition, supply with PET85 weight % to other secondary extruder, the particle that the calcium carbonate particle 15 weight % of mean grain size 1.5 μ m mix, so that being laminated in the mode on the top layer, both sides of the resin bed of extruding from main extruder, the composition of supplying with to secondary extruder melt extrudes, utilize static to apply method, cooling on the casting drum, making three is lamination layer by layer.Should stacked be stretched to 3.3 times, then make it pass through 110 ℃ of preheating zones, be stretched to 3.5 times 120 ℃ of following broad ways with stenter at 90 ℃ of lower edge long side directions of temperature.And then, under 220 ℃, carrying out the thermal treatment in 30 seconds, the thermal treatment sheet obtains stretching.At the single face of this sheet so that the dry thickness average thickness of following coating material becomes the mode of 10 μ m applies, 120 ℃ dry 2 minutes down, obtain the light reflective film of total film thickness 200 μ m.Coating material uses: to the little 1 part of (weight portion of emulsion solution (solid component concentration 33%) that is scattered in the water of the silica hollow-particle B-6C (Suzuki oil prodution industry (Co., Ltd.)) of mean grain size 2 μ m, down together), stir 2 parts of aqueous adhesive pigment solutions (solid component concentration 50%) (Japan (Co., Ltd.) very difficult to understand system, Nipol Lx407BP) that add modified phenylethylene-butadiene and constitute and the material that obtains.The flat bubble containing ratio of the light reflective film that obtains is 92.8%, and the hollow-particle area ratio/occupancy ratio is 60.9%.Like this, this film has flat bubble, but the reflecting material of embodiment does not have flat bubble.
To the film that obtains, heat-treat in the same manner etc. with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.The results are shown in the table 2.
[table 2]
Electronic unit shown in the construction drawing 2c (LED reflecting body).
With resin combination 10 sputtering formings (330 ℃ of barrel temperatures, 120 ℃ of metal pattern temperature) that use in the comparative example 4, make as shown in Figure 2 and integrally formed product lead frame 12.Element mounted 20 on this formed products (Ri Ya chemical company system, NCCU033), behind metal wire 22 joints, the double glazing paper that uses in the inside of described sputtering forming product applies embodiment 2 is scattered in the fillers dispersed liquid 24 (with reference to Fig. 2 b) of acrylic acid series compound (a), carries out thermal polymerization with 110 ℃ of 3 hours, 160 ℃ conditions of 1 hour.At this moment, the maximum ga(u)ge of thermopolymer 24 is about 0.7mm.Then, as sealing-in agent 30, the recess with acrylic acid series compound (a) input formed products carries out polymerization (with reference to Fig. 2 c) with 110 ℃ of 3 hours, 160 ℃ conditions of 1 hour.To the electronic unit energising that obtains like this, by visual investigation brightness.Estimate as described below.
◎: very bright
Zero: bright
△: not bright
*: dark
Evaluation result is illustrated in the table 3.
Embodiment 10
As the sealing-in agent, replace acrylic acid series compound (a), use silicone compound (a), carry out thermal polymerization with 160 ℃ of conditions of 3 hours, in addition, use the method identical with embodiment 9, obtain electronic unit.Energising and with visual investigation brightness.Evaluation result is illustrated in the table 3.
Comparative example 6
Replacement with the fillers dispersed of using Hollow Glass Sphere to be scattered in acrylic acid series compound (a) among the embodiment 2 in, the difficult acrylic acid series compound of the angry think of of titanium dioxide (a) that uses in the comparative example 2 is used in coating, in addition, use the method identical, obtain electronic unit with embodiment 9.To the energising of the electronic unit that obtains like this and with visual investigation brightness.Evaluation result is illustrated in the table 3.
[table 3]
| Formed body (matrix) | Polymeric layer | Seal, sealing | Brightness | |
| Embodiment | ||||
| 9 | Comparative example 4 | |
Acrylic acid series compound (a) | ◎ |
| Embodiment 10 | Comparative example 4 | |
Silicone compound (a) | ◎ |
| Comparative example 6 | Comparative example 4 | Comparative example 2 | Acrylic acid series compound (a) | ○ |
Embodiment 11
In acrylic acid series compound (b), add filler (hollow-particle),, fully disperse filler at 15 minutes ultrasound waves of supersonic wave cleaning machine internal radiation in the ratio shown in the table 4.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃, make acrylic acid series compound (b) thermal polymerization.Obtain the plectane of diameter 5cm, thickness 1mm.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 5.
Embodiment 12
In acrylic acid series compound (c), add filler (hollow-particle),, fully disperse filler at 15 minutes ultrasound waves of supersonic wave cleaning machine internal radiation in the ratio shown in the table 4.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃, make acrylic acid series compound (c) thermal polymerization.Obtain the plectane of diameter 5cm, thickness 1mm.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 5.
Embodiment 13
In silicone compound (b), add filler (hollow-particle),, fully disperse filler at 15 minutes ultrasound waves of supersonic wave cleaning machine internal radiation in the ratio shown in the table 4.This fillers dispersed liquid 2g is dropped on the aluminium dish of diameter 5cm, heat-treated in 5 hours with 70 ℃ 1 hour, 150 ℃, make silicone compound (b) thermal polymerization.Obtain the plectane of diameter 5cm, thickness 1mm.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 5.
Embodiment 14
The fillers dispersed liquid 0.7g of preparation among the embodiment 3 is dropped on the aluminium dish of diameter 5cm, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃, obtain the plectane of diameter 5cm, thickness 0.3mm.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 5.
Embodiment 15
The fillers dispersed liquid 0.25g of preparation among the embodiment 3 is dropped on the aluminium dish of diameter 5cm, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃, obtain the plectane of diameter 5cm, thickness 0.3mm.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.In addition, measure glass temperature with described method.The results are shown in the table 5.
Embodiment 16
On the aluminium sheet thick of surface, be coated in the fillers dispersed liquid 1g of preparation among the embodiment 3, heat-treated in 1 hour with 110 ℃ 3 hours, 160 ℃ by the square 1mm of silver-plated 3cm.After the polymerization, polymer layer is not peeled off and estimated from aluminium sheet.
Implement thermal treatment etc. in the same manner with embodiment 1, measuring after initial, the thermal treatment is ultraviolet postradiation reflectivity.The results are shown in the table 5.Also have, the light reflectance under the wavelength 550nm of silver is 98%.
[table 4]
| Raw material (weight %) | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 |
| Acrylic acid series compound (a) | 70 | 70 | 70 | |||
| Acrylic acid series compound (b) | 70 | |||||
| Acrylic acid series compound (c) | 70 | |||||
| Silicone compound (b) | 70 | |||||
| Hollow Glass Sphere | 30 | 30 | 30 | |||
| Cross-linked acrylic acid is a hollow-particle | 30 | 30 | 30 |
[table 5]
Industrial utilizability
Reflecting material of the present invention can be used in liquid crystal display with lamp reflector, show window with reflecting plate, each journey lighting reflection plate, LED with reflector etc. LED can be used in the various OA equipment such as display, destination display board, vehicle-mounted illumination, signal lamp, emergency lamp, mobile phone, video camera, electric/electronic device and parts, automobile component etc. with reflector.
Claims (11)
1. reflecting material, it is that the polymkeric substance of raw material constitutes by following to comprise (a) and composition (b):
(a) heat or optical polymerism compound 95～30 quality %;
(b) be hollow-particle 5～70 quality % that the material more than 50% constitutes by the ultraviolet ray transmissivity under the wavelength 350nm.
2. reflecting material according to claim 1, wherein,
Ultraviolet ray transmissivity under the wavelength 350nm of described heat or optical polymerism compound is more than 50%.
3. reflecting material according to claim 1 and 2, wherein,
Described heat or optical polymerism compound are by one or more compounds that constitute that are selected from acrylic acid series compound, epoxy based compound, the silicone compound.
4. according to each described reflecting material in the claim 1～3, wherein,
Described hollow-particle is cross-linked resin or mineral compound.
5. according to each described reflecting material in the claim 1～4, wherein,
Described hollow-particle is that cross-linked styrene is that resin, cross-linked acrylic acid are resin, unorganic glass or silica.
6. according to each described reflecting material in the claim 1～5, wherein,
Also be included in luminous ray reflectivity under the wavelength 550nm and be the matrix more than 80%, on this matrix, be laminated with described to comprise (a) and composition (b) is the polymkeric substance of raw material.
7. reflecting material according to claim 6, wherein,
Described matrix is to comprise the resin combination that the entity particle is a Chinese white.
8. reflecting material according to claim 6, wherein,
Described matrix is by one or more metals that constitute that are selected from aluminium, gold, silver, copper, nickel or the palladium.
9. reflector for light-emitting diode, it has each described reflecting material in the claim 1～8 at reflecting surface at least.
10. reflector for light-emitting diode according to claim 9, wherein,
It is on the formed body that constitutes of the resin combination of Chinese white that described reflecting material is layered in by comprising the entity particle.
11. reflector for light-emitting diode according to claim 9, wherein,
Described reflecting material is layered on the formed body that is made of one or more metals that constitute that are selected from aluminium, gold, silver, copper, nickel or the palladium.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP284068/2005 | 2005-09-29 | ||
| JP2005284068 | 2005-09-29 | ||
| JP159359/2006 | 2006-06-08 |
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| Publication Number | Publication Date |
|---|---|
| CN101278213A true CN101278213A (en) | 2008-10-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800355125A Pending CN101278213A (en) | 2005-09-29 | 2006-09-01 | Reflecting material and reflector for light emitting diode |
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| CN (1) | CN101278213A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443137A (en) * | 2010-10-05 | 2012-05-09 | 日东电工株式会社 | Epoxy resin composition for optical semiconductor device, lead frame obtained using the same for optical semiconductor device, and optical semiconductor device |
| CN102804361A (en) * | 2010-03-15 | 2012-11-28 | 欧司朗光电半导体有限公司 | Optoelectronic component and method for the production thereof |
| CN103018804A (en) * | 2012-12-28 | 2013-04-03 | 合肥乐凯科技产业有限公司 | Reflecting film |
| CN103323895A (en) * | 2013-05-22 | 2013-09-25 | 宁波长阳科技有限公司 | Silver-plated reflecting film and preparation method thereof |
| US20190389161A1 (en) * | 2013-05-22 | 2019-12-26 | Ningbo Solartron Technology Co., Ltd. | Method for manufacturing silver-plated reflecting film |
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2006
- 2006-09-01 CN CNA2006800355125A patent/CN101278213A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102804361A (en) * | 2010-03-15 | 2012-11-28 | 欧司朗光电半导体有限公司 | Optoelectronic component and method for the production thereof |
| US9121585B2 (en) | 2010-03-15 | 2015-09-01 | Osram Opto Semiconductors Gmbh | Optoelectronic component and method for the production thereof |
| CN102443137A (en) * | 2010-10-05 | 2012-05-09 | 日东电工株式会社 | Epoxy resin composition for optical semiconductor device, lead frame obtained using the same for optical semiconductor device, and optical semiconductor device |
| CN103018804A (en) * | 2012-12-28 | 2013-04-03 | 合肥乐凯科技产业有限公司 | Reflecting film |
| CN103018804B (en) * | 2012-12-28 | 2016-01-20 | 合肥乐凯科技产业有限公司 | A kind of reflectance coating |
| CN103323895A (en) * | 2013-05-22 | 2013-09-25 | 宁波长阳科技有限公司 | Silver-plated reflecting film and preparation method thereof |
| CN103323895B (en) * | 2013-05-22 | 2015-06-17 | 宁波长阳科技有限公司 | Preparation method for silver-plated reflecting film |
| US20160062002A1 (en) * | 2013-05-22 | 2016-03-03 | Ningbo Solartron Technology Co., Ltd. | Silverplated reflecting film and manufacturing method thereof |
| US20190389161A1 (en) * | 2013-05-22 | 2019-12-26 | Ningbo Solartron Technology Co., Ltd. | Method for manufacturing silver-plated reflecting film |
| US11969964B2 (en) * | 2013-05-22 | 2024-04-30 | Ningbo Solartron Technology Co., Ltd. | Method for manufacturing silver-plated reflecting film |
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