JP2007095770A - Resin composition and LED using the same - Google Patents
Resin composition and LED using the same Download PDFInfo
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- JP2007095770A JP2007095770A JP2005279855A JP2005279855A JP2007095770A JP 2007095770 A JP2007095770 A JP 2007095770A JP 2005279855 A JP2005279855 A JP 2005279855A JP 2005279855 A JP2005279855 A JP 2005279855A JP 2007095770 A JP2007095770 A JP 2007095770A
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- 239000011342 resin composition Substances 0.000 title claims abstract description 37
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000002245 particle Substances 0.000 claims abstract description 27
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011787 zinc oxide Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims description 26
- 239000011347 resin Substances 0.000 claims description 26
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 description 31
- 230000005284 excitation Effects 0.000 description 14
- 238000001723 curing Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000009261 D 400 Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000013007 heat curing Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- -1 lanthanide metals Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910018509 Al—N Inorganic materials 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
【課題】蛍光体の発光特性を安定化し、発光特性に優れ、また耐熱性にも優れ長寿命なＬＥＤ或いはＬＥＤ用部材を提供する
【解決手段】樹脂に、蛍光体粒子と３００〜８００ｎｍの領域で光透過性の粒子、好ましくは３５０〜６００ｎｍの領域で光透過性の粒子とを含有させてなることを特徴とする樹脂組成物であり、好ましくは、光透過性の粒子が、比表面積値が３０ｍ２／ｇ以上４００ｍ２／ｇ以下であり、酸化珪素、酸化アルミニウム、酸化チタン、酸化セリウム、酸化イットリウム、酸化亜鉛、酸化錫、及びＩＴＯからなる群から選ばれる１種以上であり、更に、蛍光体が酸窒化物からなることを特徴とする前記の樹脂組成物。
【選択図】なしProvided is an LED or LED member that stabilizes the light emission characteristics of a phosphor, has excellent light emission characteristics, has excellent heat resistance, and has a long service life. And a light-transmitting particle, preferably a light-transmitting particle in the region of 350 to 600 nm. Preferably, the light-transmitting particle has a specific surface area value. Is 30 m 2 / g or more and 400 m 2 / g or less, and is at least one selected from the group consisting of silicon oxide, aluminum oxide, titanium oxide, cerium oxide, yttrium oxide, zinc oxide, tin oxide, and ITO, The above-mentioned resin composition, wherein the phosphor is made of oxynitride.
[Selection figure] None
Description
本発明は、発光強度が強く、耐熱性に高く、長寿命のＬＥＤとそれに用いて好適な樹脂組成物、それからなるＬＥＤ用シートに関する。 The present invention relates to an LED having a high light emission intensity, a high heat resistance, a long life, a resin composition suitable for the LED, and an LED sheet comprising the same.
蛍光体として、母体材料に酸化物、珪酸塩、リン酸塩、アルミン酸塩、硫化物を用い、発光中心に遷移金属又は希土類元素を用いたものが広く知られている。 As phosphors, those using oxides, silicates, phosphates, aluminates, and sulfides as base materials and using transition metals or rare earth elements as emission centers are widely known.
一方、白色ＬＥＤに関しては、紫外線又は青色光などの高いエネルギーを有した励起源により励起されて可視光を発する蛍光体が注目され、開発が進んでいる。しかしながら、前記した従来の蛍光体では、励起源に曝される結果として、蛍光体の輝度が低下するという問題がある。 On the other hand, with respect to the white LED, a phosphor that emits visible light when excited by an excitation source having high energy such as ultraviolet light or blue light has been attracting attention and is being developed. However, the above-described conventional phosphor has a problem in that the luminance of the phosphor decreases as a result of exposure to the excitation source.
このため、輝度低下が少ない蛍光体として、最近、結晶構造が安定で、励起光や発光を長波長側にシフトできる材料であることから、窒化物や酸窒化物蛍光体が注目されている。 For this reason, nitrides and oxynitride phosphors have recently attracted attention as phosphors with low luminance reduction because they have a stable crystal structure and can shift excitation light and light emission to the longer wavelength side.
窒化物、酸窒化物蛍光体として、特定の希土類元素が付活されたα型サイアロンは、有用な蛍光特性を有することが知られており、白色ＬＥＤ等への適用が検討されている（特許文献１〜５、非特許文献１参照）。
α型サイアロンは、α型窒化ケイ素の固溶体であり、結晶格子内に特定の元素（Ｃａ、並びにＬｉ、Ｍｇ、Ｙ、又はＬａとＣｅを除くランタニド金属）が侵入固溶し、電気的中性を保つために、Ｓｉ−Ｎ結合が部分的にＡｌ−Ｎ結合とＡｌ−Ｏ結合で置換された構造を有している。侵入固溶する元素の一部を発光中心となる希土類元素とすることにより蛍光特性が発現する。 α-type sialon is a solid solution of α-type silicon nitride, and specific elements (Ca and Li, Mg, Y, or lanthanide metals excluding La and Ce) penetrate into the crystal lattice to form a solid solution. Therefore, the Si—N bond is partially substituted with an Al—N bond and an Al—O bond. Fluorescence characteristics are exhibited by using a rare earth element as a light emission center for a part of the element that enters and dissolves.
一般的にα型サイアロンは、窒化ケイ素、窒化アルミニウム、必要に応じて酸化アルミニウム、及び侵入固溶する元素の酸化物等からなる混合粉末を窒素中の高温で焼成することにより得られる。窒化ケイ素とアルミニウム化合物との比率と、侵入固溶させる元素の種類、並びに発光中心となる元素の割合等により、多様な蛍光特性が得られる。 In general, α-sialon is obtained by firing a mixed powder composed of silicon nitride, aluminum nitride, aluminum oxide as required, oxide of an element that enters and dissolves at high temperature in nitrogen, and the like. Various fluorescent characteristics can be obtained depending on the ratio of silicon nitride and aluminum compound, the type of element to be intruded and dissolved, the ratio of the element serving as the emission center, and the like.
ところで、現在まで得られている白色ＬＥＤは、発光効率が蛍光ランプに及ばないという事情がある。蛍光ランプよりも発光効率に優れるＬＥＤ、特に白色ＬＥＤが産業上で省エネルギーや水銀フリーといった環境面から強く要求されている。 By the way, the white LED obtained up to now has a situation that the luminous efficiency does not reach that of the fluorescent lamp. There is a strong demand for LEDs, which are superior in luminous efficiency than fluorescent lamps, in particular white LEDs, from the environmental aspect of energy saving and mercury-free in the industry.
白色は、単色とは異なる複数の色の組み合わせが必要であり、一般的な白色ＬＥＤは、紫外ＬＥＤ又は青色ＬＥＤとそれらの光を励起源とし、可視光を発する蛍光体との組み合わせにより構成されている。従って、白色ＬＥＤの効率向上と共に、そこに用いられる蛍光体の効率向上、更には、発せられた光を外部に取り出す効率の向上が必要である。白色ＬＥＤの一般照明用まで含めた用途拡大のためには、これら全ての効率向上が必要である。 White requires a combination of a plurality of colors different from a single color, and a general white LED is composed of a combination of an ultraviolet LED or a blue LED and a phosphor that emits visible light using such light as an excitation source. ing. Accordingly, it is necessary to improve the efficiency of the white LED, improve the efficiency of the phosphor used therein, and further improve the efficiency of extracting emitted light to the outside. In order to expand the application including the general illumination of the white LED, it is necessary to improve all of these efficiencies.
また、前記蛍光体は樹脂に粉末状に充填して使用されることが多いが、蛍光体粉末を樹脂に充填させるときに、特に粉末の充填率が低いときには、蛍光体粉末の沈降が生じ、その結果密度分布が生じ、発光特性が安定しない問題を生じることがある。これを防止するために、有機物系の沈降防止剤を用いることは広く知られている。 In addition, the phosphor is often used by filling the resin in a powder form, but when the phosphor powder is filled in the resin, particularly when the powder filling rate is low, the phosphor powder is precipitated, As a result, a density distribution may occur, and the light emission characteristics may not be stable. In order to prevent this, it is widely known to use organic anti-settling agents.
しかし、蛍光体粉末を樹脂に低充填するときには、従来から用いられている有機物系の沈降防止剤では励起光や発光に対して透明ではないため輝度が低下するという問題がある。 However, when the phosphor powder is low-filled into the resin, the organic anti-settling agent used conventionally has a problem that the luminance is lowered because it is not transparent to excitation light and light emission.
本発明は、蛍光体粉末を樹脂に充填したときに、蛍光体粉末の沈降を防ぎ、蛍光体粉末が樹脂中に均一分散した樹脂組成物を得ることで、蛍光体の発光特性を安定化することを目的とし、惹いては、発光特性に優れ、また耐熱性にも優れ長寿命なＬＥＤ或いはＬＥＤ用部材を提供することを目的としている。 The present invention stabilizes the light emission characteristics of a phosphor by preventing the sedimentation of the phosphor powder and obtaining a resin composition in which the phosphor powder is uniformly dispersed in the resin when the phosphor powder is filled in the resin. The purpose of this is to provide an LED or a member for an LED that has excellent light emission characteristics, excellent heat resistance, and a long life.
即ち、本発明は、樹脂に、蛍光体粒子と３００〜８００ｎｍの領域で光透過性の粒子、好ましくは３５０〜６００ｎｍの領域で光透過性の粒子とを含有させてなることを特徴とする樹脂組成物である。 That is, the present invention comprises a resin comprising phosphor particles and light-transmitting particles in a region of 300 to 800 nm, preferably light-transmitting particles in a region of 350 to 600 nm. It is a composition.
また、本発明は、光透過性の粒子が、比表面積値が３０ｍ２／ｇ以上４００ｍ２／ｇ以下であることが好ましく、更により好ましい実施態様として、光透過性の粒子が、酸化珪素、酸化アルミニウム、酸化チタン、酸化セリウム、酸化イットリウム、酸化亜鉛、酸化錫、及びＩＴＯ（チタン酸インジウム）からなる群から選ばれる１種以上であることを特徴とする。 In the present invention, it is preferable that the light-transmitting particles have a specific surface area value of 30 m 2 / g or more and 400 m 2 / g or less, and as a still more preferable embodiment, the light-transmitting particles include silicon oxide, It is one or more selected from the group consisting of aluminum oxide, titanium oxide, cerium oxide, yttrium oxide, zinc oxide, tin oxide, and ITO (indium titanate).
また、本発明は、蛍光体が酸窒化物からなることを特徴とする前記の樹脂組成物であり、好ましくは、前記樹脂がエポキシ樹脂、シリコーン樹脂、及びフッ素を含む樹脂からなる群から選ばれる１種以上であることを特徴とする前記の樹脂組成物である。 Further, the present invention is the above resin composition, characterized in that the phosphor is made of oxynitride, and preferably the resin is selected from the group consisting of an epoxy resin, a silicone resin, and a resin containing fluorine. 1 or more types of said resin composition characterized by the above-mentioned.
更に、本発明は、前記の樹脂組成物を用いてなることを特徴とするＬＥＤである。加えて、本発明は、前記の樹脂組成物を用いてなることを特徴とするＬＥＤ用シートである。 Furthermore, the present invention is an LED comprising the resin composition described above. In addition, the present invention is an LED sheet characterized by using the above resin composition.
本発明の樹脂組成物は、蛍光体粉末と特定波長領域で光透過性を有する粒子とを樹脂中に含有するので、蛍光体粉末が少量配合される場合であっても、樹脂中に蛍光体粉末が均一に分散した樹脂組成物が得られるので、その結果、蛍光体の励起光並びに発光時の輝度のばらつきを低減でき、その結果、発光特性が長期に渡って安定であり、ＬＥＤを初めとするいろいろな照明装置の蛍光体として好適である。 Since the resin composition of the present invention contains phosphor powder and particles having light transmittance in a specific wavelength region in the resin, even if a small amount of the phosphor powder is blended, the phosphor in the resin As a result, a resin composition in which the powder is uniformly dispersed can be obtained. As a result, it is possible to reduce variations in the excitation light of the phosphor and the luminance at the time of light emission. As a result, the light emission characteristics are stable over a long period of time. It is suitable as a phosphor for various lighting devices.
本発明のＬＥＤは、前記発光特性に優れる樹脂組成物を用いているので、その特徴が反映されて、発光特性が長期に渡って安定である特徴を有している。 Since the LED of the present invention uses the resin composition having excellent light emission characteristics, the characteristics are reflected and the light emission characteristics are stable over a long period of time.
本発明のＬＥＤ用シートは、前記発光特性に優れる樹脂組成物を用いているので、例えば、ＬＥＤの前面に用いられて、ＬＥＤの波長変更、ＬＥＤ表面に発生する傷や汚れ等からの保護の機能を果たすことができる。 Since the LED sheet of the present invention uses the resin composition having excellent light emission characteristics, for example, the LED sheet is used on the front surface of the LED to protect the LED from wavelength changes, scratches and dirt generated on the LED surface, and the like. Can fulfill the function.
本発明に於いて、樹脂組成物からなる硬化体の中を通過する蛍光体粉末の励起光並びに発光光の波長領域で光透過性の粒子を前記蛍光体粉末と併用することで、蛍光体粉末が少量配合される場合においても、蛍光体粉末の樹脂中での均一分散が達成でき、その結果として、蛍光体の光学特性が極めて均質で安定なものにすることができる。 In the present invention, the phosphor powder is used together with the phosphor powder by using light-transmitting particles in the wavelength region of the excitation light and emission light of the phosphor powder passing through the cured body made of the resin composition. Even when a small amount is blended, uniform dispersion of the phosphor powder in the resin can be achieved, and as a result, the optical properties of the phosphor can be made extremely uniform and stable.
本発明に於いて、紫外光或いは青色光線を励起光として用い、前記励起光から黄色〜橙色に発光する蛍光体粉末と組み合わせて白色光を得ることを前提にすると、３００〜８００ｎｍの領域で光透過性の粒子を樹脂と蛍光体粉末とに組み合わせて用いることを特徴としている。光透過性の粒子として３５０〜６００ｎｍの領域で光透過性のものが好ましい。尚、本発明に於いて、光透過性であることは、前記波長領域においてある波長の光の透過率が９５％以上であることが好ましく、９９％以上であることが一層好ましい。 In the present invention, on the premise that white light is obtained by using ultraviolet light or blue light as excitation light and combining with the phosphor powder that emits yellow to orange light from the excitation light, light is emitted in the region of 300 to 800 nm. The transmissive particles are used in combination with resin and phosphor powder. The light transmissive particles are preferably light transmissive in the region of 350 to 600 nm. In the present invention, the light transmittance is preferably such that the transmittance of light having a certain wavelength in the wavelength region is 95% or more, and more preferably 99% or more.
光透過性の粒子について、その大きさは蛍光体粉末と混合しやすく、樹脂とも混合しやすい大きさであることが好ましく、発明者の検討結果によれば、比表面積値が３０ｍ２／ｇ以上であれば良く、５０ｍ２／ｇ以上であることが一層好ましい。また、上限値については、格別技術的な意味合いは認められないが、通常入手しやすさから４００ｍ２／ｇ以下のものが一応の制限となる。 The light-transmitting particles preferably have a size that can be easily mixed with the phosphor powder and can be easily mixed with the resin. According to the results of the inventors' investigation, the specific surface area value is 30 m 2 / g or more. It is sufficient that it is 50 m 2 / g or more. In addition, no special technical meaning is recognized for the upper limit value, but a value of 400 m 2 / g or less is a temporary restriction because of its normal availability.
光透過性の粒子の樹脂組成物中での添加量については、光透過性の粒子の種類、比表面積、比重、蛍光体の粒子の比重、粒子径、粒子形状、充填率、更に樹脂の粘度により適宜調整すれば良いが、一般的には、０．０３〜１０体積％が選択される。 Regarding the amount of light transmissive particles added in the resin composition, the type of light transmissive particles, specific surface area, specific gravity, specific gravity of phosphor particles, particle diameter, particle shape, filling rate, and resin viscosity However, it is generally selected from 0.03 to 10% by volume.
本発明に於いて、３５０〜６００ｎｍの領域で光透過性の粒子の具体的な例としては、酸化珪素、酸化アルミニウム、酸化チタン、酸化セリウム、酸化イットリウム、酸化亜鉛、酸化錫、ＩＴＯ（チタン酸インジウム）が挙げられ、本発明ではこれらを単独で、或いは２種以上を混合して用いることができる。 In the present invention, specific examples of the light transmissive particles in the region of 350 to 600 nm include silicon oxide, aluminum oxide, titanium oxide, cerium oxide, yttrium oxide, zinc oxide, tin oxide, ITO (titanic acid). Indium), and in the present invention, these can be used alone or in admixture of two or more.
また、前記光透過性の粒子うち、酸化珪素、酸化アルミニウムはいずれも、高純度でしかも球状の形状のものが入手しやすく、本発明の効果を達成しやすいので、好ましい。 Of the light-transmitting particles, silicon oxide and aluminum oxide are both preferable because they are highly pure and have a spherical shape and can easily achieve the effects of the present invention.
本発明に用いる樹脂としては、透明で、紫外線或いは可視光線を受けても長期に渡り光学特性の変化のないものが用いられ、本発明者の検討に拠れば、エポキシ樹脂、シリコーン樹脂、フッ素を含む樹脂が好ましく選択される。なお、これらの２種以上を混合した樹脂も勿論使用することができる。 As the resin used in the present invention, a resin that is transparent and does not change in optical properties over a long period of time even when it receives ultraviolet rays or visible light is used. According to the study of the present inventors, epoxy resin, silicone resin, fluorine are used. The resin to be included is preferably selected. Of course, a resin in which two or more of these are mixed can also be used.
尚、前記樹脂について、その硬化方法は、常温硬化、加熱硬化が知られているが、本発明の樹脂組成物の硬化に際しては、加熱硬化が蛍光体粉末の不均一化を防止する上で好ましい方法である。 As for the resin, curing methods of room temperature curing and heat curing are known, but when curing the resin composition of the present invention, heat curing is preferable in order to prevent non-uniformity of the phosphor powder. Is the method.
本発明に用いる蛍光体粉末については、紫外光或いは青色光線を励起光として用い、前記励起光から黄色〜橙色に発光する蛍光体粉末と組み合わせて白色光を得ることを前提にすると、紫外光或いは青色光線を励起光とし前記励起光から黄色〜橙色に発光する蛍光体の粉末が選択され、このような蛍光体粉末としてα型サイアロン等の酸窒化物からなる蛍光体粉末が知られている。また、前記蛍光体粉末は、色調調整のために、やはり紫外光或いは青色光線を励起光とするが、黄色〜橙色とは異なる色調の発光を呈する他の蛍光体粉末を含有することもできる。 As for the phosphor powder used in the present invention, ultraviolet light or blue light is used as excitation light, and it is assumed that white light is obtained in combination with the phosphor powder that emits yellow to orange light from the excitation light. A phosphor powder that emits yellow light to orange light from the excitation light using blue light as an excitation light is selected, and a phosphor powder made of an oxynitride such as α-sialon is known as such a phosphor powder. In addition, the phosphor powder uses ultraviolet light or blue light as excitation light for color tone adjustment, but may also contain other phosphor powder that emits light having a color tone different from yellow to orange.
蛍光体粉末の樹脂組成物中での配合割合は、光源の種類、蛍光体粉末がどのように光源に曝されるかという環境条件や、目標とする色調等により一概に定めることができないが、前記酸窒化物からなる蛍光体粉末を用いる場合には、０．５〜３０体積％が一般的である。 The blending ratio of the phosphor powder in the resin composition cannot be determined unconditionally depending on the type of light source, the environmental conditions of how the phosphor powder is exposed to the light source, the target color tone, etc. When the phosphor powder made of the oxynitride is used, the content is generally 0.5 to 30% by volume.
尚、蛍光体粉末、並びに光透過性の粒子を樹脂に分散させる方法としては、自転、公転を利用した攪拌方法が好ましい。攪拌羽根を使用する方法は、攪拌中に不純物が混入したり、樹脂中に気泡が含有しやすいので避けたほうが良い。 In addition, as a method of dispersing the phosphor powder and the light transmissive particles in the resin, a stirring method using rotation or revolution is preferable. The method using a stirring blade should be avoided because impurities are mixed during stirring or bubbles are easily contained in the resin.
本発明は、前記の樹脂組成物を用いてなることを特徴とするＬＥＤであり、紫外光或いは青色光線を発光するＬＥＤ等の光源の前方に、前記樹脂組成物の硬化体を配置する構造を有する。硬化体の厚みを適宜調整することにより、白色ＬＥＤを得ることができる。また、本発明のＬＥＤ用シートは、前記の樹脂組成物をシート状に成形し、硬化して得られるもので、前記の紫外光或いは青色光線を発光するＬＥＤ等の光源の前方に貼り付けることで容易にＬＥＤを得ることができる。又、予め蛍光体の配合量やシート厚みを調整しておくことで、容易に白色ＬＥＤを得ることができるし、得られたＬＥＤは表面が当該樹脂組成物硬化体で覆われるので、他部材と接触して傷が入り、その結果発光特性が劣化する等の問題発生を防止できる効果がある。 The present invention is an LED comprising the resin composition, and has a structure in which a cured body of the resin composition is disposed in front of a light source such as an LED that emits ultraviolet light or blue light. Have. A white LED can be obtained by appropriately adjusting the thickness of the cured body. In addition, the LED sheet of the present invention is obtained by molding the resin composition into a sheet shape and curing, and is pasted in front of a light source such as an LED that emits ultraviolet light or blue light. Thus, an LED can be easily obtained. Also, by adjusting the blending amount of phosphor and sheet thickness in advance, a white LED can be easily obtained, and the surface of the obtained LED is covered with the cured resin composition, so that other members There is an effect that it is possible to prevent the occurrence of problems such as scratches caused by contact with the substrate, resulting in deterioration of the light emission characteristics.
（実施例１）
エポキシ樹脂エピコート８２８（ジャパンエポキシレジン社製）８３．３ｍｌ（１００ｇ）に、平均粒子径１５μｍ（ＣＯＵＬＴＥＲ社製、ＬＳ２３０）のα型サイアロン蛍光体（電気化学工業社製）を７．７５ｍｌ（２４．８ｇ）、比表面積８０ｍ２／ｇの酸化珪素（電気化学工業社製、ＵＦＰ−８０）を０．８６ｍｌ（１．９ｇ）配合し、エポキシ樹脂硬化剤として、ジェファーミンＤ−４００（ＨＵＮＴＳＭＡＮ社製）を３９．２ｍｌ（３８．０ｇ）、並びにジェファーミンＤ−２０００（ＨＵＮＴＳＭＡＮ社製）を２５ｍｌ（２５．０ｇ）配合して、スーパーミキサーＡＲ−２５０（シンキー社製）で攪拌して樹脂組成物を得た。
Example 1
Epoxy resin Epicoat 828 (manufactured by Japan Epoxy Resin Co., Ltd.) 83.3 ml (100 g) and 7.75 ml (24. 8 g), 0.86 ml (1.9 g) of silicon oxide having a specific surface area of 80 m 2 / g (manufactured by Denki Kagaku Kogyo Co., Ltd., UFP-80) is blended, and Jeffamine D-400 (manufactured by HUNTSMAN Co., Ltd.) is used as an epoxy resin curing agent. ) 39.2 ml (38.0 g) and Jeffermin D-2000 (HUNTSMAN) 25 ml (25.0 g) were blended and stirred with Supermixer AR-250 (Sinky Corporation). Got.
前記樹脂組成物をガラス製のサンプル管瓶に流し込み、８０℃２時間、１２５℃３時間の加熱をし、硬化させた。硬化後、サンプル管瓶に流し込んだ樹脂組成物の上端部からサイアロン蛍光体が沈降して透明になった部分の距離を測定した。その結果、沈降距離が０ｍｍであり、沈降は発生しなかった。 The resin composition was poured into a glass sample tube bottle and heated at 80 ° C. for 2 hours and 125 ° C. for 3 hours to be cured. After curing, the distance from the upper end of the resin composition poured into the sample tube bottle to the portion where the sialon phosphor settled and became transparent was measured. As a result, the settling distance was 0 mm, and no settling occurred.
（実施例２）
ガラス板上に塗布し、硬化後の厚さが５０μｍとなるように実施例１の樹脂組成物を塗布し、８０℃２時間、１２５℃３時間の加熱をし、硬化させてシートを作製した。
(Example 2)
The sheet was coated on a glass plate, coated with the resin composition of Example 1 so that the thickness after curing was 50 μm, heated at 80 ° C. for 2 hours and 125 ° C. for 3 hours, and cured to prepare a sheet. .
これを青色ＬＥＤの発光面に貼り付けたところ、白色光が得られた。 When this was affixed to the light emitting surface of a blue LED, white light was obtained.
（実施例３）青色ＬＥＤの発光面に実施例１の樹脂組成物を硬化後の厚さが５０μｍとなるように塗布し、８０℃２時間、１２５℃３時間の加熱をしてＬＥＤを得た。これを動作させたところ、白色に発光した。 (Example 3) The resin composition of Example 1 was applied to the light emitting surface of a blue LED so that the thickness after curing was 50 μm, and the LED was obtained by heating at 80 ° C. for 2 hours and at 125 ° C. for 3 hours. It was. When this was operated, white light was emitted.
（比較例）
エポキシ樹脂エピコート８２８（ジャパンエポキシレジン社製）８３．３ｍｌ（１００ｇ）に、平均粒子径１５μｍ（ＣＯＵＬＴＥＲ社製、ＬＳ２３０）のα型サイアロン蛍光体（電気化学工業社製）を８．５９ｍｌ（２７．５ｇ）配合し、エポキシ樹脂硬化剤として、ジェファーミンＤ−４００（ＨＵＮＴＳＭＡＮ社製）を３９．２ｍｌ（３８．０ｇ）、並びにジェファーミンＤ−２０００（ＨＵＮＴＳＭＡＮ社製）を２５ｍｌ（２５．０ｇ）配合して、スーパーミキサーＡＲ−２５０（シンキー社製）で攪拌して、ガラス製のサンプル管瓶に流し込み、８０℃２時間、１２５℃３時間加熱し、硬化させた。実施例１と同じように、サンプル管瓶に流し込んだ樹脂組成物の上端部からサイアロン蛍光体が沈降して透明になった部分の距離を測定した。その結果、沈降距離が５ｍｍであり、沈降が発生した。
(Comparative example)
Epoxy resin Epicoat 828 (manufactured by Japan Epoxy Resin Co., Ltd.) 83.3 ml (100 g) and 8.59 ml (27. 5g), 39.2 ml (38.0 g) of Jeffermin D-400 (manufactured by HUNTSMAN) and 25 ml (25.0 g) of Jeffermin D-2000 (manufactured by HUNTSMAN) as an epoxy resin curing agent Then, the mixture was stirred with a super mixer AR-250 (manufactured by Sinky), poured into a glass sample tube, heated at 80 ° C. for 2 hours, and 125 ° C. for 3 hours to be cured. As in Example 1, the distance from the upper end of the resin composition poured into the sample tube bottle to the portion where the sialon phosphor settled and became transparent was measured. As a result, the sedimentation distance was 5 mm and sedimentation occurred.
本発明の樹脂組成物は、樹脂中に蛍光体粉体が少量配合される場合であっても、均一に分散している特徴を有するので、当該樹脂組成物の硬化体は、発光特性が長期に渡って安定であり、ＬＥＤを初めとするいろいろな照明装置の蛍光体として好適であり、産業上極めて有用である。 Since the resin composition of the present invention has a characteristic of being uniformly dispersed even when a small amount of phosphor powder is blended in the resin, the cured product of the resin composition has a long-term emission characteristic. Therefore, it is suitable as a phosphor for various lighting devices including LEDs and is extremely useful in the industry.
本発明のＬＥＤは、前記発光特性に優れる樹脂組成物を用いているので、その特徴が反映されて、発光特性が長期に渡って安定である特徴を有しているので、産業上有用である。 Since the LED of the present invention uses the resin composition having excellent light emission characteristics, the characteristics are reflected and the light emission characteristics are stable over a long period of time, which is industrially useful. .
本発明のＬＥＤ用シートは、前記発光特性に優れる樹脂組成物を用いているので、例えば、ＬＥＤの前面に用いられて、ＬＥＤの波長変更、ＬＥＤ表面に発生する傷や汚れ等からの保護の機能を果たすことができるので、産業上有用である。 Since the LED sheet of the present invention uses the resin composition having excellent light emission characteristics, for example, the LED sheet is used on the front surface of the LED to protect the LED from wavelength changes, scratches and dirt generated on the LED surface, and the like. Since it can fulfill its function, it is industrially useful.
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| JP2005279855A JP2007095770A (en) | 2005-09-27 | 2005-09-27 | Resin composition and LED using the same |
| KR1020077029117A KR101201266B1 (en) | 2005-06-14 | 2006-06-14 | Resin composition and sheet containing phosphor, and light emitting element using such composition and sheet |
| PCT/JP2006/311955 WO2006134982A1 (en) | 2005-06-14 | 2006-06-14 | Resin composition and sheet containing phosphor, and light emitting element using such composition and sheet |
| CN2010101651406A CN101851432B (en) | 2005-06-14 | 2006-06-14 | Phosphor-containing resin composition and sheet, and light-emitting device using same |
| EP09004769.7A EP2075288B1 (en) | 2005-06-14 | 2006-06-14 | Resin composition and sheet containing phosphor, and light emitting element using such composition and sheet |
| CN2006800206991A CN101193983B (en) | 2005-06-14 | 2006-06-14 | Phosphor-containing resin composition and sheet, and light-emitting device using same |
| EP06766724.6A EP1892268B1 (en) | 2005-06-14 | 2006-06-14 | Resin composition and sheet containing phosphor, and light emitting element using such composition and sheet |
| KR1020127021881A KR20120109645A (en) | 2005-06-14 | 2006-06-14 | Resin composition and sheet containing phosphor, and light emitting element using such composition and sheet |
| US11/917,513 US8497623B2 (en) | 2005-06-14 | 2006-06-14 | Phosphor-containing resin composition and sheet, and light emitting devices employing them |
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| JP2005136379A (en) * | 2003-10-08 | 2005-05-26 | Nichia Chem Ind Ltd | Semiconductor device |
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| JP2005136379A (en) * | 2003-10-08 | 2005-05-26 | Nichia Chem Ind Ltd | Semiconductor device |
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