JP5966692B2 - 蛍光体シート形成用樹脂組成物 - Google Patents
蛍光体シート形成用樹脂組成物 Download PDFInfo
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- JP5966692B2 JP5966692B2 JP2012151246A JP2012151246A JP5966692B2 JP 5966692 B2 JP5966692 B2 JP 5966692B2 JP 2012151246 A JP2012151246 A JP 2012151246A JP 2012151246 A JP2012151246 A JP 2012151246A JP 5966692 B2 JP5966692 B2 JP 5966692B2
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 177
- 239000011342 resin composition Substances 0.000 title claims description 78
- 239000010410 layer Substances 0.000 claims description 37
- 229920001577 copolymer Polymers 0.000 claims description 23
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- 238000007789 sealing Methods 0.000 claims description 15
- 239000012790 adhesive layer Substances 0.000 claims description 14
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000002356 single layer Substances 0.000 claims description 7
- 229920006132 styrene block copolymer Polymers 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims 1
- 125000000101 thioether group Chemical group 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 18
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 12
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- MHCLJIVVJQQNKQ-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical compound CCOC(N)=O.CC(=C)C(O)=O MHCLJIVVJQQNKQ-UHFFFAOYSA-N 0.000 description 6
- 230000031700 light absorption Effects 0.000 description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
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- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- RIWRBSMFKVOJMN-UHFFFAOYSA-N 2-methyl-1-phenylpropan-2-ol Chemical compound CC(C)(O)CC1=CC=CC=C1 RIWRBSMFKVOJMN-UHFFFAOYSA-N 0.000 description 1
- ROGIWVXWXZRRMZ-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1 ROGIWVXWXZRRMZ-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
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- 239000005058 Isophorone diisocyanate Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
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- 239000004721 Polyphenylene oxide Substances 0.000 description 1
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- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical class C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- KOMDZQSPRDYARS-UHFFFAOYSA-N cyclopenta-1,3-diene titanium Chemical compound [Ti].C1C=CC=C1.C1C=CC=C1 KOMDZQSPRDYARS-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
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- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
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- MGFYSGNNHQQTJW-UHFFFAOYSA-N iodonium Chemical compound [IH2+] MGFYSGNNHQQTJW-UHFFFAOYSA-N 0.000 description 1
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
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- 229920002492 poly(sulfone) Polymers 0.000 description 1
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- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
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- 229920000570 polyether Polymers 0.000 description 1
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- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
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Description
成膜用樹脂組成物が、スチレン単位の割合が20〜30質量%であり、かつ水添率が95%以上のスチレン−エチレン−ブチレン−スチレン共重合体を含有し、
蛍光体が、硫化物系蛍光体を含有する蛍光体シート形成用樹脂組成物を提供する。
(赤色蛍光体シート形成用樹脂組成物の調製)
トルエン100質量部と、スチレン−エチレン−ブチレン−スチレンブロック(SEBS)共重合体(セプトンV9827、(株)クラレ)40質量部とを均一に混合し、得られた混合物に、平均粒径9μmのCaS:Eu(硫化物系赤色蛍光体)4質量部を均一に分散させることにより、赤色発光の蛍光体シート形成用樹脂組成物を調製した。
厚さ25μmのポリエチレンテレフタレートフィルム(T11、東レ(株))に、蛍光体シート形成用樹脂組成物を乾燥厚で25μmとなるように塗布し、乾燥処理(100℃、5分)して蛍光体層を形成した。その蛍光体層上に厚さ38μmのポリエチレンテレフタレートフィルム(A4300、東洋紡(株))を積層し、熱圧着処理(100℃、0.2MPa)を行うことにより図1の構造の蛍光体シートを得た。
厚さ25μmのポリエチレンテレフタレートフィルム(T−11、東レ(株))の片面に厚さ20〜25μmのポリオレフィン系接着層(セプトンV9827、(株)クラレ)を形成した。このポリエチレンテレフタレートフィルムの他面に、ウレタン系接着層が形成された表面保護フィルムを、ウレタン系接着層を介して積層することにより封止フィルムを作成した。表面保護フィルムは、厚さ約20nmの酸化ケイ素蒸着層が形成された厚さ12μmのポリエチレンテレフタレートフィルム(テックバリア、三菱樹脂(株))の当該酸化ケイ素蒸着層上に、厚さ1〜2μmのウレタン系接着層を形成することにより作成したものである。得られた封止フィルムの透湿度は0.3g/m2・24hr・atmであった。
図1の構造の蛍光体シートの両面に封止フィルムを配し、熱圧着処理(100℃、0.2Pa)することにより、封止フィルムで封止された蛍光体シートを得た。
(赤色発光の蛍光体シート形成用樹脂組成物の調製)
トルエン100質量部と、スチレン−エチレン−ブチレン−スチレンブロック(SEBS)共重合体(セプトンV9827、(株)クラレ)40質量部とを均一に混合し、得られた混合物に、平均粒径9μmのCaS:Eu(硫化物系赤色蛍光体)4質量部を均一に分散させることにより、赤色発光の蛍光体シート形成用樹脂組成物を調製した。
光硬化型のウレタンメタクリレート(アロニックス M1600、東亜合成(株))100質量部に、光重合開始剤(BASF社製、ダロキュア1173)0.5質量部、平均粒径6μmのSrGa2S4:Eu(硫化物系蛍光体)を1.5質量部、均一に分散させることにより、緑色発光の蛍光体シート形成用組成物を調整した。
厚さ25μmのポリエチレンテレフタレートフィルム(T11、東レ(株))に、緑色蛍光体シート形成用樹脂組成物を乾燥厚が115μmとなるように塗布した後に、紫外線を照射して(7000mJ/cm2)、ウレタンメタクリレートを重合させることにより、蛍光体層を形成した。その上に厚さ38μmの透明セパレータ(ポリエチエレンテレフタレートフィルム(A4300、東洋紡(株)))を積層し、熱圧着処理(100℃、20Pa)した。処理後の透明セパレータ上に、赤色蛍光体シート形成用樹脂組成物を乾燥厚で30μmとなるように塗布し、乾燥処理(100℃、5分)して蛍光体層を形成し、その上に更に、厚さ25μmのポリエチレンテレフタレートフィルムを積層し、熱圧着処理(100℃、0.2MPa)することにより図2の構造の蛍光体シートを得た。
図2の構造の蛍光体シートの両面に、実施例1で使用したものと同じ封止フィルムを配し、熱圧着処理(100℃、0.2MPa)することにより、封止フィルムで封止された蛍光体シートを得た。
SEBS共重合体に代えて、実施例2で使用した光硬化型のウレタンメタクリレートを使用すること以外、実施例1と同様にして蛍光体シート形成用樹脂組成物を調製し、図1、更に図3の構造の蛍光体シートを製造した。
SEBS共重合体に代えて、実施例2で使用した光硬化型のウレタンメタクリレートを使用すること以外、実施例2と同様にして蛍光体シート形成用樹脂組成物を調製し、図2、更に図4の構造の蛍光体シートを製造した。
赤色発光の蛍光体シート形成用樹脂組成物におけるSEBS共重合体に代えて、BMA-GMA共重合体(DF−242、藤倉化成(株))を使用すること以外、実施例1と同様にして蛍光体シート形成用樹脂組成物を調製し、図1、更に図3の構造の蛍光体シートを製造した。
各実施例及び各比較例の封止された蛍光体シートについて、以下のように色度差と発光スペクトル強度比とを測定し、評価した。得られた結果を表1に示す。
得られた封止された蛍光体シートを、60℃、90%Rhの環境中に500時間放置した。放置前後の色度差(JIS Z8518)Δu′v′を求め、以下の基準で評価した。
A: Δu′v′<0.005
B: 0.005≦Δu′v′<0.010
C: 0.010≦Δu′v′
得られた封止された蛍光体シートを、85℃、85%Rhの環境中に48時間放置し、放置前と放置後の発光スペクトル強度(SR)を分光放射計(トプコンSR−3、(株)トプコン)を用いて測定し、放置前の発光スペクトル強度(SR)に対する放置後の発光スペクトル強度(SR)の比を求め、以下の基準で評価した。実用上、SR比は0.7以上が望まれ(A評価)、実用上0.5以上(B評価)が必要である。
A: 0.7≦SR比
B: 0.5≦SR比<0.7
C: SR比<0.5
2、2a、2b 透明基材
3 透明セパレータ
10 蛍光体シート
20 積層蛍光体層
30a、30b 封止フィルム
31 ベースフィルム
32 接着層
33 酸化ケイ素層
34 表面保護フィルム
Claims (9)
- 成膜用樹脂組成物と、励起光の照射により蛍光を発する粉末状の蛍光体とを含有する蛍光体シート形成用樹脂組成物であって、
成膜用樹脂組成物が、スチレン単位の割合が20〜30質量%であり、かつ水添率が95%以上のスチレン−エチレン−ブチレン−スチレン共重合体を含有し、
蛍光体が、硫化物系蛍光体を含有する蛍光体シート形成用樹脂組成物。 - 成膜用樹脂組成物中のスチレン−エチレン−ブチレン−スチレンブロック共重合体の含有割合が、20〜30質量%である請求項1記載の蛍光体シート形成用樹脂組成物。
- 蛍光体が、青色励起光の照射により620〜660nmの赤色蛍光ピークを有する硫化物系蛍光体である請求項1又は2記載の蛍光体シート形成用樹脂組成物。
- 硫化物系蛍光体が、CaS:Euである請求項1〜3のいずれかに記載の蛍光体シート形成用樹脂組成物。
- 励起光の照射により蛍光を発する蛍光体層が一対の透明基材に挟持されている蛍光体シートであって、蛍光体層が、請求項1〜4のいずれかに記載の蛍光体シート形成用樹脂組成物を成膜したものである蛍光体シート。
- 蛍光体層が、透明セパレータの片面に請求項1〜4のいずれかに記載の蛍光体シート形成用樹脂組成物を単層で成膜した赤色蛍光体層と、透明セパレータの他面に青色励起光の照射により530〜550nmの緑色蛍光ピークを有する緑色蛍光体層が積層された構造となっている請求項5記載の蛍光体シート。
- 緑色蛍光体層が、蛍光体としてSrGa2S4:Euを含有するものである請求項6記載の蛍光体シート。
- 片面に接着層を有する封止フィルム2枚で、更に、両側から封止した請求項5〜7のいずれかに記載の蛍光体シート。
- 請求項5〜8のいずれかに記載の蛍光体シートと、蛍光体シートに照射する励起光を発する励起光源とを有する発光装置。
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