JPWO2019021926A1 - 光学部材用樹脂シート、それを備える光学部材、積層体又は発光デバイス、及び光学部材用樹脂シートの製造方法 - Google Patents
光学部材用樹脂シート、それを備える光学部材、積層体又は発光デバイス、及び光学部材用樹脂シートの製造方法 Download PDFInfo
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- JPWO2019021926A1 JPWO2019021926A1 JP2019532546A JP2019532546A JPWO2019021926A1 JP WO2019021926 A1 JPWO2019021926 A1 JP WO2019021926A1 JP 2019532546 A JP2019532546 A JP 2019532546A JP 2019532546 A JP2019532546 A JP 2019532546A JP WO2019021926 A1 JPWO2019021926 A1 JP WO2019021926A1
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Abstract
Description
(A)酸化物系蛍光体、酸窒化物系蛍光体、窒化物系蛍光体、硫化物系蛍光体、フッ化物系蛍光体及び酸硫化物系蛍光体から選ばれる1種類又は2種類以上の蛍光体、並びに
(B)分子内にRASiO3/2(式中、RAは炭素原子数6〜14のアリール基である)で表されるアリールシロキサン単位及び(R2SiO2/2)n(式中、Rはハロゲン原子で置換されてもよい炭素原子数1〜20のアルキル基又は炭素原子数6〜14のアリール基であり、nは3〜1000の範囲の数である)で表されるポリジオルガノシロキサン構造を有するオルガノポリシロキサン
を含むことが好ましい。
(A)酸化物系蛍光体、酸窒化物系蛍光体、窒化物系蛍光体、硫化物系蛍光体、フッ化物系蛍光体、及び酸硫化物系蛍光体から選ばれる1種類又は2種類以上の蛍光体、並びに
(B)分子内にRASiO3/2(式中、RAは炭素原子数6〜14のアリール基である)で表されるアリールシロキサン単位及び(R2SiO2/2)n(式中、Rはハロゲン原子で置換されてもよい炭素原子数1〜20のアルキル基又は炭素原子数6〜14のアリール基であり、nは3〜1000の範囲の数である)で表されるポリジオルガノシロキサン構造を有するオルガノポリシロキサン
を含むことが好ましい。
{(R2SiO2/2)}a{RASiO3/2}1−a
で表されるオルガノポリシロキサンであることが好ましい。式中、R及びRAは前記同様の基であり、aは0.8〜0.2の範囲の数であり、より好適には、0.8〜0.4の範囲の数である。
例2: 基材/剥離層/本発明の光学部材用樹脂シート/その他の任意の層/剥離層/基材
合成例1
2Lの四ツ口丸底フラスコにフェニルシルセスキオキサン加水分解物(324g、2.37molのSi)とプロピオン酸プロピル(275g)を入れて混合した。窒素雰囲気下で、当該混合物を還流させながら30分にわたって加熱し反応させた。反応混合物を100℃に冷却した後、ジアセトキシ末端ポリフェニルメチルシロキサン(シロキサン重合度:170)のプロピオン酸プロピル溶液(66%、610.8g)を加えた。2時間加熱還流した後、一晩放置した。ビニルメチルジアセトキシシラン(21g、0.11molのSi)を加え、混合物を1時間にわたって還流させた後、水(57mL)を加え、共沸脱水することにより酢酸濃度を低下させた。得られた反応混合物を100℃に冷却した後、メチルトリアセトキシシランとエチルトリアセトキシランの1:1混合物(38.7g、0.17molのSi)を加え、1時間にわたって還流させた。水(57mL)を加え、共沸脱水することにより酢酸濃度を低下させた。この操作をさらに2回繰り返した後、プロピオン酸プロピルを一部留去することにより、透明なレジン−リニアポリマー構造を有するオルガノポリシロキサンのプロピオン酸プロピル溶液(重量平均分子量:83000、固形分濃度:74.2%)を得た。
2Lの四ツ口丸底フラスコにフェニルシルセスキオキサン加水分解物(324g、2.37molのSi)とトルエン(268g)を入れて混合した。窒素雰囲気下で、当該混合物を還流させながら30分にわたって加熱し反応させた。反応混合物を100℃に冷却した後、ジアセトキシ末端ポリフェニルメチルシロキサン(シロキサン重合度:100)のトルエン溶液(65%、608g)を加えた。反応混合物を還流させながら2時間にわたって加熱した後、メチルトリアセトキシシラン(38g、0.17molのSi)を加え、混合物を2.5時間にわたって還流させた。ビニルメチルジアセトキシシラン(21g、0.11molのSi)を加え、混合物を2時間にわたって還流させた後、水(76mL)を加え、30分共沸させ、有機層が分離するのを待ってから水層を下から除去した。次に水を飽和食塩水に置き換え、これと同様の手順を更に2回繰り返して酢酸濃度を低下させた後、同様の手順をさらに水で2回繰り返した。トルエンを一部留去することにより、透明なレジン−リニアポリマー構造を有するオルガノポリシロキサンのトルエン溶液(重量平均分子量:60000、固形分濃度:75.8%)を得た。このトルエン溶液をロータリーエバポレーターを用いて、プロピオン酸プロピルを加えてはトルエンを除くことを3回繰り返して、透明なレジン−リニアポリマー構造を有するオルガノポリシロキサンのプロピオン酸プロピル溶液(固形分濃度:78%)を得た。
実施例1
上記合成例1により得られた溶液8.0g、蛍光体(インテマティックス社製、NYAG 4454−L)5.93g、シリカ粒子(デンカ社製、FB−5SDC、平均粒径:5μm)9.59g、及びプロピオン酸プロピル3.25gを混合し、真空脱気機構を備えた自公転式撹拌機(シンキー社製、ARV−310LED)を用いて均一になるまで撹拌し、樹脂シート用組成物1を得た。粘度は2173mPa・s(10 1/s)と5105mPa・s(1 1/s)を有するチクソ性溶液であった。ダイセルバリューコーティング社製のT788 PETフィルムに塗工機(PI−1210 FILM COATER)を用いて、井元製作所製フレームアプリケーター(IMC−3501型)により260μmのギャップでコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅150mm×長さ310mmの長方形シートであった。
上記合成例1により得られた溶液8.0g、蛍光体(インテマティックス社製、NYAG 4454−L)15.53g、及びプロピオン酸プロピル1.75gを混合し、真空脱気機構を備えた自公転式撹拌機(シンキー社製、ARV−310LED)を用いて均一になるまで撹拌し、樹脂シート用組成物2を得た。粘度は3269mPa・s(10 1/s)であった。ダイセルバリューコーティング社製のT788 PETフィルムに塗工機(PI−1210 FILM COATER)を用いて、井元製作所製フレームアプリケーター(IMC−3501型)により253μmのギャップでコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅150mm×長さ310mmの長方形シートであった。
上記合成例1により得られた溶液40.0g及び蛍光体(インテマティックス社製、NYAG 4454−S)7.56gを混合し、真空脱気機構を備えた自公転式撹拌機(シンキー社製、ARV−310LED)を用いて均一になるまで撹拌し、樹脂シート用組成物3を得た。粘度は10573mPa・s(10 1/s)であった。ダイセルバリューコーティング社製のT788 PETフィルムに塗工機(PI−1210 FILM COATER)を用いて、井元製作所製フレームアプリケーター(IMC−3501型)により236μmのギャップでコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅150mm×長さ310mmの長方形シートであった。
上記合成例1により得られた溶液40.0g、蛍光体(インテマティックス社製、NYAG 4454−S)7.33g、及びレオロシール(DM−30)0.25gを混合し、真空脱気機構を備えた自公転式撹拌機(シンキー社製、ARV−310LED)を用いて均一になるまで撹拌し、樹脂シート用組成物4を得た。粘度は11988mPa・s(10 1/s)であった。ダイセルバリューコーティング社製のT788 PETフィルムに塗工機(PI−1210 FILM COATER)を用いて、井元製作所製フレームアプリケーター(IMC−3501型)により236μmのギャップでコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅160mm×長さ310mmの長方形シートであった。
上記合成例2により得られた溶液40.0g及び酸化チタン(SX−3103、平均0.2μmD)20.12gを混合し、真空脱気機構を備えた自公転式撹拌機(シンキー社製、ARV−310LED)を用いて均一になるまで撹拌し、樹脂シート用組成物5を得た。粘度は9554mPa・s(10 1/s)であった。樹脂シート用組成物5を、ダイセルバリューコーティング社製のT788 PETフィルムに塗工機(PI−1210 FILM COATER)を用いて、井元製作所製フレームアプリケーター(IMC−3501型)により254μmのギャップでコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅160mm×長さ310mmの長方形シートであった。
実施例3で調製した樹脂シート用組成物3を、バー(R.D.Specialties社製、No.10)を用いて、剥離シート(ダイセル社製 T788)上にコートした。その後、コートされたシートを70℃のオーブンで30分間乾燥した。得られたシートは幅150mm×長さ300mmの長方形シートであった。
2 チャンバ
3 スロット
4 ステージ
5 固定台
6 可動部
7 可動部
Claims (18)
- シートの幅方向について、シート末端の厚みとシート中央の厚みの差がシートの総膜厚に対して5.0%以内であり、シート中央の厚みが10〜1000μmの範囲であり、かつ、シート面積が225mm2以上であり、少なくとも1種類以上の蛍光体又は反射材を含有することを特徴とする、光学部材用樹脂シート。
- 前記シートの幅及び長さがそれぞれ15mm以上であり、前記シート面積が400mm2以上である、請求項1に記載の光学部材用樹脂シート。
- 前記シート中央の厚みが30〜900μmの範囲であり、シートの幅方向について、シート末端の厚みとシート中央の厚みの差がシートの総膜厚に対して2.5%以内である、請求項1又は2に記載の光学部材用樹脂シート。
- 前記蛍光体又は反射材が、シートの総重量に対して10〜90質量%の範囲で含まれる、請求項1から3のいずれか1項に記載の光学部材用樹脂シート。
- 前記蛍光体又は反射材が、少なくともシリコーン樹脂を含有するバインダー樹脂中に分散された構造を有する、請求項1から4のいずれか1項に記載の光学部材用樹脂シート。
- 加熱溶融性を有することを特徴とする、請求項1から5のいずれか1項に記載の光学部材用樹脂シート。
- (A)酸化物系蛍光体、酸窒化物系蛍光体、窒化物系蛍光体、硫化物系蛍光体、フッ化物系蛍光体及び酸硫化物系蛍光体から選ばれる1種類又は2種類以上の蛍光体、並びに
(B)分子内にRASiO3/2(式中、RAは炭素原子数6〜14のアリール基である)で表されるアリールシロキサン単位及び(R2SiO2/2)n(式中、Rはハロゲン原子で置換されてもよい炭素原子数1〜20のアルキル基又は炭素原子数6〜14のアリール基であり、nは3〜1000の範囲の数である)で表されるポリジオルガノシロキサン構造を有するオルガノポリシロキサン
を含む、請求項1から6のいずれか1項に記載の光学部材用樹脂シート。 - 成分(A)が、シートの総重量に対して10〜90質量%の範囲で含まれる、請求項7に記載の光学部材用樹脂シート。
- 成分(B)が、少なくとも成分(A)を含む固体粒子成分のバインダー樹脂であり、かつ、{(R2SiO2/2)}a{RASiO3/2}1−a(式中、R及びRAは前記同様の基であり、aは0.8〜0.2の範囲の数である)で表されるオルガノポリシロキサンである、請求項7又は8に記載の光学部材用樹脂シート。
- 前記蛍光体又は反射材の少なくとも一部が、有機ケイ素化合物により表面処理されている、請求項1から9のいずれか1項に記載の光学部材用樹脂シート。
- 前記反射材が、酸化チタン、酸化バリウム、酸化クロム、酸化鉄、窒化ホウ素、及び窒化チタンから選ばれる1種類又は2種類以上である、請求項1から10のいずれか1項に記載の光学部材用樹脂シート。
- (C)シリカ粒子をさらに含む、請求項1から11のいずれか1項に記載の光学部材用樹脂シート。
- 請求項1から12のいずれか1項に記載の光学部材用樹脂シートを備える、光学部材。
- 請求項1から12のいずれか1項に記載の光学部材用樹脂シートを備える、積層体。
- 剥離層をさらに備える、請求項14に記載の積層体。
- 請求項1から12のいずれか1項に記載の光学部材用樹脂シートにより封止された構造を有する、発光デバイス。
- 光学部材用樹脂シートの原料を25℃における粘度10〜10,000mPa・s、ウエット状態での膜厚が10〜1000μmとなる条件で、シート塗布製造機によって基材上に塗布して製造されたことを特徴とする、請求項1から12のいずれか1項に記載の光学部材用樹脂シートの製造方法。
- 前記シート塗布製造機としてスリットコーターを用い、塗布速度w(cm/sec)の条件において、液圧立ち上がり時間を1.0/w sec以下の条件で製造されたことを特徴とする、請求項17に記載の光学部材用樹脂シートの製造方法。
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