JP5741811B2 - 発光素子向け増反射透明膜用組成物、発光素子、および発光素子の製造方法 - Google Patents
発光素子向け増反射透明膜用組成物、発光素子、および発光素子の製造方法 Download PDFInfo
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- JP5741811B2 JP5741811B2 JP2011037726A JP2011037726A JP5741811B2 JP 5741811 B2 JP5741811 B2 JP 5741811B2 JP 2011037726 A JP2011037726 A JP 2011037726A JP 2011037726 A JP2011037726 A JP 2011037726A JP 5741811 B2 JP5741811 B2 JP 5741811B2
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating
- H01L33/46—Reflective coating, e.g. dielectric Bragg reflector
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
Description
(1)発光層と、透光性基板と、増反射透明膜と、発光層からの発光を反射する反射膜とを、この順に備える発光素子向け増反射透明膜用組成物であって、増反射透明膜用組成物が、透光性バインダーを含むことを特徴とする、発光素子向け増反射透明膜用組成物。
(2)さらに、透明粒子を含む、上記(1)記載の発光素子向け増反射膜透明膜用組成物。
(3)発光層と、透光性基板と、増反射透明膜と、発光層からの発光を反射する反射膜とを、この順に備える発光素子であって、増反射透明膜が、透光性バインダーを含むことを特徴とする、発光素子。
(4)増反射膜用透明膜が2層からなり、透光性基板側の増反射膜用透明膜の屈折率が、反射膜側の増反射膜用透明膜の屈折率より低い、上記(3)記載の発光素子。
(5)さらに、反射膜が、増反射膜用透明膜の反対面に、バインダーを含む保護膜を備える、上記(3)または(4)記載の発光素子。
(6)増反射透明膜および/または反射膜が、湿式塗工法で製造される、上記(3)〜(5)のいずれか記載の発光素子。
(7)透光性基板上に、透光性バインダーを含む増反射透明膜用組成物を湿式塗工法により塗布した後、焼成または硬化することにより増反射透明膜を形成し、形成した増反射透明膜上に、金属ナノ粒子と添加物を含む反射膜用組成物を、湿式塗工法により塗布した後、焼成または硬化することにより反射膜を形成し、透光性基板の反射膜の反対面に発光層を形成することを特徴とする、発光素子の製造方法。
(8)反射膜を形成した後、発光層を形成する前に、さらに、反射膜上に、バインダーを含む保護膜用組成物を、湿式塗工法により塗布した後、焼成または硬化することにより保護膜を形成する、上記(7)記載の発光素子の製造方法。
本発明の発光素子向け増反射透明膜用組成物(以下、増反射透明膜用組成物という)は、発光層と、透光性基板と、増反射透明膜と、発光層からの発光を反射する反射膜とを、この順に備える発光素子向け増反射透明膜用組成物であって、増反射透明膜用組成物が、透光性バインダーを含むことを特徴とする。
高屈折率増反射透明膜用組成物には、上述の増反射透明膜用組成物を使用することができるが、以下、より屈折率が高い増反射透明膜用組成物の製造方法を説明する。
低屈折率増反射透明膜用組成物は、上記の透光性バインダー、透明導電性粒子を含み、さらに、シルセスキオキサン粒子(屈折率:1.15〜1.45)、およびフッ化マグネシウム粒子(屈折率:1.18〜1.38)からなる群より選ばれる少なくとも1種の透明粒子を含むと好ましい。低屈折透明粒子の平均粒径は、1〜50nmが好ましい。
発光素子向け反射膜用組成物(以下、反射膜用組成物という)は、金属ナノ粒子を含む。なお、反射膜は、発光素子の構造によっては電極の役割も要求される。
発光素子向け保護膜用組成物(以下、保護膜用組成物という)は、バインダーを含む。保護膜用組成物は、保護膜を形成することができ、また、反射膜に空孔がある場合には、反射膜に浸透し、反射膜の空孔および/または反射膜と増反射透明膜との界面に、バインダーを含有させ、反射膜自体の強度や反射膜と増反射透明膜との密着強度を高くすることができる。
増反射透明膜が、透光性基板と、反射膜との間に形成されると、発光素子から放出された光を反射する反射膜の反射率を高くし、発光素子の発光効率を高めることができる。増反射透明膜中の透光性バインダーは、上述のとおりであり、好ましくは、透明粒子、カップリング剤等を含む。
反射膜は、基体を通過した発光層の光を反射する。反射膜は、金属ナノ粒子を含み、さらに添加物を含むと好ましい。金属ナノ粒子、添加物は、上述のとおりである。
保護膜は、反射膜の耐熱性および耐食性を高くし、さらに、透光性基板と反射膜の密着性も高くし、発光素子の製造工程でダイシングを使用するときの反射膜の剥離を抑制する。保護膜は、バインダーを含み、バインダーは上述のとおりである。
密着層は、導電性反射膜と基材の間の密着性を向上させる。密着層の材質は、シランカップリング剤等が挙げられ、密着層の厚さは、0.005〜0.5μmであると好ましく、0.01〜0.3μmであると、より好ましい。密着層の厚さが、0.005μm以上であれば、密着力が十分であり、0.5μm以下であれば、経時変化が少ないためである。
本発明の発光素子の製造方法は、透光性基板上に、透光性バインダーを含む増反射透明膜用組成物を湿式塗工法により塗布した後、焼成または硬化することにより増反射透明膜を形成し、形成した増反射透明膜上に、金属ナノ粒子と添加物を含む反射膜用組成物を、湿式塗工法により塗布した後、焼成または硬化することにより反射膜を形成し、透光性基板の反射膜の反対面に発光層を形成することを特徴とする。ここで、増反射透明膜を、低屈折率増反射透明膜、高屈折率増反射透明膜の2層以上で構成する場合には、透光性基板上に、低屈折率増反射透明膜用組成物、高屈折率増反射透明膜用組成物の順に塗布すればよい。
50cm3のガラス製の4つ口フラスコを用い、140gのトリメチルメトキシシランと、140gのメチルアルコールを加え、攪拌しながら、1.7gの60%硝酸を120gの純水に溶解した溶液を、一度に加え、その後50℃で3時間反応させることにより、平均粒径:10nmのシルセスキオキサン球状粒子を製造した。
50cm3のガラス製の4つ口フラスコを用い、140gのテトラエトキシシランと、140gのエチルアルコールを加え、攪拌しながら、1.7gの60%硝酸を120gの純水に溶解した溶液を一度に加え、その後50℃で3時間反応させることにより、SiO2結合剤を製造した。
上記により作製したSiO2結合剤:10gと、平均粒径:25nmのITO粒子:3gと、エタノール:87gを、100cm3のガラス瓶中に入れ、直径:0.3mmのジルコニアビーズ(ミクロハイカ、昭和シェル石油製):100gを用いて、ペイントシェーカーで6時間分散することにより、SiO2結合剤およびITO粒子含有増反射透明膜用組成物(表1に、SiO2結合剤+ITOと記載)を作製した。
硝酸銀を脱イオン水に溶解して、金属塩水溶液を調製した。また、クエン酸ナトリウムを脱イオン水に溶解して、濃度が26質量%のクエン酸ナトリウム水溶液を調製した。このクエン酸ナトリウム水溶液に、35℃に保持された窒素ガス気流中で、粒状の硫酸第1鉄を直接加えて溶解させ、クエン酸イオンと第一鉄イオンを3:2のモル比で含有する還元剤水溶液を調製した。
銀ナノ粒子分散液を作製後、得られた金属ナノ粒子:10質量部を水、エタノール及びメタノールを含む混合溶液:90質量部に添加混合することにより分散させ、この分散液に、ポリビニルピロリドン(PVP、分子量:360,000)、金属ナノ粒子:96質量部、PVP:4質量部の割合となるように加えて、銀ナノ粒子およびPVP含有反射膜用組成物を作製した。
アクリル系にはネオペンチルグリコールジアクリレートを、エポキシ系にはビスフェノールA型エポキシ樹脂を、セルロース系にはメチルセルロースを、ウレタン系にはジフェニルメタンイソシアネートとメチルフェノールを使用した。
表1に示す構成の複合膜を作製した。まず、透光性基板としてのガラス基板上に、シルセスキオキサン含有増反射透明膜用組成物をスピンコーティングにより塗布し、窒素雰囲気中、160℃で20分焼成することにより、厚さ:25nmの低屈折率増反射透明膜を得た。ここで、膜厚の測定は、日立ハイテクノロジーズ製走査型電子顕微鏡(SEM、装置名:S−4300、SU−8000)による断面観察により測定した。他の実施例、比較例においても、膜厚を同様に測定した。同様にして、高屈折率増反射膜:25nmを形成した。次に、高屈折率増反射膜上に、銀ナノ粒子含有反射膜組成物をスピンコーティングにより塗布し、窒素雰囲気中、200℃で20分焼成することにより、反射膜を得た。
表1の構成にしたこと以外は、実施例1と同様にして、実施例2〜10の複合膜を作製した。ここで、保護膜は、保護膜用組成物をスピンコーティングにより塗布した後、SiO2結合剤の場合は、窒素雰囲気中、160℃で20分焼成し、それ以外の保護膜用塗膜は、窒素雰囲気中、150℃で15分焼成した。
ガラス基板に、真空成膜法のスパッタ法により、厚さ:100nmの銀薄膜を形成した。
ガラス基板に、スパッタ法により、厚さ:100nmの銀薄膜を形成し、さらにスパッタ法により、厚さ:30nmのチタン薄膜を形成した。
実施例1〜10、比較例1〜2の反射率の評価は、紫外可視分光光度計と積分球の組み合わせにより、波長450nmにおける反射膜の拡散反射率(初期反射率)を測定した。また、熱処理試験を、200℃、1000時間で、耐食性試験としての硫化試験を、硫化水素:10ppm、温度:25℃、相対湿度:75%RH、504時間行い、それぞれの試験後の反射率を測定した。表1に、これらの結果を示す。
10、11、12 反射膜
20、21、22 増反射透明膜
221 高屈折率増反射膜用透明膜
222 低屈折率増反射膜用透明膜
30、31、32 透光性基板
40、41、42 発光層
50、51、52 封止材
60、61、62 接着層
70、71、72 支持基板
81、82 保護膜
Claims (7)
- 発光層と、透光性基板と、厚さが20〜300nmの増反射透明膜と、発光層からの発光を反射する反射膜とを、この順に備える発光素子向け増反射透明膜用組成物であって、
増反射透明膜用組成物が、シルセスキオキサン球状粒子、またはシリコンのアルコキシドおよび硝酸触媒含有ノンポリマー型バインダーを含むことを特徴とする、発光素子向け増反射透明膜用組成物。 - 発光層と、透光性基板と、厚さが20〜300nmの増反射透明膜と、発光層からの発光を反射する反射膜とを、この順に備える発光素子であって、増反射透明膜が、シルセスキオキサン球状粒子を含む増反射透明膜用組成物、またはシリコンのアルコキシドおよび硝酸触媒含有ノンポリマー型バインダーを含む増反射透明膜用組成物から形成されたことを特徴とする、発光素子。
- 増反射膜用透明膜が2層からなり、透光性基板側の増反射膜用透明膜の屈折率が、反射膜側の増反射膜用透明膜の屈折率より低い、請求項2記載の発光素子。
- さらに、反射膜が、増反射膜用透明膜の反対面に、バインダーを含む保護膜を備える、請求項2または3記載の発光素子。
- 増反射透明膜および/または反射膜が、湿式塗工法で製造される、請求項2〜4のいずれか1項記載の発光素子。
- 透光性基板上に、シルセスキオキサン球状粒子を含む増反射透明膜用組成物、またはシリコンのアルコキシドおよび硝酸触媒含有ノンポリマー型バインダーを含む増反射透明膜用組成物を湿式塗工法により塗布した後、焼成または硬化することにより厚さが20〜300nmの増反射透明膜を形成し、形成した増反射透明膜上に、金属ナノ粒子と添加物を含む反射膜用組成物を、湿式塗工法により塗布した後、焼成または硬化することにより反射膜を形成し、透光性基板の反射膜の反対面に発光層を形成することを特徴とする、発光素子の製造方法。
- 反射膜を形成した後、発光層を形成する前に、さらに、反射膜上に、バインダーを含む保護膜用組成物を、湿式塗工法により塗布した後、焼成または硬化することにより保護膜を形成する、請求項6記載の発光素子の製造方法。
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KR102595727B1 (ko) | 2017-11-30 | 2023-10-30 | 악살타 코팅 시스템즈 게엠베하 | 고 전달 효율 어플리케이터를 활용하는 코팅 조성물의 적용을 위한 시스템 및 상응하는 방법 |
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JP4685169B2 (ja) * | 2007-07-11 | 2011-05-18 | 日本写真印刷株式会社 | 筐体用加飾板及び筐体 |
WO2009035112A1 (ja) * | 2007-09-12 | 2009-03-19 | Mitsubishi Materials Corporation | スーパーストレート型太陽電池用の複合膜及びその製造方法、並びにサブストレート型太陽電池用の複合膜及びその製造方法 |
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