JP2014024918A - 蛍光体シート - Google Patents
蛍光体シート Download PDFInfo
- Publication number
- JP2014024918A JP2014024918A JP2012165056A JP2012165056A JP2014024918A JP 2014024918 A JP2014024918 A JP 2014024918A JP 2012165056 A JP2012165056 A JP 2012165056A JP 2012165056 A JP2012165056 A JP 2012165056A JP 2014024918 A JP2014024918 A JP 2014024918A
- Authority
- JP
- Japan
- Prior art keywords
- phosphor
- coated
- silicon dioxide
- dioxide film
- sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 309
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 139
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 68
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 67
- 239000000843 powder Substances 0.000 claims abstract description 54
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 49
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 49
- 239000011342 resin composition Substances 0.000 claims abstract description 35
- 239000003505 polymerization initiator Substances 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
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- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 32
- 229910052717 sulfur Inorganic materials 0.000 abstract description 32
- 239000011593 sulfur Substances 0.000 abstract description 32
- 230000006866 deterioration Effects 0.000 abstract description 14
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- 238000005260 corrosion Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000010408 film Substances 0.000 description 106
- 239000010410 layer Substances 0.000 description 50
- 239000007789 gas Substances 0.000 description 31
- 239000000126 substance Substances 0.000 description 23
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- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 5
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
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- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
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- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 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
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/7731—Chalcogenides with alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7732—Halogenides
- C09K11/7733—Halogenides with alkali or alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77342—Silicates
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Abstract
【解決手段】蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有し、蛍光体のうち少なくとも硫化物蛍光体2が、金属酸化物粉末3を含む二酸化ケイ素膜4で被覆されてなる蛍光体含有樹脂組成物を用いる。これにより、蛍光体層の端部を露出させた蛍光体シートでも、硫黄系ガスの放出を防止することができ、さらに色度ズレを減少させることができる。
【選択図】図1
Description
1.被覆蛍光体
2.蛍光体含有樹脂組成物
3.蛍光体シート及びその製造方法
4.白色光源、照明装置への適用例
5.実施例
本実施の形態における被覆蛍光体は、蛍光体が二酸化ケイ素膜で被膜されている。これにより、蛍光体内部への水分の浸入を防止し、水分による蛍光体の劣化を防止することができる。また、蛍光体のうち少なくとも硫化物蛍光体は、金属酸化物粉末を含む二酸化ケイ素膜で被覆される。これにより、硫化物蛍光体の劣化による硫化水素や二酸化硫黄を主成分とする硫黄系ガスの放出を防止することができる。したがって、本実施の形態における被覆蛍光体を用いることにより、蛍光体含有樹脂組成物で形成される蛍光体層の色度ズレや、LED素子の電極等の腐食を抑制することができる。
本実施の形態における蛍光体含有樹脂組成物は、蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有し、蛍光体のうち少なくとも硫化物蛍光体が、金属酸化物粉末を含む二酸化ケイ素膜で被覆されている。青色LEDを用いて白色を発光させる場合、青色励起光の照射により波長590nm〜620nmの赤色蛍光ピークを有する赤色蛍光体と、青色励起光の照射により波長530nm〜550nmの緑色蛍光ピークを有する緑色蛍光体との混合蛍光体を使用することが好ましい。
次に、蛍光体含有樹脂組成物を使用した蛍光体シートについて、図面を参照しながら説明する。
前述した蛍光体含有樹脂組成物及び蛍光体シートは、例えば、白色光源や照明装置に適用することができる。
図11は、白色光源の一例を示す断面図である。図11に示すように、白色光源40は、素子基板41上に形成されたパッド部42上に青色発光素子43を有している。素子基板41には、青色発光素子43を駆動するための電力を供給する電極44,45が絶縁性を保って形成され、それぞれの電極44,45は、例えばリード線46,47によって青色発光素子43に接続されている。
図12は、照明装置の一例を示す正面図である。図12に示すように、照明装置60は、照明基板43上に図11を用いて説明した白色光源40が複数配置されている。その配置例は、例えば、図12(A)に示すように、正方格子配列としてもよく、または図12(B)に示すように、1行おきに例えば1/2ピッチずつずらした配列としてもよい。また、ずらすピッチは、1/2に限らず、1/3ピッチ、1/4ピッチであってもよい。さらには、1行ごとに、もしくは複数行(例えば2行)ごとにずらしてもよい。
以下、本発明の実施例について説明する。本実施例では、UV硬化系アクリル樹脂中に硫化物蛍光体が分散された蛍光体層を有する蛍光体シートを作製し、蛍光体シートの輝度及びCIE色度を測定し、色度ズレを評価した。また、蛍光体シートの硫黄系ガスの発生の有無を評価した。なお、本発明はこれらの実施例に限定されるものではない。
蛍光体シートの輝度及びCIE色度を、分光放射計(SR−3、トプソン社製)を用いて測定した。
蛍光体シートを60℃、90%RHの環境中に1000時間放置し、放置前後の白色度差(JIS Z8518)△u’v’を求めた。そして、ガス吸着剤が分散されていない蛍光体シートの△u’v’の値を1としたときの相対値を算出した。
硫黄系ガスの放出の指標として銀片試験を行った。直径15mm、厚さ2mmの銀片(JIS H 2141 「銀地金」に規定されている銀地金(純度99.95%以上))を金属研磨剤(ピカール、日本磨料工業社製)で研磨し、アセトン中で超音波洗浄した。超音波洗浄後の銀片を密閉ビン(100mlのガラス製秤量ビン)の蓋の裏に両面テープで張り付け、密閉ビン内部の底面上に、蛍光体シート(2cm×4cm)を置いた。湿度100%RHとするために、ガラスセルに水を加え、密閉ビンに入れた。また、密閉ビンの蓋を閉め、パラフィルム、ポリイミドテープで止め、85℃で168時間オーブンに入れた。168時間放置後の銀片の変色具合から硫黄系ガスの発生の有無を判断した。銀片が黒色に変化したものを×、銀片が茶色に変化したものを△、及び銀片が変色しなかったものを○と評価した。
樹脂容器(PE)に、赤色蛍光体((Ba,Sr)3SiO6:Eu)10g、エタノール80g、純水5g、28%のアンモニア水6gを投入し、マグネチックスターラーを投入し、40℃の恒温槽にて10分間攪拌後、テトラエトキシシラン5g、エタノール35gを投入した。投入が完了した時点を0分として3時間攪拌を行った。攪拌終了後、真空ポンプを用いて吸引濾過を行い、回収したサンプルをビーカーに移し、水やエタノールで洗浄後、再度濾過を行い、サンプルを回収した。回収したサンプルを85℃で2時間乾燥し、200℃で8時間焼成を行い、蛍光体が二酸化ケイ素膜で被覆された被覆赤色蛍光体を得た。
緑色蛍光体を被覆処理せずに使用し、図14に示すように蛍光体層105の端部に額縁131を設けて封止した以外は、実施例1と同様にして蛍光体シートを得た。この蛍光体シートの色度ズレの相対値は1.00であり、硫黄系ガスの発生評価は○であった。
緑色蛍光体を被覆処理せずに使用した以外は、実施例1と同様にして蛍光体シートを得た。この蛍光体シートの色度ズレの相対値は1.00であり、硫黄系ガスの発生評価は×であった。
緑色蛍光体の被覆処理において、酸化亜鉛粉末を投入しなかった以外は、実施例1と同様にして蛍光体シートを得た。この蛍光体シートの色度ズレの相対値は1.20であり、硫黄系ガスの発生評価は△であった。
Claims (8)
- 蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有する蛍光体含有樹脂組成物から形成された蛍光体層と、
前記蛍光体層を挟持する一対の透明基材とを備え、
前記蛍光体のうち少なくとも硫化物蛍光体が、金属酸化物粉末を含む二酸化ケイ素膜で被覆されてなる蛍光体シート。 - 前記蛍光体層が、前記一対の透明基材の間に露出部を有する請求項1記載の蛍光体シート。
- 前記金属酸化物粉末が、酸化亜鉛粉末である請求項1又は2記載の蛍光体シート。
- 前記硫化物蛍光体が、(SrxM1−x−y)Ga2S4:Euy(MはCa、Mg、Baのいずれかであり、0≦x≦1、0<y<0.05を満たす。)である請求項1乃至3のいずれか1項に記載の蛍光体シート。
- 前記重合性化合物が、光硬化型アクリレートを含有し、
前記重合開始剤が、光重合開始剤である請求項1乃至4のいずれか1項に記載の蛍光体シート。 - 蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有し、
前記蛍光体のうち少なくとも硫化物蛍光体が、金属酸化物粉末を含む二酸化ケイ素膜で被覆されてなる蛍光体含有樹脂組成物。 - 蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有し、前記蛍光体のうち少なくとも硫化物蛍光体が、金属酸化物粉末を含む二酸化ケイ素膜で被覆されてなる蛍光体含有樹脂組成物が青色発光素子を覆う状態で硬化してなる白色光源。
- 青色発光素子が透明樹脂で包含された発光構造体と、
前記発光構造体が二次元配置された基板と、
前記基板と離間して配置され、前記青色発光素子の青色光から白色光を得る粉末状の蛍光体を含有する蛍光体シートとを備え、
前記蛍光体シートは、蛍光体が二酸化ケイ素膜で被膜された被覆蛍光体と、重合性化合物と、重合開始剤とを含有し、前記蛍光体のうち少なくとも硫化物蛍光体が、金属酸化物粉末を含む二酸化ケイ素膜で被覆されてなる蛍光体含有樹脂組成物から形成された蛍光体層が一対の透明基材に挟持されてなる照明装置。
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JP2012165056A JP6038524B2 (ja) | 2012-07-25 | 2012-07-25 | 蛍光体シート |
CN201380039337.7A CN104471024A (zh) | 2012-07-25 | 2013-07-16 | 荧光体片 |
KR1020157003913A KR102120951B1 (ko) | 2012-07-25 | 2013-07-16 | 형광체 시트 |
PCT/JP2013/069289 WO2014017334A1 (ja) | 2012-07-25 | 2013-07-16 | 蛍光体シート |
TW102125365A TWI596189B (zh) | 2012-07-25 | 2013-07-16 | 螢光體片 |
TW106118004A TWI680180B (zh) | 2012-07-25 | 2013-07-16 | 被覆螢光體 |
EP13823548.6A EP2878646B1 (en) | 2012-07-25 | 2013-07-16 | Phosphor sheet |
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DE102014107472A1 (de) | 2014-05-27 | 2015-12-03 | Osram Opto Semiconductors Gmbh | Halbleiterbauelement und Beleuchtungsvorrichtung |
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KR102120951B1 (ko) | 2020-06-09 |
TW201732019A (zh) | 2017-09-16 |
KR20150038078A (ko) | 2015-04-08 |
TWI596189B (zh) | 2017-08-21 |
EP2878646B1 (en) | 2017-12-13 |
EP2878646A1 (en) | 2015-06-03 |
JP6038524B2 (ja) | 2016-12-07 |
CN104471024A (zh) | 2015-03-25 |
TWI680180B (zh) | 2019-12-21 |
TW201420723A (zh) | 2014-06-01 |
WO2014017334A1 (ja) | 2014-01-30 |
US9850427B2 (en) | 2017-12-26 |
US20150197689A1 (en) | 2015-07-16 |
EP2878646A4 (en) | 2016-08-10 |
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