JP5915527B2 - ガラスセラミックス組成物、発光素子用基板、および発光装置 - Google Patents
ガラスセラミックス組成物、発光素子用基板、および発光装置 Download PDFInfo
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- JP5915527B2 JP5915527B2 JP2012526585A JP2012526585A JP5915527B2 JP 5915527 B2 JP5915527 B2 JP 5915527B2 JP 2012526585 A JP2012526585 A JP 2012526585A JP 2012526585 A JP2012526585 A JP 2012526585A JP 5915527 B2 JP5915527 B2 JP 5915527B2
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- glass
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- light emitting
- zirconia
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- 239000000758 substrate Substances 0.000 title claims description 163
- 239000006112 glass ceramic composition Substances 0.000 title claims description 44
- 239000000843 powder Substances 0.000 claims description 222
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 204
- 239000011521 glass Substances 0.000 claims description 112
- 239000002245 particle Substances 0.000 claims description 92
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 63
- 238000004519 manufacturing process Methods 0.000 claims description 30
- 238000010304 firing Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 14
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 claims description 5
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- 229910018068 Li 2 O Inorganic materials 0.000 description 4
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
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- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 150000003609 titanium compounds Chemical class 0.000 description 2
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- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
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- 239000004803 Di-2ethylhexylphthalate Substances 0.000 description 1
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- 229940088601 alpha-terpineol Drugs 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
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- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
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- 239000000156 glass melt Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
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- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 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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- 239000002244 precipitate Substances 0.000 description 1
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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Description
また、本発明の発光素子用基板の製造方法は、上記したガラスセラミックス組成物の成形物を前記ガラス粉末のガラスが軟化する温度で焼成することを特徴とする。
実施形態のガラスセラミックス組成物は、発光ダイオード素子(LED素子)等の発光素子を搭載するための発光素子用基板(LTCC基板、以下では単に基板という)の製造に用いられるガラスセラミックス組成物である。本発明のガラスセラミックス組成物は、ガラス粉末、アルミナ粉末およびジルコニア粉末を含み、それら無機粉末のみの混合物を意味するばかりでなく、それら無機粉末とバインダーや溶剤などの有機成分を含む組成物(たとえば、後述のスラリーやグリーンシートである組成物)を意味する。本発明のガラスセラミックス組成物に含まれる無機粉末は、上記3種の無機粉末のみに限られず、他の無機粉末が含まれていてもよい。
本発明の組成物に含まれる上記3種の無機粉末の含有割合は、上記3種の無機粉末の合計量に対してガラス粉末が30〜45質量%、アルミナ粉末が35〜50質量%およびジルコニア粉末が10〜30質量%である。さらに、本発明の組成物において、ジルコニア粉末の平均粒径はアルミナ粉末の平均粒径の1/4以下であることを特徴とする。
ブレーク性の向上のためには、ジルコニア粉末の充填が効果的である。ジルコニアはガラス熔解の耐火レンガに使用される事例があるように、高融点であり、熔融したガラスと反応しにくい。この性質により、LTCC焼成時の熔融したガラスと反応しにくいと考えられる。このため、ジルコニア粉末をLTCCに充填した場合、ガラス相が不連続となりやすく、ブレーク性が向上すると考えられる。アルミナ粉末の場合、LTCC焼成時に熔融したガラスと反応しやすく、ガラス相に融け込み、ガラス相と一体化することにより、ガラス相が不連続になりにくく、充填してもブレーク性が向上しにくいと考えられる。
ジルコニア粉末の平均粒径はアルミナ粉末の平均粒径の1/6以下が好ましく、1/8以下が好ましい。通常、ジルコニア粉末の平均粒径はアルミナ粉末の平均粒径の1/50以上が好ましく、1/30以上がより好ましい。
上記チタニア等の粉末の場合と同様に、本発明のガラスセラミックス組成物はガラス粉末、アルミナ粉末、ジルコニア粉末の3種以外の無機粉末の1種以上を含有していてもよい。しかし、3種以外の無機粉末の合計量は、全無機粉末に対して10質量%未満が好ましく、5質量%未満がより好ましい。特に、焼成後に無機質成分として残留する無機粉末(上記3種以外)は、実質的に含有しないことが好ましい。
さらに、結晶化しやすいガラスの場合、焼結させる工程で、例えば焼成炉の炉内温度分布などにより、温度のばらつきを生じた時に、結晶化の度合いが異なる部位を生じやすくなり、その結果、基板が反ったり、変形したりする問題が生じる。また、一般的に内部、表面に形成するAg系導体と接するガラスが結晶化しやすいなど、結晶化の度合いが異なる部位を生じやすくなり、その結果、基板が反ったり、変形したりする問題が生じる。
バインダーは、無機粉末の粒子間を結合し、無機粉末を所定の形状に保つために使用される。バインダーとしては、焼成時の温度下で速やかに分解して消失する、合成樹脂や天然樹脂などの樹脂が好ましい。加工助剤としては、バインダーを溶解する低沸点溶剤や高沸点溶剤が好ましい。そのほか、分散剤などの加工助剤を使用することもできる。
無機粉末を所定の形状(たとえば、シート状)に成形するために、バインダーと溶剤とを含む流動性の組成物(以下、スラリーという)が使用される。スラリーをたとえばシート状に成形し、スラリー中の低沸点溶剤を蒸発除去することにより、シート状の固体組成物(以下、グリーンシートという)が得られる。シート状に限られず、スラリーや溶剤の少ない組成物から種々の形状の成形物を得ることができる。グリーンシートやこの成形物は、バインダーとともにバインダーを溶解した高沸点溶剤(以下、可塑剤という)を含んでいることが好ましい。
さらに、低沸点溶剤を含む本発明のガラスセラミックス組成物(スラリーなど)における有機成分の割合は、その組成物に対して7〜50質量%であることが好ましく、10〜40質量%であることがより好ましい。そのうち、低沸点溶剤の割合は、その組成物に対して5〜30質量%であることが好ましく、10〜25質量%であることがより好ましい。
まず、SiO2 60.4モル%、B2O3 15.6モル%、Al2O3 6.0モル%、CaO 15.0モル%、Na2O 2.0モル%、K2O 1.0モル%となるように原料を配合、混合し、この混合物を白金ルツボに入れて1500〜1600℃で60分間溶融後、溶融ガラスを冷却してガラスブロックを得た。得られたガラスのガラス軟化点(Ts)は830℃であった。このガラス軟化点(Ts)は、株式会社リガク製の示差熱分析装置(商品名:Thermo Plus TG8110)で測定した値である。
上記ガラスブロックをアルミナ製ボールミルにより水を溶媒として20〜60時間粉砕し、ホウケイ酸系ガラス粉末を得た。ガラス粉末の平均粒径は、いずれも2.0μmであった。なお、ガラス粉末の平均粒径は、上記したように、樹脂包埋したガラス粉末をSEMで観察することによって評価した値である。
グリーンシート、導電金属ペーストを用いて、光束量評価用基板を作製した。まず、一辺が40mm程度の正方形のグリーンシートを6枚積層したものについて、サーマルビアとなる部分に孔空け機を用いて直径0.3mmの貫通孔を形成し、スクリーン印刷法により金属ペーストを充填して未焼成サーマルビアを形成すると共に、未焼成接続端子、未焼成外部接続端子を形成して未焼成基板を得た。この未焼成基板について、550℃で5時間保持する脱脂を行い、さらに870℃で30分間保持する焼成を行って評価用基板を製造した。
反射率は以下の方法で測定した。すなわち、一辺が30mm程度の正方形のグリーンシートを1枚としたもの、2枚積層したもの、3枚積層したものについてそれぞれ550℃で5時間保持して樹脂成分を分解除去した後、870℃で30分間保持して焼成行い、厚みが、140μm、280μm、420μm程度の3種類の評価用基板を得た。これらの評価用基板の反射率を、オーシャンオプティクス社の分光器USB2000と小型積分球ISP−RFを用いて測定し、厚みに関して線形補完することで、厚み300μmの評価用基板の反射率(単位:%)を算出した。反射率は波長460nmにおけるものとし、リファレンスとしては硫酸バリウムを使用した。
一辺が40mm程度の正方形のグリーンシートを6枚積層したものについて、550℃で5時間保持して樹脂成分を分解除去した後、870℃で30分間保持して焼成行い、厚みが0.85mm程度の評価用基板を得た。この評価用基板について、レーザーフラッシュ法により常温での熱伝導率を測定した。測定装置には、アルバック理工社のTC―7000を用いた。
一辺が40mm程度の正方形のグリーンシートを6枚積層したものについて、550℃で5時間保持して樹脂成分を分解除去した後、870℃で30分間保持して焼成行い、厚みが0.85mm程度の評価用基板を得た。この評価用基板について、JIS−B0601(1994年)に記載された方法に準じて、接触式表面粗さ計(株式会社東京精密、商品名:サーフコム1400D)を用いて表面粗さRaを測定した。
一辺が40mm程度の正方形のグリーンシートを6枚積層したものについて、UHT社のG−Cut6を用いて、縦、横方向にそれぞれ8等分(計64等分)できるように、5mm間隔の切り込みを入れた。切り込みの深さは0.25mmとした。なお、グリーンシート全体の厚みは1.0mm程度であった。得られたグリーンシートを550℃で5時間保持して樹脂成分を分解除去した後、870℃で30分間保持して評価用集合基板を得た。この評価用集合基板を、深さ5mmの溝の入ったポリカーカーボネートを用いて、上述のG−Cut6による切り込みに沿って分割し、割れやチッピング等の発生割合を評価した。割れやチッピングの発生割合が小さいほど、ブレーク性がよく、量産性に優れている。割れやチッピングの発生割合は5%以下であることが好ましい。
2…発光素子用基板
4…発光素子
Claims (10)
- ガラス粉末、アルミナ粉末および前記アルミナ粉末の平均粒径の1/4以下の平均粒径のジルコニア粉末を含み、
前記ガラス粉末、前記アルミナ粉末および前記ジルコニア粉末の合計量に対する前記ガラス粉末の割合が30〜45質量%、前記アルミナ粉末の割合が35〜50質量%、前記ジルコニア粉末の割合が10〜30質量%、
前記アルミナ粉末の平均粒径が1.0〜4.0μm、前記ジルコニア粉末の平均粒径が0.03〜0.5μmであることを特徴とするガラスセラミックス組成物。 - 前記ガラス粉末、前記アルミナ粉末および前記ジルコニア粉末の合計量に対する前記ジルコニア粉末の量が15〜30質量%である、請求項1に記載のガラスセラミックス組成物。
- 前記ジルコニア粉末が、安定化ジルコニアまたは部分安定化ジルコニアからなる、請求項1または2に記載のガラスセラミックス組成物。
- 前記ガラス粉末のガラスのガラス軟化点(Ts)が650〜950℃である、請求項1〜3のいずれか一項に記載のガラスセラミックス組成物。
- さらに、焼成により消失しうる有機成分を含む、請求項1〜4のいずれか一項に記載のガラスセラミックス組成物。
- 前記有機成分の含有量が、ガラスセラミックス組成物に対して3〜35質量%である、請求項5に記載のガラスセラミックス組成物。
- 発光素子を搭載するための基板の製造に用いられる、請求項1〜6のいずれか一項に記載のガラスセラミックス組成物。
- 請求項1〜7のいずれか一項に記載のガラスセラミックス組成物の成形物を前記ガラス粉末のガラスが軟化する温度で焼成することを特徴とする発光素子用基板の製造方法。
- 焼成温度が850〜900℃である、請求項8に記載の発光素子用基板の製造方法。
- 発光素子用基板と、前記発光素子用基板に搭載された発光素子とを具備する発光装置の製造方法であって、
前記発光素子用基板の製造方法が請求項8または9記載の発光素子用基板の製造方法であることを特徴とする発光装置の製造方法。
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