JP5370595B2 - 光変換用セラミック複合体及びその製造方法 - Google Patents
光変換用セラミック複合体及びその製造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims description 108
- 239000002131 composite material Substances 0.000 title claims description 108
- 238000006243 chemical reaction Methods 0.000 title claims description 106
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 238000005498 polishing Methods 0.000 claims description 104
- 239000013078 crystal Substances 0.000 claims description 75
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 73
- 239000007788 liquid Substances 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 229910052684 Cerium Inorganic materials 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- 238000012545 processing Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 21
- 239000002002 slurry Substances 0.000 description 15
- 229910052688 Gadolinium Inorganic materials 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 239000008119 colloidal silica Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000016507 interphase Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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Description
YAG:Ce相は、400〜500nmの紫〜青色励起光で、ピーク波長530〜560nmの蛍光を発し、YAG:Gd,Ce相は、ピーク波長540〜580nmの蛍光を発することから、Al2O3以外の前記酸化物結晶相が、YAG:Ce相またはYAG:Gd,Ce相である前記凝固体は、青色光または紫色光の発光素子と組み合わせて使用される白色発光装置用の光変換用部材として好適である。
先ず、実施例に用いられる凝固体を製造した。α−Al2O3粉末(純度99.99%)をAlO3/2換算で0.82モル、Y2O3粉末(純度99.9%)をYO3/2換算で0.175モル、CeO2粉末(純度99.9%)を0.005モルとなるよう秤量した。これらの粉末をエタノール中、ボールミルによって16時間湿式混合した後、エバポレーターを用いてエタノールを脱媒して原料粉末を得た。原料粉末は、真空炉中で予備溶解し一方向凝固の原料とした。次に、この原料をそのままモリブデンルツボに仕込み、一方向凝固装置にセットし、1.33×10−3Pa(10−5Torr)の圧力下で原料を融解した。次に同一の雰囲気においてルツボを5mm/時間の速度で下降させ、Al2O3(サファイア)相と、蛍光を発する酸化物結晶相(YAG相)とが連続的にかつ三次元的に相互に絡み合った組織を有する凝固体を得た。
次に、本発明に係る光変換用セラミック複合体の実施例1について説明する。先ず、参考例において製造された凝固体から直径2インチ、厚さ0.4mmの円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.020μmであった。この円板状試料について、下記の条件にてCMPを行い、実施例1に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、0.4質量%になるように純水で希釈した(株)フジミインコーポレーテッド製コロイダルシリカ研磨スラリーの「COMPOL(登録商標)Type120」に1mol/LのNaOH水溶液を添加し、pHが11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重10kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を150分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11〜12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例2について説明する。CMP用研磨液中のシリカ粒子の含有量を4質量%、CMPの加工時間を60分間とした以外は実施例1と同様にして実施例2に係る光変換用セラミック複合体を作製した。
次に、本発明に係る光変換用セラミック複合体の実施例3について説明する。先ず、参考例において製造された凝固体から実施例1と同様の円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.015μmであった。この円板状試料から正方形:15mm×15mmの四角板状試料を切り出し、下記の条件にてCMPを行い、実施例3に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、2質量%になるように純水で希釈した扶桑化学工業(株)製コロイダルシリカ研磨スラリーの「クォートロン(登録商標)PL−2L」に1mol/LのNaOH水溶液を添加し、pHを11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重10kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を270分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11〜12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例4について説明する。先ず、参考例において製造された凝固体から実施例1と同様の円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.015μmであった。この円板状試料について、下記の条件にてCMPを行い、実施例4に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、2質量%になるように純水で希釈した扶桑化学工業(株)製コロイダルシリカ研磨スラリーの「クォートロン(登録商標)PL−2L」に1mol/LのNaOH水溶液を添加し、pHを11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重13kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を270分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11〜12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例5について説明する。研磨パッドの単位荷重を33kPa、CMPの加工時間を180分間とした以外は実施例4と同様にして実施例5に係る光変換用セラミック複合体を作製した。また、実施例5について、加工中のpHの状態を図6に示す。
次に、本発明に係る光変換用セラミック複合体の実施例6について説明する。研磨パッドの単位荷重を50kPa、CMPの加工時間を120分間とした以外は実施例4と同様にして実施例6に係る光変換用セラミック複合体を作製した。
次に、本発明に係る光変換用セラミック複合体の実施例7について説明する。研磨パッドの格子状溝間隔を7mm、研磨パッドの単位荷重を33kPa、CMPの加工時間を90分間とした以外は実施例4と同様にして実施例7に係る光変換用セラミック複合体を作製した。
比較として、参考例において製造された凝固体から実施例1及び実施例2と同様の円板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例1に係る光変換用セラミック複合体を得た。
次に、比較として、参考例において製造された凝固体から実施例3と同様の四角板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例2に係る光変換用セラミック複合体を得た。
また、比較として、参考例において製造された凝固体から実施例3と同様の四角板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例3に係る光変換用セラミック複合体を得た。
次に、比較として、参考例において製造された凝固体から実施例4と同様の円板状試料を切り出し、研磨パッドの単位荷重を13kPa、CMPの加工時間を270分間とした以外は比較例3と同様にして比較例4に係る光変換用セラミック複合体を作製した。
次に、比較として、CMP用研磨液として、シリカ粒子の含有量が、0.4質量%になるように純水で希釈した(株)フジミインコーポレーテッド製コロイダルシリカ研磨スラリーの「COMPOL(登録商標)Type120」に1mol/LのNaOH水溶液を添加し、pHが12を超えるように調整した。その結果、研磨液中のシリカ粒子の凝集等の問題が発生した。
2 発光素子(発光ダイオード素子)
3 フリップチップ電極端子
4 アノード電極
5 カソード電極
Claims (7)
- Al2O3相及びAl2O3以外の酸化物結晶相が連続的にかつ三次元的に相互に絡み合った組織を有する凝固体の表面にCMPを行なう研磨工程を備え、
CMPを行なう際の研磨液のpHを11〜12に調整していることを特徴とする光変換用セラミック複合体の製造方法。 - 前記凝固体の表面における前記Al2O3相と前記酸化物結晶相との相間段差を0.010μm以下にすることを特徴とする請求項1記載の光変換用セラミック複合体の製造方法。
- 前記酸化物結晶相が、蛍光を発する蛍光体であり、Ceを含有するYAG((Y、Ce)3Al5O12)相であることを特徴とする請求項1または2記載の光変換用セラミック複合体の製造方法。
- 前記研磨液のpHを11.3〜11.6に調整していることを特徴とする請求項1乃至3いずれか記載の光変換用セラミック複合体の製造方法。
- 前記研磨液がシリカ粒子を含有し、その含有量が0.1〜5質量%未満であることを特徴とする請求項1乃至4いずれか記載の光変換用セラミック複合体の製造方法。
- 前記CMPの単位荷重が10〜50kPaであることを特徴とする請求項1乃至5いずれか記載の光変換用セラミック複合体の製造方法。
- Al2O3相及びAl2O3以外の酸化物結晶相が連続的にかつ三次元的に相互に絡み合った組織を有する凝固体からなり、該凝固体の表面における前記Al2O3相と前記酸化物結晶相との相間段差が0.010μm以下である光変換用セラミック複合体。
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