JP7450701B2 - 蛍光セラミックス及びその製造方法、光源装置 - Google Patents
蛍光セラミックス及びその製造方法、光源装置 Download PDFInfo
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- JP7450701B2 JP7450701B2 JP2022506668A JP2022506668A JP7450701B2 JP 7450701 B2 JP7450701 B2 JP 7450701B2 JP 2022506668 A JP2022506668 A JP 2022506668A JP 2022506668 A JP2022506668 A JP 2022506668A JP 7450701 B2 JP7450701 B2 JP 7450701B2
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- 239000000919 ceramic Substances 0.000 title claims description 192
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000000843 powder Substances 0.000 claims description 211
- 238000005245 sintering Methods 0.000 claims description 78
- 239000011148 porous material Substances 0.000 claims description 53
- 239000013078 crystal Substances 0.000 claims description 45
- 239000011159 matrix material Substances 0.000 claims description 39
- 239000000758 substrate Substances 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 33
- 239000002994 raw material Substances 0.000 claims description 33
- 239000011812 mixed powder Substances 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005467 ceramic manufacturing process Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- -1 titanium ions Chemical class 0.000 description 2
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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Description
本実施例において、蛍光セラミックスを製造するためにセラミックスマトリックス原料粉体を提供する。ここで、セラミックスマトリックス原料粉体は、蛍光セラミックスのセラミックスマトリックスを形成するために用いられる。
本実施例において、セラミックスマトリックス原料粉体を焼結することによって、第1粉体が得られる。第1粉体は、後続の蛍光セラミックスの製造プロセスにおいて蛍光セラミックスのセラミックスマトリックスを形成するために用いられる。ここで、第1粉体の結晶粒内部には気孔が形成され、入射レーザ光の散乱を増加させることによって、蛍光セラミックスの発光効率を向上させるために用いられる。
本実施例において、上記ステップで得られた第1粉体と蛍光粉体を混合して焼結し、すなわち、二次焼結を行うことによって、セラミックス基体及びセラミックス基体内に散布された蛍光粉体を得る。蛍光粉体は、レーザ光で励起されて発光し、蛍光セラミックスの発光機能を実現する。また、二次焼結によって、一次焼結で得られた気孔は、セラミックス基体の結晶粒内部に保持され、さらに結晶粒内に気孔が存在する蛍光セラミックスを製造した。
本実施例において、第2粒径を有するセラミックスマトリックス原料粉体を提供し、セラミックスマトリックス原料粉体に対して前処理を行うことによって、第1粒径を有する第1粉体が得られる。具体的には、一部のセラミックスマトリックス原料粉体を取得して焼結し、第1粉体ブランクが得られ、残りのセラミックスマトリックス原料粉体が、すなわち第2粉体であることを含むことができる。第1粉体ブランクを破砕し、ラッピングし、結晶粒内部に気孔が形成された第1粉体を得る。ここで、セラミックスマトリックス原料粉体、第1粉体及び第2粉体は、同じ材質である。
本実施例において、前処理で得られた第1粉体、第2粉体、蛍光粉体及び焼結助剤をボールミリングして混合し(ボールミリングは当業者の理解範囲に属し、ここで説明を省略する)、第1混合粉体ブランクが得られて、後続の焼結段階に用いられる。ここで、第1粉体と第2粉体の質量比は、4:6~7:3であり、蛍光粉体は、第1混合粉体ブランクの総質量の30%~70%を占め、焼結助剤は、前記第1混合粉体ブランクの総質量の0.1%~1%を占めている。発明者らは、大量の実験データのまとめによって、第1粉体、第2粉体、蛍光粉体及び焼結助剤の添加量が上記に示されるようになる場合、製造された蛍光セラミックスが各方面で良好な性能を示すことができることを見出した。
本実施例において、混合して得られた第1混合粉体ブランクを黒鉛金型に充填し、第1混合粉体に対して小さな圧力で予圧処理を行い、その後に第1混合粉体ブランクが充填された黒鉛金型をSPSホットプレス炉に配置し、真空又は保護ガスの雰囲気で保温焼結を行うことによって、第2混合粉体ブランクを得る。
本実施例において、第1混合粉体ブランクを焼結して第2混合粉体ブランクを得た後、蛍光セラミックスを得るために、第2混合粉体ブランクにアニール処理を行う必要がある。具体的には、第2混合粉体ブランクを空気雰囲気に配置してアニール処理を行う。アニール処理の温度は、1200℃~1400℃であり、時間長は、5h~20hである。
本実施例において、アニール処理によって蛍光セラミックスの粗ブランクを得た後、蛍光セラミックスが製品の寸法仕様及び表面性質の要件を満たすように、蛍光セラミックスに後処理を行う必要がある。具体的には、蛍光セラミックスに対して行われる後処理は、ダイシング処理、ラッピング処理及びポリッシング処理などのうちの少なくとも一種を含む。ここで、ダイシング処理は、蛍光セラミックスの粗ブランクを製品に要求される大きさ、形状の蛍光セラミックスに切断することを目的とするものであり、ラッピング処理及びポリッシング処理は、蛍光セラミックスの表面平坦度、平滑度などの表面特性が製品の要求を満たすことを目的とするものである。
Claims (11)
- 蛍光セラミックスであって、
セラミックス基体と、前記セラミックス基体内に散布された蛍光粉体と、を含み、前記セラミックス基体の結晶粒内部には気孔が形成され、
前記セラミックス基体の材質は、アルミナであり、
前記気孔の孔径は、0.1μm~2μmであり、前記気孔の孔径は、前記気孔の算術平均孔径であり、
前記セラミックス基体の結晶粒径は、5μm~20μmであり、前記結晶粒径は、前記セラミックス基体の結晶粒の算術平均結晶径であることを特徴とする蛍光セラミックス。 - 前記セラミックス基体の結晶粒内部には、均一に分布した複数の前記気孔が形成されていることを特徴とする請求項1に記載の蛍光セラミックス。
- 前記蛍光粉体の粒径は、5μm~30μmであり、前記蛍光粉体の粒径は、前記蛍光粉体の算術平均径であることを特徴とする請求項1又は2に記載の蛍光セラミックス。
- 蛍光セラミックスの製造方法であって、
セラミックスマトリックス原料粉体を提供するステップと、
前記セラミックスマトリックス原料粉体を焼結し、結晶粒内部に気孔が形成された第1粉体を得るステップと、
前記第1粉体と蛍光粉体を混合して焼結することによって、前記気孔をセラミックス基体の結晶粒の内部に保持するステップと、を含み、
前記セラミックスマトリックス原料粉体を焼結し、結晶粒内部に気孔が形成された第1粉体を得る前記ステップは、
一部の前記セラミックスマトリックス原料粉体を取得して焼結し、第1粉体ブランクを得ることであって、残りの前記セラミックスマトリックス原料粉体が第2粉体であるステップと、
前記第1粉体ブランクを破砕し、ラッピングし、結晶粒内部に前記気孔が形成された前記第1粉体を得るステップと、を含み、
前記第1粉体の粒径は、前記第2粉体の粒径よりも大きく、前記第1粉体の粒径と前記第2粉体の粒径は、それぞれ前記第1粉体の算術平均径、前記第2粉体の算術平均径であることを特徴とする蛍光セラミックスの製造方法。 - 前記第1粉体の粒径は、5μm~10μmであり、前記第2粉体の粒径は、0.05μm~0.5μmであることを特徴とする請求項4に記載の製造方法。
- 前記一部の前記セラミックスマトリックス原料粉体を取得して焼結し、第1粉体ブランクを得るステップは、
取得された一部の前記セラミックスマトリックス原料粉体を温度1600℃~1800℃の雰囲気に配置して2h~6h焼結し、前記第1粉体ブランクを得るステップ、を含むことを特徴とする請求項4に記載の製造方法。 - 前記第1粉体と蛍光粉体を混合して焼結するステップは、
前記第1粉体、前記第2粉体、前記蛍光粉体及び焼結助剤を混合して焼結するステップであって、前記焼結助剤が酸化マグネシウム、酸化イットリウム、酸化ランタン、酸化チタンのうちの少なくとも一種であるステップ、を含むことを特徴とする請求項4乃至6のいずれか1項に記載の製造方法。 - 前記焼結助剤は、少なくとも酸化チタンを含むことを特徴とする請求項7に記載の製造方法。
- 前記第1粉体、前記第2粉体、前記蛍光粉体及び焼結助剤を混合して焼結するステップは、
前記第1粉体、前記第2粉体、前記蛍光粉体及び前記焼結助剤をボールミリングして混合し、第1混合粉体ブランクを得るステップと、
前記第1混合粉体ブランクを真空又は保護ガス雰囲気に配置して保温焼結し、第2混合粉体ブランクを得るステップであって、焼結温度が1300℃~1600℃であり、焼結時の圧力が20MPa~180MPaであり、焼結時間長が0.5h~4hであるステップと、
前記第2混合粉体ブランクを空気雰囲気に配置してアニール処理を行い、前記蛍光セラミックスを得るステップであって、前記アニール処理の温度が1200℃~1400℃であり、時間長が5h~20hであるステップと、を含むことを特徴とする請求項7又は8に記載の製造方法。 - 前記蛍光粉体の質量は、前記第1混合粉体ブランクの総質量の30%~70%を占め、前記焼結助剤の質量は、前記第1混合粉体ブランクの総質量の0.1%~1%を占め、かつ、前記第1粉体と前記第2粉体との質量比は、4:6~7:3であることを特徴とする請求項9に記載の製造方法。
- 請求項1~3のいずれか一項に記載の蛍光セラミックスを含むことを特徴とする光源装置。
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