JP5837289B2 - 光ルミネセンス蛍リン光体粒子を含む安全管理用製品 - Google Patents
光ルミネセンス蛍リン光体粒子を含む安全管理用製品 Download PDFInfo
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- JP5837289B2 JP5837289B2 JP2010183169A JP2010183169A JP5837289B2 JP 5837289 B2 JP5837289 B2 JP 5837289B2 JP 2010183169 A JP2010183169 A JP 2010183169A JP 2010183169 A JP2010183169 A JP 2010183169A JP 5837289 B2 JP5837289 B2 JP 5837289B2
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Classifications
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- C—CHEMISTRY; METALLURGY
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- 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
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/20—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the material in which the electroluminescent material is embedded
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
- C09K11/582—Chalcogenides
- C09K11/584—Chalcogenides with zinc or cadmium
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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- C09K11/592—Chalcogenides
- C09K11/595—Chalcogenides with zinc or cadmium
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
- C09K11/621—Chalcogenides
- C09K11/623—Chalcogenides with zinc or cadmium
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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- C09K11/641—Chalcogenides
- C09K11/642—Chalcogenides with zinc or cadmium
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- C09K11/643—Chalcogenides with alkaline earth metals
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- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
- C09K11/644—Halogenides
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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- C09K11/661—Chalcogenides
- C09K11/662—Chalcogenides with zinc or cadmium
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- C09K11/666—Aluminates; Silicates
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Description
蛍リン光体粒子を製造するための多くの方法が提案されている。こうした方法の1つに固体法と呼ばれるものがある。この方法では、蛍リン光体の前駆物質を固体の状態に混合して加熱することにより、この前駆物質が反応して蛍リン光物質の粉体が形成される。例として、カセンガ(Kasenga)等に付与された特許文献1には、マンガン活性化珪酸亜鉛蛍リン光体(ZnSiO4:Mn)の製造方法が開示されている。この方法では、酸化亜鉛、珪酸、及び炭酸マンガンなどの開始成分の混合物を乾燥配合し、この配合混合物を約1250℃で焼成する工程が行われる。得られた蛍リン光体はより小さな粒子に破砕または粉砕される。固体法や他の多くの製造方法では、磨砕工程を行って粉体の粒径を小さくする。この機械的磨砕工程によって蛍リン光体の表面が損傷し、死層が形成されて、蛍リン光粉体の輝度が損なわれる。
請求項3に記載の発明は、請求項1に記載の安全管理用製品において、製品は通貨の形態である、ことをその要旨とする。
請求項9に記載の発明は、請求項1に記載の安全管理用製品において、前記粒子は、ほぼ団粒化されていない、ことをその要旨とする。
本発明は蛍リン光粉体及び該粉体の製造方法、ならびに該粉体を使用した装置に一般的に関する。蛍リン光体は、電子(陰極ルミネセンス蛍リン光体)、光子(光ルミネセンス蛍リン光体)、電場(エレクトロルミネセンス蛍リン光体)やX線エネルギー(X線蛍リン光体)などのエネルギー源によって刺激した場合に光、一般に可視光、を放射する。特定の蛍リン光体化合物の例を下記に列記した。蛍リン光体化合物の中にはこれらのカテゴリーの2以上に属するものがあることは理解されよう。
Re=ρvd/μ
ここで、ρ=流体密度
v=流体平均速度
d=導管内径
μ=流体粘度
なお、密度、速度、及び粘度に関する値は炉110の長さに応じて変化する。
炉110内での最大レイノルズ数は、ガス速度は加熱された場合のガス膨張により非常に高い値であるので、通常、最大レイノルズ数平均ストリーム温度が最大の場合に達成される。
酸化イットリウム製造のための前駆体溶液は好ましくは約4−約6重量パーセントの前駆体を含んでいるべきであることが知られている。
SiCl4は揮発性が高く、室温では液体であり、このことは反応器への移送をより制御しやすくしてくれる。三塩化アルミニウム(AlCl3)はアルミナ被膜を形成するために同様の方法で用いることができる。
ほとんどの金属アルコキシドは妥当な高い蒸気圧を有しており、従って、被膜前駆体として適している。
Mg(O2CCH3)2――――>MgO+CH3(O)OC(O)CH3
金属酢酸塩は水溶性で、それほど高価でないので、被膜前駆体として好適である。
本発明による蛍リン光体粉体はしばしば量子効率とも呼ばれる高い効率を提供してくれる。効率は励起エネルギーの放出される可視光子への全体的な転化を意味している。本発明による蛍リン光体粉体の高い効率は高い結晶度及びホスト物質内でのアクチベータ・イオンの均一な分散、及びほぼ欠陥のない粒子表面などによるものと考えられる。
持続性とは光放出がそのピーク輝度の10%まで崩壊するのにかかる時間である。表示用途の場合、長期崩壊時間を有する蛍リン光体の場合、画像がその表示内で移動する時にぼやけた画像になってしまう。本発明による蛍リン光体粉体の改良された(減少された)崩壊時間は主としてホスト物質内でのアクチベータ・イオンの均一な分布によるものと考えられる。
蛍リン光体は表示スクリーンから剥離すべきでなく、色付きの蛍リン光体との相互汚染が起きてはならない。これらの特性は蛍リン光体粒子の形状、粒径、及び表面の状態によってもかなり影響を受ける。
創られた粉体を図50のSEM顕微鏡写真に示す。また粒子径分布を図51に示す。平均粒子径は2.476μmであり、粒子の90パーセントは4.150μm以下の大きさである。図52に示すX線回折パターンは粒子がほぼ相純粋なY2O3であることを示している。
つくられた粉体を図53のSEM顕微鏡写真に示す。粒子径分布は図54に示されている。平均粒子径は2.533μmであり、粒子の90パーセントは4.467μmの大きさであった。図55のX線回折パターンは粒子がほぼ相純粋なZn2SiO4であることを示している。
1.BAM前駆体の選択
アルミニウム硝酸塩水和物(Al(NO3)3・9H2O)を用いて、Ba0.95Eu0.05MgAl10O17(すなわち微量添加物としての原子パーセントユーロピウム)に基づいて5重量パーセント溶液がつくられた。前記溶液を攪拌すると硝酸バリウムの結晶性沈殿物が得られた。4当量分のエチレン・グリコールをキレート剤として加えたところ、硝酸バリウムの溶解性が増大した。しかし沈殿物は残存した。
2.BAM処理温度
上に述べたように、燻蒸粒子状アルミナが前駆体成分として選択された。硝酸ユーロピウム、硝酸バリウム及びマ硝酸グネシウムを最終BAM組成物でその総前駆体濃度が7.5重量パーセントとなるような割合で、残留前駆体として用いられた。溶液はエアロゾルを形成するために約1.6MHzの周波数で超音波トランスデューサを用いて霧化された。このエアロゾルは表IVに示すようないろいろな温度でチューブ式加熱炉を通じて移送された。
3.BAM前駆体濃度
上記確認されたアルミン酸塩不純物を除去するために、前記前駆体溶液の金属化学当量を変化させた。溶液及び処理の結果を表Vに要約して示す。すべての溶液は約1.6MHzの周波数で超音波霧化器を用いてエアロゾルに転化され、加熱炉の中で750℃の温度でスプレイ転化された。
前記の例に基づいて、BAM粉体が以下のように製造した。硝酸バリウMム、硝酸ユーロピウム、硝酸マグネシウム及びコロイド状アルミナを、BAMの当量に基づいて約8重量パーセントの濃度を有する前駆体溶液内に形成した。ユーロピウムは5原子パーセントで組み込まれた。溶液は約1.6MHzの周波数で超音波トランスデューサを用いて霧化した。エアロゾルはスプレイ転換された中間前駆体粉体を形成するために950℃の反応温度で、チューブ式加熱炉内で熱分解された。粉体はその後、H2/N2雰囲気の下で1450℃の温度で、2時間加熱処理された。この粉体を図57の顕微鏡写真に示す。粉体の粒子径分布は図58に示されている。平均粒子径は1.88μmであり、重量による粒子の90%は大きさの面では3.51μm以下であった。粉体は強い光ルミネセンスを示した。
つくられた粉体を図59のSEM顕微鏡写真に示す。粒子径分布は図60に示されている。平均粒子径は2.139μmであり、前記粒子の90パーセントは3.608μm以下の大きさであった。図61のX線回折パターンは粒子がほぼ相純粋なホウ酸イットリウム及び高い結晶性を有するホウ酸ガドリニウムであることを示している。
上に本発明のいろいろな実施例が詳細に示したが、これらの実施例の改変及び適用が可能であることは当業者にも自明であろう。しかし、それらの修正や適用も本発明の精神及びその範囲内であることは容易に理解されよう理解されるところであろう。
Claims (8)
- 光ルミネセンス蛍リン光体粒子を含む安全管理用製品であって、
前記粒子は、0.1μmから10μmの体積平均粒径を有するとともに球状の形態をしており、前記粒子の少なくとも70体積パーセントが前記平均粒径の2倍以下であり、前記蛍リン光体粒子はホスト物質と、同ホスト物質にわたって均一に分散された1つ以上の微量添加物と、を含み、かつ、
前記蛍リン光体粒子は、イットリウム−ガドリニウム・ホウ酸塩を含み、
前記微量添加物は、Euを含む、安全管理用製品。 - 前記蛍リン光体粒子は、印刷された印の形状である、請求項1に記載の安全管理用製品。
- 前記製品は、通貨の形態である、請求項1に記載の安全管理用製品。
- 前記粒子は、0.3μmから5μmの体積平均粒径を有する、請求項1に記載の安全管理用製品。
- 前記粒子の少なくとも90体積パーセントが前記平均粒径の2倍以下である、請求項1に記載の安全管理用製品。
- 前記粒子は、少なくとも25ナノメートルの平均結晶体サイズを有する結晶体を含む、請求項1に記載の安全管理用製品。
- 前記粒子は1原子パーセント以下の不純物を含む、請求項1に記載の安全管理用製品。
- 前記粒子は、ほぼ団粒化されていない、請求項1に記載の安全管理用製品。
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US09/141,393 US6197218B1 (en) | 1997-02-24 | 1998-08-27 | Photoluminescent phosphor powders, methods for making phosphor powders and devices incorporating same |
US09/140,525 | 1998-08-27 | ||
US09/141,393 | 1998-08-27 | ||
US09/141,386 US6210604B1 (en) | 1997-02-24 | 1998-08-27 | X-ray phosphor powders, methods for making phosphor powders and devices incorporating same |
US09/141,405 | 1998-08-27 | ||
US09/141,386 | 1998-08-27 | ||
US09/141,405 US6168731B1 (en) | 1997-02-24 | 1998-08-27 | Cathodoluminescent phosphor powders, methods for making phosphor powders and devices incorporating same |
US09/140,525 US6193908B1 (en) | 1997-02-24 | 1998-08-27 | Electroluminescent phosphor powders, methods for making phosphor powders and devices incorporating same |
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JP2010183169A Expired - Fee Related JP5837289B2 (ja) | 1998-08-27 | 2010-08-18 | 光ルミネセンス蛍リン光体粒子を含む安全管理用製品 |
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JP (3) | JP2002523610A (ja) |
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-
1999
- 1999-08-26 AU AU60212/99A patent/AU6021299A/en not_active Abandoned
- 1999-08-26 EP EP99968245A patent/EP1127098A4/en not_active Ceased
- 1999-08-26 WO PCT/US1999/019582 patent/WO2000012649A1/en active Application Filing
- 1999-08-26 CA CA2345300A patent/CA2345300C/en not_active Expired - Fee Related
- 1999-08-26 JP JP2000567645A patent/JP2002523610A/ja active Pending
-
2010
- 2010-08-18 JP JP2010183169A patent/JP5837289B2/ja not_active Expired - Fee Related
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2014
- 2014-08-08 JP JP2014162326A patent/JP2015018812A/ja active Pending
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WO2000012649A1 (en) | 2000-03-09 |
EP1127098A4 (en) | 2006-05-24 |
JP2015018812A (ja) | 2015-01-29 |
EP1127098A1 (en) | 2001-08-29 |
AU6021299A (en) | 2000-03-21 |
CA2345300C (en) | 2012-01-24 |
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