TW201038718A - Co-doped 2-5-8 nitrides - Google Patents
Co-doped 2-5-8 nitrides Download PDFInfo
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- TW201038718A TW201038718A TW099105745A TW99105745A TW201038718A TW 201038718 A TW201038718 A TW 201038718A TW 099105745 A TW099105745 A TW 099105745A TW 99105745 A TW99105745 A TW 99105745A TW 201038718 A TW201038718 A TW 201038718A
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- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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Description
201038718 六、發明說明: 【發明所屬之技術領域】 本發明係關於由以Eu及/或Ce活化之經Hf4+、Zr4+、 Li+、Na+及/或K+共摻雜之2-5-8鹼土金屬矽氮化物組成之 化合物,關於其製備及其於暖白色光LED或所謂的隨選色 彩應用中作為磷光體及LED轉換磷光體之用途。 【先前技術】 隨選色彩概念係意指藉由使用一或多個磷光體之 pcLED(=磷光體轉換LED)方法獲得具有某一色點之光。使 用此概念係(例如)為生產某些企業設計,例如用於闡明公 司標誌、商標等。 磷光體轉換LED代表一重要光技術,其創新潛能導致傳 統人工光源(白熾燈、放電燈等)之替代增加。雖然LED幾 乎已用盡半導體技術,但是所使用之磷光體提供改善之空 間。LED製造商係重複強調紅色磷光體對於(功率)LED之 必要性。紅色磷光體高效及有效地用於LED之必需特性尤 其係: 發射能帶之波長範圍係610至620 nm(具有CRI或高CCT之 一般照明),或63 0 nm及65 0 nm(用於具有大色空間之LC顯 示器之背光)。 高螢光淬火溫度(TQ5〇»150°C )。 對酸及水分之高化學安定性。 高光產率,其係由激發LED之發射能帶之光譜區域内之高 吸收、自磷光體至環境之高發射光萃取率及高轉換效率 146469.doc 201038718 (QE) 〇 有諸多符合某些(但不是全部)上述LED製造商所要求之 條件之磷光體材料系統。然而,僅符合全部條件才能顯著 加速藉由LED替代傳統電子光源並導致全世界照明 能之減少。 發射紅色營光且原則上可與藍光(或uv)led組合之市售 磷光體材料特定言之為: 原矽酸鹽: 此等物質具有高亮度及效率,但是最長發射波長為約 610 nm。 硫化物、硫代鎵酸鹽及硫砸化物: 此等磷光體能發射上述波長範圍。含硫材料之最大缺點 係其對大氣中氧氣及水分之不安定性。兩者藉由聚矽氧黏 合劑材料擴散通過至磷光體並與其反應而非常容易進入 LED中,其在此期間分解。此外,僅低摻雜程度經常可在 高激發密度下產生飽和現象。 氮化物及氮氧化物: 共價氮化物原則上可用作磷光體之基質,因為其具有大 能帶間隙,活化劑離子之HOMO及LUMO係位於其中。因 為高共價性,氮化物具有大電子雲擴散效應,因此稀土活 化劑(例如’ Eu2+,Ce3+)已激發4f5d組態之最低晶體場組 分之能量下降。此導致氮化物磷光體之長波激發及發射 (參見 Krevel等人 ’ J. Alloys Conmpd· 1998, 268,272)。 尤其係矽氮化物與氧基矽化合物顯示一密切關係,因為 146469.doc 201038718 兩系統皆係由Six*四面體(X=0、N)所建立。然而,由於矽 氮化物比氧基矽化合物的縮合程度更高,所以具有比其更 高的化學安定性(參見Xie等人,Sci. Tech. Adv. Matei·. 2007, 8, 588)。 特定言之’矽氮化物係適於以活化劑離子(如Eu2+及 Ce3 + )摻雜,其中至少一個處於激發態之電子未受晶體場 (5 s及5d)作用遮蔽。此等活化劑具有高度取決於環境(對稱 性、共價性、配位、場強度、鍵長、晶格位置大小)之光 譜特性。對照於氧之低形式電荷(〇2-),氮之高形式電荷 (N3_)使矽氮化物中上述活化劑比類似Si_〇材料的情況經歷 較大5d軌道之晶體場分裂,且5d軌道之能量中心係偏移至 更低能量。因此,該活化劑之激發及發射能帶顯示光譜紅 位移。此外,相較於氧基矽化合物,矽氮化物之更穩固及 更剛性的晶格導致斯托克斯(Stokes)位移減少,因此熱淬 火僅發生在較南溫度下且轉換效率增加。 待公開之第一個矽氮化物磷光體系統係CaSiN2:Eu2+(參 見 Lim 專人 ’ SPIE 第 3241 卷 ’ 1997, Photoluminescence of
CaSiNyEu)。此磷光體係適宜作為發射藍光及uv之LED之 轉換器,因為其在此等波長範圍内激發下於約63〇 nm處顯 示螢光。 EP 1153101 及 EP 1238041 描述所謂具有(Ca、Sr、Ba)2x
SisNyEux組成之「2-:5-8」矽氮化物。此等磷光體可自近_ UV激發至藍光光譜區域並取決於化學組成發射橘色至深 紅色光。 146469.doc 201038718 f發明内容】 因此,本發明之目標係以此等化合物達到 率之方式改良上述2-5-8鹼土金屬矽氮化物。 甚至更高光效 已驚人地發現,如果以四價及/或單價陽離子進行共摻 雜’則可滿足進-步增加(Ca,Sr,Ba)2 xSi5N8:EUx鱗光體之 轉換效率之經濟重要的需求。 ❹ 因此,本發明係關於具銪及/或鈽摻雜之2_5_8鹼土金屬 矽氮化物型之化合物,其另外包括銓、錯、鋰、鈉及/或 鉀作為共掺雜劑。 2-5-8鹼土金屬矽氮化物」(亦稱為「2_5_8氮化物」或 「2-5-8鹼土金屬氮基矽酸鹽」)意指M2Si5N8:Eu2+組合物, 其中Μ表示鹼土金屬或複數個鹼土金屬之混合物。 較佳係式(I)化合物:
Ma2.y(Ca,Sr,Ba)i.x.ySi5.zMezN8:EuxCey ⑴ 其中 ❾
Ma=Li、Na及/ 或 K Me=Hf4+及 / 或 Zr4+ x=0.0015 至 0.20 y=0至 0.15 及 z<4 ° 較佳係z值(其表示共摻雜劑Me之原子濃度)<1,更佳係 <0.1 ’ 最佳係 0.0002 至 〇.〇2。 較佳係 x=0.005 至 0.19 且 y=〇 至 0.08。 146469.doc 201038718 相較於彼等相同組成但無共摻雜劑Hf& /或△者,根據 本發明之式I化合物或磷光體之較高亮度可藉由熟習此項 技術者已知理論以此等離子對活化劑離子之激發態壽命有 影響來解釋··在發射螢光之相對短的時間之後,此等鱗光 體之激發電子回歸至基態,# :該等電子在相同時間間隔 内可進行更多激發及鬆弛過程(參見s. Shi〇n〇ya,w m
Yen, Phosphor Handbook, CRC Press, New York, 1999, ISBN 0-8493-7560-6)。 熟習此項技術者已知使用Ce3 +共活化Eu2 +磷光體可導致 該Eu2+磷光體之有利特性,而使該磷光體更有效或更安 定。 此外,該等共摻雜劑可具有增加效率之作用因為其等 可結合矽氮化物中所存在之非所需氧(其導致亮度或效率 降低及色點位移)。 根據本發明化合物之粒徑係在5〇 nm與3〇 μιη之間,較佳 係1 μιη與20 μιη之間,更佳係2 1 5 pm之間。 較佳可將單價離子(如Li、Na及/或尺,及函素,如?或 C1)併入根據本發明化合物之晶格中。該等單價離子較佳 係用作磷光體製備期間之助熔劑,並用於增加結晶品質、 粗略設定粒徑及顆粒形態,並因此具有增加該等磷光體效 率之尚潛能。此程序係為熟習此項技術者已知(參見(例
如)H.S_ Kang 等人,Mater. Science and Engineering B 121(2005)81-85)。 此外,氧及碳可以<〇·2 at_%之含量存在於根據本發明之 146469.doc 201038718 2-5-8氮化物之晶格中。已知該等物質經由助熔劑的使用或 自起始材料係適宜作為該等氮化物之成分(參見Hintzen等 人,Chem. Mater. 2005 17,3242-48「Synthese von
Me2Si5N8:Eu aus Me-Carbonaten」[Synthesis of Me2Si5N8: Eu from Me carbonates]或 X· Piao 等人,Applied Physics Lett. 88,161908(2006)「C/mrac/erkai/ow /wmhescence properties of Sr2S15N8:Eu2+ phosphor for white light- ⑽」或 r Xie等人,chem. Mater. 2006,18(23),5578-5583「J awi/zei/c route to SrSiN:Eu-based red phosphors for white LED Λ )。 2-5-8氮化物亦可能經Μη、Mg、Be、Ni、Co、Th及/或 Ru共摻雜’其中可將F、〇或C另外併入本文之晶格中。 本發明另外關於一種能藉由以固態擴散方法使含氮化 石夕、销、鈽及#5及/或總及/或鎖之起始材料與至少一種含 铪、锆、鋰、鈉及/或鉀之共摻雜劑混合及隨後進行熱後 處理而獲得之化合物。 本發明另外關於一種製備經銪及/或鈽掺雜之2_5_8鹼土 金屬矽氮化物型之化合物之方法,其具有以下製程步驟: •藉由混合至少4種選自含氮化矽、銪、鈽、鈣、勰、 鋇、給、結、鍾、鈉及/或鉀之材料之起始材料製備 經含铪、錘、鋰、鈉及/或鉀之材料共摻雜之如及/或 Ce摻雜的2-5-8鹼土金屬矽氮化物, •熱後處理經Hf及/或Zr共摻雜之化合物。 用於製備該化合物之起始材料係由以下各者組成(如上 146469.doc 201038718 :述般):氮切(Si3N4)、氫㈣、氟化銪及/或氟化飾及 /種输^⑽及糾之共掺雜齊卜除較佳的 鼠化物、氫化物及氟化物以外,適宜的起始材料亦為其他 :機及/或有機物質,#氰胺類、二氰胺類、氰化物、草 酸鹽、丙二酸鹽、I馬酸鹽、碳酸鹽、檸檬酸鹽、抗壞血 酉欠鹽及乙酿丙綱酸鹽。 上述之熱後處理(參見製程步_係在還原條件下(例如) 以成形氣體(例如9〇/1())、純氫氣及/或在氨氣氛圍下及/或 具或不具上述氛圍之氮氣或甲烧與氮氣之混合物需進行多 個小時中此處理亦可在超大氣壓下進行。煅燒製程期 間之溫度係在100(rc與180(rc之間,較佳為i2〇(rc與 165 0°C 之間。 借助於上述製程,可生產根據本發明化合物或磷光體之 任何所需外形,如球形顆粒、薄片及結構化材料及陶瓷。 該等形狀根據本發明係概括於術語「成形主體」中。該成 形主體較佳係「磷光體元件」。 因此,本發明另外關於一種包含根據本發明化合物之具 有粗糙表面的成形主體’該粗糙表面具有包括si〇2、 Ti〇2、Al2〇3 ' ZnO、ZrOj/或γ2〇3或其混合氧化物之奈 米微粒及/或包括含或不含選自銪、鈽、姶、鉛、鋰 '鈉 及/或鉀系列之摻雜劑的根據本發明化合物之顆粒。 在另一項較佳實施例中,該成形主體在LED晶片之相對 側上具有結構化(例如錐形)表面(參見w〇 2〇〇8/〇58619, Merck ’將其全部範疇以引用的方式併入本發明申請案之 146469.doc 10 201038718 内文中)。此可使該磷光體儘可能耦合輸出較多的光。 在成形主體上之結構化表面係藉由隨後用經已結構化之 適宜枋料塗覆’或在隨後步驟中藉由(光)微影製程、餘刻 ' #程或藉由使用能量束或材料喷射或機械力作用之寫入製 . 程製造。 在另-項較佳實施例中,根據本發明之成形主體在 曰曰片之相對側上具有粗糙表面,該粗糙表面具有包含 〇 ⑽2、加2、Ah〇3、Μ、Zr〇2及/或Y2〇3或該等材料之 組合之奈米微粒,及/或具有含或不含選自Μη、吨、Be、 Ni Co、Th及/或RU系列之捧雜劑的式j鱗光體組合物之微 粒。本文之粗糙表面具有至多數1〇〇 nm之粗糙度。經塗覆 之表面具有可減少或避免總内反射且根據本發明碟光體可 更好地耦合輸出光之優點(參見w〇 2〇〇8/〇586ΐ9(ΜαΑ), 將其全部範疇以引用的方式併入本發明申請案之内文 中)。 〇 此外’根據本發明之成形主體較佳在與晶片相對的表面 上具有折射率匹配之層’其可簡化-次輻射及/或由磷光 體元件所發射之輻射之耦合輸出。 .在另"'項較佳實施财,該等成形主體具有-由Si〇2、 乃〇2、A1203、Zn0、响及/或γ2〇3或其混合氧化物及/或 由不含活化劑銪及/或飾之U化合物組成之連續表面塗 層。此表面塗層具有適宜逐漸變化之塗料折射率能使折射 率與環境相匹配之優點。在此情況下,在鱗光體表面之光 散射減少且較大比例之光可穿透進入麟光體並於該處被吸 146469.doc 201038718 收及轉換。此外,因為總内反射減少,匹配折射率之表面 塗層能使磷光體耦合輪出更多光。 此外’如果必須封裝該磷光體,則以連續層為宜。為了 抵消磷光體或其部分對於擴散水或切身環境中之其他物質 之敏感性,可能必需有此步驟。以封閉護套封裝之另一原 因係κ際鱗光體因晶片中形成熱而熱去耦合。此熱導致填 光體之螢光光產率減少且亦影響螢光之顏色。最後,此類 型之塗層藉由阻止磷光體中形成的晶格振動傳播至環境中 使其可增加碟光體之效率。 此外,該成形主體較佳係具有由Si〇2、Ti〇2、Ahh、
ZnO、Zr〇2及/或ΙΑ或其混合氧化物及/或由含或不含選 自Eu、Ce、Hf、Zr、Li、他及/或〖系列之摻雜劑之式工化 合物組成之多孔表面塗層。此等多孔塗層提供進一步降低 單層折射率之可能性。此類型之多孔塗層可藉由三種習知 方法製造,如W〇 〇3/〇27〇15(將其全部範疇以引用的方式 併入本發明申請案之内文)中所述:玻璃之链刻(例如_ 玻璃(參見US 4019884))、多孔層之應用及多孔層與蝕刻方 法之組合。 又丨土只犯w 丫,该成形主體具有表面,該表 具有利於化學或物理鍵結至較佳由環氧樹脂或聚珍氧樹 組成之環境之官能基。此等官能基可係酯類或其他“列 經由能與基於環氧化物及,或聚矽氧之黏合劑成分形成 接之氧基鍵結之衍生物。此類型之表面具有利於均質混 鱗光體至黏合劑中之優點。此外,因此可將碟光體_ 146469.doc •12- 201038718 劑系統之流變特性以及適用期調整至某一程度。因此簡化 混合物之處理。在此連接中物理鍵結至環境意指該等系統 之間經由電荷波動或部分電荷之靜電相互作用。 □為'塗覆至led晶片中之根據本發明填光體層較佳係由 - 料氧及均㈣光體微粒之混合物組成,且該聚石夕氧具有 表面張力,所以此磷光體層在微觀級下係不均一或該層之 厚度係完全不固定。 〇 作為另—項較佳實施例,薄片形磷光體係藉由習知方法 自相應金屬及/或稀土鹽製備。該製備方法係詳細描述於 EP聰73及W0 2_/㈣㈣中,將其等之全部範β壽以引 用=方式併入本發明申請案之内文中。此等薄片形填光體 可藉由在水性分散液或懸浮液中之沉殿反應,利用麟光體 層塗覆天然或合成製造之具有極大縱橫比、原子級光滑表 面及可調整厚度的高穩固性支揮體或基板(其包括(例如)雲 母缚片、Si〇2_ 片、Ain Α】2〇3溥片、Zr〇2溥片、玻璃薄片或 〇 Ti〇2薄片)而製得。除了雲母、加2、_2、八12〇3、玻璃 或Ti〇2或其混合物以外,該等薄片亦可由麟光體材料本身 組成或自一材料建立。如果該薄片本身僅作為磷光體塗層 之支撐體,則後者必須係由對來自LED之-次輻射為透明 或=收該一次韓射並傳送此能量至磷光體層之材料組成。 X薄片开/ 4光體係分散於樹脂中(例如聚矽氧或環氧樹 脂),及此分散液係塗覆至LED晶片上。 該薄片形磷光體可以厚度為50 nm至約20 _,較佳在 150⑽心叫間的大工業規模製得。本文之直徑係50 146469.doc 201038718 nm至 20 μηι。 其等-般所具有之縱橫比(直徑對微粒厚度之比例)係i: i 至400:1,及尤其係3:1至100:1。 薄片尺寸(長度X寬度)係取決於配置。薄片亦係適宜作 為轉化層内之散射中心,尤其係如果其具有特別小的尺 寸。 面對LED晶片之根據本發明薄片形碟光體之表面可具備 一具有相對於LED晶片所發射之—次㈣具有反射減少作 用之塗層。此使-次輻射之反向散射減少,增強後者與根 據本發明之磷光體元件之搞合。適於此目的者係(例如)折 射率匹配之塗層’其必須具有下列厚度d:d=[來自[即晶片 之一次輻射之波長/(4*磷光體陶瓷之折射率)],參見(例 如)Gerthsen,Physik[Physics],Springer VerUg,第 18版, 。此塗層亦可由光子晶體組成,其亦包括結構化薄片 形磷光體之表面以實現某些功能。 製備呈陶瓷元件形式之根據本發明成形主體係以類似於 彻_/〇17353(Merck)中所描述之方法進行,將其全部 範疇以引用的方式併入本發明申請案之内文中。本文之磷 光體係藉由相應、&始材料及摻雜劑混纟,隨後均衡擠壓混 &物並以均g、薄且無孔薄片形式將該混合物直接塗覆在 曰曰片表面或離晶片一段距離處(遠端磷光體概念)的方式製 備匕各別配置尤其取決於LED裝置之結構,賓办習此項技術 者月匕選擇有利白勺西己置。碟光體之激發及發射因此發生無位 置依賴性之變化’使其所提供之該led發射固定色彩之均 146469.doc •14· 201038718 質錐形光束並具有高光功率。該陶竟鱗光體元件可以大型 工業規模生產’例如厚度為數1〇〇 nm至約5〇〇 薄片。 該薄片尺寸(長度X寬度)係取決於配置。在直接塗覆於晶 片之情況下’該薄片之尺寸應根據在適宜的晶片配置(例 • 如覆晶配置)或對應情況下具有晶片表面之約1〇%至3〇%之 某一超出尺寸之晶片尺寸(約1〇〇 μιη*1〇〇 0111至數1111112)選 擇。如果該磷光體薄片係安裝於完成LED之頂端,則所有 0 發射之錐形光束將碰撞該薄片。 該陶瓷磷光體70件之側表面可以輕或貴金屬(較佳係鋁 或銀)金屬化。該金屬化具有使光不會自磷光體元件側面 射出之作用。光側面射出會減少LED耦合輸出之光通量。 β亥陶瓷磷光體元件之金屬化係在均衡擠壓以獲得桿狀物或 薄片後之製程步驟進行’其中若需要,該等桿狀物或薄片 可先切割成所需尺寸,再金屬化。為此目的,將側表面 (例如)經硝酸銀及葡萄糖溶液潤濕,及隨後將其暴露於高 〇 溫下氨氣氛圍中。在此操作期間’在側表面上形成(例如) 銀塗層。 或者,無電鍍金屬化方法係適宜的’參見(例如) Hollemann-Wiberg, Lehrbuch der Anorganischen Chemie [Text-book of Inorganic Chemistry], Walter de Gruyter Verlag、或 Ullmanns EnzyklopSdie der chemischen Technologie [Ullmann's Encyclopaedia of Chemical Techonology]。 如果需要’可使用水玻璃溶液將該陶瓷磷光體元件固定 至LED晶片之基板上。 146469.doc 15 201038718 在另一項實施例中,該陶瓷磷光體元件在LED晶片之相 對側上具有結構化(例如錐形)表面。此能使磷光體元件儘 可能耦合輸出較多的光。在磷光體元件上之結構化表面係 藉由使用具有結構化擠壓盤之模子進行均衡擠壓並因此將 結構壓印至該表面的方式製得。如果目標係製造最薄的可 月b砑光體元件或薄片,則需要結構化表面。擠壓條件係熟 S此項技術者已知(參見j KriegSmann,Technjsche ramische Werkstoffe [Industrial Ceramic Materials],第 4 早,Deutscher Wirtschaftsdienst ’ 1998)。重要的是,所使 用之擠壓溫度為待擠壓物質之炫點之2/3至5/6。 本發明另外關於一種製備成形主體,較佳為磷光體元件 之方法,其具有下列製程步驟: a) 藉由混合至少4種選自含氮化矽、銪、鈽、鈣、锶、 鋇、铪、錯、鋰、鈉及/或鉀之材料之起始材料,製備經 含铪及/或鍅之材料共摻雜的銪摻雜之2 5_8撿土金屬矽氮 化物化合物, b) 熱後處理該共摻雜之化合物並形成一具有粗糙表面之成 形主體, c) 以包括 Si02、Τι〇2、A1203、ZnO、&02及/或 γ2〇3或其昆 合乳化物之奈米微粒或以包括根據本發明化合物之奈米微 粒塗覆該粗糙表面。 此外’根據本發明之鱗光體可在寬範圍内激發,該範圍 係由約250 nm延伸至53G _,較佳為43() _延伸至約· 職。因此’此等磷光體不僅適於藉由發射或藍光之一 146469.doc -16· 201038718 次光源(如LED或習知放電燈(例如基於^^者)),而且亦適 於類似彼等利用45 1 nm之藍光ΐη3 +線之絲激發。 本發明另外關於一種具有至少一種發射最大值在250 nm 至530 nm之範圍,較佳為43〇 nm至約5〇〇 nm ,特佳為44〇 與480 nm之間之範圍之一次光源的發光單元,其中該一次 輻射係藉由根據本發明之化合物或磷光體部分或完全轉換 為車父長波長之輻射。此發光單元較佳係發射白光或發射具 有某一色點之光(隨選色彩原則)。根據本發明之發光單元 之較佳實施例係描述於圖9至2〇中。 在根據本發明發光單元之-項較佳實施例中,該光源係 發光氮化鋁鎵銦,尤其係式hGajAlkN者,其中,〇匀, 〇分,及i+j+k=l。此類型光源之可能形式係為熟習此項技 術者已知。其可係具有各種結構之發光led晶片。 在根據本發明發光單元之另一項較佳實施例中該光源 係基於ZnO、TCO(透明傳導氧化物)、ZnS^沉之發光 配置或有機發光配置(oled)。 在根據本發明發光單元之另_項較佳實施例中,該光源 係一顯示電致發光及/或光致發光之源。此外,該光源亦 可係電漿或放電源。 根據本發明之填光體可分散於樹脂中(例如環氧樹脂或 聚石夕氧樹脂),或依適宜的尺寸比例直接配置於—次光源 上’或根據應用遠離其配置(後一配置亦包括「遠端石粦光 體技術」)。遠端磷光體技術之優點係為熟習此項技術者 已知並揭示於(例如)下列公開案中:Japanese J_· of 146469.doc 17 201038718
Appl.Phys·第 44卷,第 21號(2〇〇5) l649 l65i。 在另一項實施例中,在磷光體與—次光源間之 之先料合較佳係、藉由光傳導配置方法實現。此能使一: 光源女裝在中心位置處並藉由光傳導裝置(如(例如)光傳 纖維)之方法光㈣合至磷光體。依此方式可實現與發光 願景相配且僅由-或不同個可經配置以形成光屏之鱗光體 及耦合至-次光源之光傳導器組成之燈。依此方法可在有 利於2力設備之位置安置—強—次光源,且可在任何所需 位置安裝包括耦合至光傳導器之磷光體之燈而無需其他電 纜’但僅由操作光傳導器替代。 本發明另外關於根據本發明之化合物及成形主體作為磷 光體或填光體元件之用途。 本發明另外關於根據本發明之化合物用於部分或完全轉 換來自發光二極體之藍光或近_UV發射之用途。 此外’根據本發明之化合物較佳係用於將藍光或近_uv 發射轉換成可見白色輻射。此外,根據本發明之化合物較 佳係用於根據「隨選色彩」概念將一次輻射轉換成某一色 點。 根據本發明之式I化合物可個別或以混合物形式使用下 列熟習此項技術者熟知的磷光體:
Ba2Si04:Eu2+, BaSi2Os:Pb2+, BaxSri,.xF2:Eu2+, BaSrMgSi2〇7:Eu2+, BaTiP207, (Ba,Ti)2P2〇7:Ti, Ba3W06:U, BaY2F8 Er3+,Yb+, Be2Si04:Mn2+, Bi4Ge30]2, CaAl204:Ce3+, CaLa407:Ce3+, CaAl2〇4:Eu2+, CaAl204:Mn2+, CaAl407:Pb2+,Mn2+, CaAl204:Tb3+, Ca3Al2Si3〇i2:Ce3+, 146469.doc -18- 201038718
Ca3Al2Si30i2:Ce3+,Ca3Al2Si30,2:Eu2+,Ca2B509BnEu2+, Ca2B509Cl:Eu2+,Ca2B509Cl:Pb2+,CaB204:Mn2+,Ca2B205:Mn2+, CaB204:Pb2+, CaB2P2〇9:Eu2+, Ca5B2SiO10:Eu3+,
Ca0.5Baa5Al12O19:Ce3+,Mn2+, Ca2Ba3(P04)3Cl:Eu2+,CaBr2:Eu2+ in Si02, ' CaCl2:Eu2+ in Si02, CaCl2:Eu2+,Mn2+ in Si02, CaF2:Ce3+, - CaF2:Ce3+,Mn2+, CaF2:Ce3+,Tb3+, CaF2:Eu2+, CaF2:Mn2+, CaF2:U,
CaGa2〇4:Mn2+, CaGa407:Mn2+, CaGa2S4:Ce3+, CaGa2S4:Eu2+, CaGa2S4:Mn2+, CaGa2S4:Pb2+5 CaGe03:Mn2+, CaI2:Eu2+ in Si02, CaI2:Eu2+,Mn2+ in Si02, CaLaB04:Eu3+, CaLaB307:Ce3+,Mn2+, 〇 Ca2La2B〇6.5:Pb2+5 Ca2MgSi2075 Ca2MgSi207:Ce3+, CaMgSi206:Eu2+,
Ca3MgSi208:Eu2+, Ca2MgSi207:Eu2+,CaMgSi206:Eu2+,Mn2+, Ca2MgSi2〇7:Eu2+,Mn2+, CaMo04, CaMo04:Eu3+, CaO:Bi3+, CaO:Cd2+, CaO:Cu+, CaO:Eu3+, CaO:Eu3+, Na+, CaO:Mn2+, CaO:Pb2+, CaO:Sb3+, CaO:Sm3+, CaO:Tb3+, CaO:Tl, CaO:Zn2+, Ca2P207:Ce3+, a-Ca3(P04)2:Ce3+, P-Ca3(P04)2:Ce3+5 Ca5(P〇4)3Cl:Eu2+, Ca5(P04)3Cl:Mn2+, Ca5(P04)3Cl:Sb3+, Ca5(P04)3Cl:Sn2+,a-Ca3(P04)2:Eu2+,Mn2+,Ca5(P04)3F:Mn2+, Cas(P04)3F:Sb3+5 Cas(P04)3F:Sn2+, a-Ca3(P04)2:Eu2+, p-Ca3(P04)2:Eu2+, ❹ Ca2P207:Eu2+,Ca2P207:Eu2+,Mn2+,CaP206:Mn2+, a-Ca3(P04)2:Pb2+, a-Ca3(P〇4)2:Sn2+,p-Ca3(P〇4)2:Sn2+,P-Ca2P2〇7:Sn,Mn, a-Ca3(P〇4)2:Tr, CaS:Bi3+, CaS:Bi3+,Na, CaS:Ce3+, CaS:Eu2+, CaS:Cu+,Na+, CaS:La3+, CaS:Mn2+, CaS04:Bi, CaS04:Ce3+5 CaS04:Ce3+,Mn2+, CaS04:Eu2+, CaS04:Eu2+,Mn2+, CaS04:Pb2+, CaS:Pb2+, CaS:Pb2+,Cl, CaS:Pb2+,Mn2+ CaS:Pr3+5Pb2+,Cl, CaS:Sb3+, CaS:Sb3+,Na, CaS:Sm3+, CaS:Sn2+, CaS:Sn2+,F, CaS:Tb3+, CaS:Tb3+,Cl, CaS:Y3+, CaS:Yb2+, CaS:Yb2+5Cl, CaSi03:Ce3+, Ca3Si04Cl2:Eu2+, Ca3Si04Cl2:Pb2+, CaSi03:Eu2+, CaSi03:Mn2+,Pb, CaSi03:Pb2+, CaSi03:Pb2+,Mn2+, CaSi03:Ti4+, CaSr2(P04)2:Bi3+,p-(Ca,Sr)3(P04)2:Sn2+Mn2+,CaTi"Al(M〇3:Bi3+, 146469.doc •19- 201038718
CaTi03:Eu3+,CaTi03:Pr3+,Ca5(V04)3Cl,CaW04, CaW04:Pb2+, CaW04:W, Ca3W06:U, CaYA104:Eu3+, CaYB04:Bi3+, CaYB04:Eu3+, CaYB〇.803.7:Eu3+, CaY2Zr06:Eu3+, (Ca,Zn,Mg)3(P〇4)2:Sn5 CeF3, (Ce,Mg)BaAln〇i8:Ce, (Ce,Mg)SrAl„018:Ce, CeMgAlu019:Ce:Tb,Cd2B6011:Mn2+,CdS:Ag+,Cr,
CdS:In, CdS:In, CdS:In,Te, CdS:Te, CdW04, CsF,Csl,CsI:Na+,CsI:Tl, (ErCl3)〇.25(BaCl2)〇.75, GaN:Zn, Gd3Ga5012:Cr3+, Gd3Ga5〇12:Cr,Ce,
GdNb04:Bi3+, Gd202S:Eu3+, Gd202Pr3+, Gd202S:Pr,Ce,F, Gd202S:Tb3+, Gd2Si05:Ce3+, KAI„017:T1+, KGau017:Mn2+, K2La2Ti3〇i〇:Eu, KMgF3:Eu2+, KMgF3:Mn2+, K2SiF6:Mn4+, LaAl3B40,2:Eu3+, LaAlB206:Eu3+, LaA103:Eu3+, LaAl〇3:Sm3+, LaAs04:Eu3+, LaBr3:Ce3+, LaB03:Eu3+, ◎ (La,Ce,Tb)P04:Ce:Tb, LaCl3:Ce3+, La203:Bi3+, LaOBr:Tb3+, LaOBr:Tm3+, LaOCl:Bi3+, LaOCl:Eu3+, LaOF:Eu3+, La203:Eu3+, La203:Pr3+, La202S:Tb3+, LaP04:Ce3+5 LaP04:Eu3+, LaSi03Cl:Ce3+, LaSi03Cl:Ce3+,Tb3+, LaV04:Eu3+, La2W3〇i2:Eu3+5 LiAlF4:Mn2+, LiAl508:Fe3+, LiA102:Fe3+, LiA102:Mn2+, LiAl508:Mn2+, Li2CaP207:Ce3+,Mn2+, LiCeBa4Si4014:Mn2+, LiCeSrBa3Si4〇i4:Mn2+, LiIn02:Eu3+, LiIn02:Sm3+, LiLa02:Eu3+,
LuA103:Ce3+,(Lu,Gd)2Si05:Ce3+, Lu2Si05:Ce3+,Lu2Si207:Ce3+,
LuTa〇4:Nb5+, Lui.xYxAl〇3:Ce3+, MgAl2〇4:Mn2+, MgSrAli〇〇n:Ce,
MgB204:Mn2+,MgBa2(P04)2:Sn2+, MgBa2(P04)2:U,MgBaP207:Eu2+, O
MgBaP207:Eu2+>Mn2+, MgBa3Si208:Eu2+, MgBa(S04)2:Eu2+,
Mg3Ca3(P04)4:Eu2+,MgCaP207:Mn2+, Mg2Ca(S04)3:Eu2+,
Mg2Ca(S04)3:Eu2+,Mn2, MgCeAln019:Tb3+, Mg4(F)Ge06:Mn2+, Mg4(F)(Ge,Sn)06:Mn2+5 MgF2:Mn2+, MgGa2〇4:Mn2+, Mg8Ge2〇nF2:Mn4+, MgS:Eu2+, MgSi03:Mn2+, Mg2Si04:Mn2+, Mg3Si03F4:Ti4+, MgS04:Eu2+, MgS04:Pb2+, MgSrBa2Si2〇7:Eu2+, MgSrP207:Eu2+, MgSr5(P04)4:Sn2+, MgSr3Si208:Eu2+,Mn2+, Mg2Sr(S04)3:Eu2+,Mg2Ti04:Mn4+, MgW04, MgYB04:Eu3+,Na3Ce(P04)2:Tb3+,NaI:Tl,NaiuKowEuo.uTiSLA^Eu3' 146469.doc -20- 201038718
Nai.23K〇.42Eu〇j2TiSi5〇i3-xH20:Eu3+, Nai.29K〇.46Er〇 〇8TiSi4〇ii:Eu3+,
Na2Mg3Al2Si2〇K):Tb,Na(Mg2.xMnx)LiSi4O10F2:Mn,NaYF4:Er3+,Yb3+, NaY02:Eu3+, P46(70°/〇) + P47 (30%), SrAl12019:Ce3+, Mn2+, SrAl204:Eu2+, SrAl407:Eu3+, SrAl12〇i9:Eu2+, SrAl2S4:Eu2+, Sr2B509Cl:Eu2+, • SrB407:Eu2+(F,Cl,Br), SrB407:Pb2+, SrB407:Pb2+5 Mn2+, SrB8013:Sm2+, • SrxBayClzAl204.z/2: Mn2+, Ce3+, SrBaSi04:Eu2+, Sr(Cl5Br,I)2:Eu2+ in Si02, SrCl2:Eu2+ in Si02, Sr5Cl(P04)3:Eu,SrwFxB406.5:Eu2+,SrwFxByOz:Eu2+,Sm2+, SrF2:Eu2+, SrGai2〇i9:Mn2+, SrGa2S4:Ce3+, SrGa2S4:Eu2+, SrGa2S4:Pb2+, SrIn204:Pr3+,Al3+, (Sr,Mg)3(P04)2:Sn,SrMgSi206:Eu2+, Sr2MgSi207:Eu2+, ® Sr3MgSi208:Eu2+, SrMo04:U, SrO-3B203:Eu2+,Cl, fi-SrO-3B2〇3:Pb2+, B-Sr0-3B203 :Pb2+,Mn2+, a-Sr0-3B203:Sm2+, Sr6P5B〇2〇:Eu, Sr5(P04)3Cl:Eu2+, Sr5(P04)3Cl:Eu2+sPr3+, Sr5(P04)3Cl:Mn2+, Sr5(P04)3Cl:Sb3+, Sr2P207:Eu2+,P-Sr3(P04)2:Eu2+,Sr5(P04)3F:Mn2+,
Sr5(P04)3F:Sb3+, Sr5(P04)3F:Sb3+,Mn2+, Sr5(P04)3F:Sn2+, Sr2P207:Sn2+, P-Sr3(P04)2:Sn2+,P-Sr3(P04)2:Sn2+,Mn2+(Al),SrS:Ce3+,SrS:Eu2+,SrS:Mn2+, SrS:Cu+,Na,SrS04:Bi,SrS04:Ce3+, SrS04:Eu2+,SrS04:Eu2+,Mn2+, Sr5Si4〇i〇Cl6:Eu2+, Sr2Si04:Eu2+, SrTi03:Pr3+, SrTi03:Pr3+,Al3+, Sr3W06:U, ❹ SrY203:Eu3+, Th02:Eu3+, Th02:Pr3+, Th02:Tb3+, YAl3B4〇i2:Bi3+5 YAl3B40,2:Ce3+, YAl3B4〇i2:Ce3+,Mn, YAl3B4〇,2:Ce3+,Tb3+5 YA13B40,2:Eu3+5 YAl3B40,2:Eu3+,Cr3+, YAl3B40,2:Th4+,Ce3+,Mn2+, YA103:Ce3+, Υ3Α15〇ΐ2:〇63+, Y3Al5〇i2:Cr3+, YA103:Eu3+, Y3Al5012:Eu3r, Y4A12〇9:Eu3+, Y3Al5〇i2:Mn4+, YA103:Sm3+,YA103:Tb3+, Y3Al5012:Tb3+,YAs04:Eu3+,YB03:Ce3+, ’ YB03:Eu3+, YF3:Er3+,Yb3+, YF3:Mn2+, YF3:Mn2+,Th4+, YF3:Tm3+,Yb3+, (Y,Gd)B03:Eu,(Y,Gd)B03:Tb,(Y,Gd)203:Eu3+,Y134Gci0.60O3(Eu,Pr), Y203:Bi3+5 YOBr:Eu3+, Y2〇3:Ce, Y203:Er3+, Y203:Eu3+(Y0E), Y203:Ce3+,Tb3+, YOCl:Ce3+, YOC1:Eu3+, YOF:Eu3+, YOF:Tb3+, Y2〇3:Ho3+, Y202S:Eu3+,Y202S:Pr3+,Y202S:Tb3+,Y203:Tb3+,YP〇4:Ce3+, 146469.doc -21 · 201038718 YP〇4:Ce3+5Tb3+, YP04:Eu3+, YP04:Mn2+,Th4+, YP04:V5+, Y(P,V)04:Eu, Y2Si05:Ce3+, YTa04, YTa04:Nb5+, YV04:Dy3+5 YV04:Eu3+, ZnAl204:Mn2+, ZnB204:Mn2+, ZnBa2S3:Mn2+,(Zn,Be)2Si04:Mn2+,Zn0.4Cd06S:Ag, Zn〇.6Cd〇.4S:Ag, (Zn,Cd)S:Ag,Cl, (Zn,Cd)S:Cu, ZnF2:Mn2+, ZnGa204, ZnGa2〇4:Mn2+, ZnGa2S4:Mn2+, Zn2Ge04:Mn2+, (Zn,Mg)F2:Mn2+, ZnMg2(P04)2:Mn2+, (Zn,Mg)3(P04)2:Mn2+,ZnO:Al3+,Ga3+, ZnO:Bi3+, ZnO:Ga3+, ZnO:Ga, ZnO-CdO:Ga, ZnO:S, ZnO:Se5 ZnO:Zn, ZnS:Ag+,Cl'5 ZnS:Ag5Cu,Cl, ZnS:Ag,Ni, ZnS:AusIn, ZnS-CdS (25-75), ZnS-CdS (50-50), ZnS-CdS (75-25), ZnS-CdS:Ag5Br,Ni5 ZnS-CdS:Ag+,Cl, ZnS-CdS:Cu,Br, ZnS-CdS:Cu,I, ZnS:Cl', ZnS:Eu2+, ZnS:Cu, ZnS:Cu+,Al3+, ZnS:Cu+,Cl', ZnS:Cu,Sn, ZnS:Eu2+, ZnS:Mn2+, ZnS:Mn,Cu, ZnS:Mn2+5Te2+, ZnS:P, ZnS:P3-,Cr, ZnS:Pb2+, ZnS:Pb2+,Cl'5 ZnS:Pb,Cu, Zn3(P04)2:Mn2+, Zn2Si04:Mn2+, Zn2Si04:Mn2+,As5+, Zn2Si04:Mn,Sb202, Zn2Si〇4:Mn2+,P, Zn2Si04:Ti4+,ZnS:Sn2+,ZnS:Sn,Ag,ZnS:Sn2+,Li+,ZnS:Te,Mn,ZnS-ZnTe:Mn2+, ZnSe:Cu+,Cl, ZnW〇4。 【實施方式】 下列實例意欲闡述本發明。然而’絕不應將其視作限 制。所有組合物中可使用之化合物或組分係已知且可購得 或可藉由已知方法合成得到。實施中所指之溫度總是以。C 提供。無需多言,在描述以及實例中,組合物中組分之添 加量合計總是總和為1 〇〇%。總應將所提供之百分比數據 視為既定關係。但是,其通常總是相對於所指部分量或總 量之重量。 實例 1.製備共摻雜之Ca2Si5N8:Eu(其包括2%及10%之Eu) 實例la :製備作為參考磷光體之Ca2Si5N8:Eu(2°/〇) 146469.doc -22- 201038718 將 2.8730 g 之 CaH2(Alfa Aesar 99.8%)、0.2479 g 之 EuF3(ChemPur 99.9%)A 6.9356 g^Si3N4(UBE 99.99%)^# 除氧氣及水分之手套箱中彼此密切混合,及隨後轉移至内 襯有鉬之剛玉坩堝。隨後將坩堝移入經成形氣體(N2/H2= 90/10)沖洗之管狀爐中並在關閉該爐後,在1400t下煅燒 14 h。最終,將所得燒結餅磨碎、過篩並分類。 實例lb :製備經0.1% Hf共摻雜之Ca2Si5N8:Eu(2%) 將 2.4428 g 之 CaH2(Alfa Aesar 99.8%) ' 0.2477 g 之 EuF3(ChemPur 99.9%)、0.0151 g之HfF4(Alfa Aesar 99.9%) 及6.9299 §之3丨#4(1^£ 99.99%)於排除氧氣及水分之手套 箱中彼此密切混合,及隨後移入内概有鉬之剛玉坩堝。隨 後將坩堝移入經成形氣體(N2/H2=90/l 0)沖洗之管狀爐中並 在關閉該爐後,在1400°C下煅燒14 h。最終,將所得燒結 餅磨碎、過篩並分類。 實例lc :製備經0.1% Zr共摻雜之Ca2Si5N8:Eu(2%) 將 2.4441 g 之 CaH2(Alfa Aesar 99.8%)、0.2479 g 之 EuF3(ChemPur 99.9%)、0.0099 g之 ZrF4(Alfa Aesar 98%)及 6.9335 g之Si3N4(UBE 99.99%)於排除氧氣及水分之手套箱 中彼此密切混合並隨後移入内襯有鉬之剛玉坩堝中。隨後 將坩堝移入經成形氣體(N2/H2=90/l 0)沖洗之管狀爐中並在 關閉該爐後,在1400°C下煅燒14 h。最終,將所得燒結餅 磨碎、過篩並分類。 實例Id :製備作為參考磷光體之Ca2Si5N8:Eu(10°/〇) 將 2.1342 g 之 CaH2(Alfa Aesar 99.8%)、1.1772 g 之 146469.doc -23- 201038718
EuF3(ChemPUr 99.9%)及 6·5858 gui3N4(UBE 99 99%)於排 除氧氣及水分之手套箱中彼此密切混合並隨後移入内襯有 鉬之剛玉坩堝中。隨後將坩堝移入經成形氣體= 90/10)沖洗之管狀爐中並關閉該爐後,在14〇〇〇c下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分類。 實例U :製備經0.1% Hf共摻雜之Ca2Si5N8:Eu(10%) 將 2.1302 g 之 CaH2(Alfa Aesar 99.8%)、1.1762 g 之 EuF3(ChemPUr 99.9%)、0.0143 g之HfF4(Alfa Aesar 99.9%) 及6.5807 g之Si^dUBE 99.99%)於排除氧氣及水分之手套 箱中彼此密切混合並隨後轉入内襯有鉬之剛玉坩禍中。隨 後將掛堝轉入經成形氣體(N2/H2=90/l 0)沖洗之管狀爐中並 在關閉該爐後,在14001下煅燒14 h。最終,將所得燒結 餅磨碎、過篩並分類。 實例If :製備經〇.1% Zr共摻雜2Ca2Si5N8:Eu(1〇0句 將 2.1312 g 之 CaH2(Alfa Aesar 99.8%)、1.1768 g 之 EuF3(ChemPur 99.9%)、0.0094 g之ZrF4(Alfa Aesar 99.9%) 及6.5839 §之8丨3队(1^£ 99.99%)於排除氧氣及水分之手套 箱中彼此密切混合並隨後移入内襯有鉬之剛玉坩堝中。隨 後將坩堝移入經成形氣體(N2/H2=90/10)清洗之管狀爐中並 在關閉該爐後,在14〇(TC下煅燒14 h。最終,將所得燒結 餅磨碎、過篩並分類。 2·製備共摻雜之Sr2Si5N8:Eu(其包括2%之Eu) 實例2a :製備作為參考磷光體之Sr2Si5N8:Eu(2%) W4.4164 g^Sr3N2' 0.1942 EuF3(ChemPur 99.9%)Bl 146469.doc -24- 201038718 5.4337 §之8丨3队(1^£ 99.99%)於排除氧氣及水分之手套箱 中彼此密切混合並隨後移入内襯有鉬之剛玉坩堝中。隨後 將坩堝移入經成形氣體(N2/H2=90/10)沖洗之管狀爐中並在 關閉該爐後’在14 0 0 C下锻燒14 h。最終,將所得燒結餅 磨碎、過篩並分類。 實例2b :製備經0_1% Hf共摻雜之Sr2Si5N8:Eu(2〇/〇)
將 4.4100 g之 Sr3N2、0.1942 g之EuF3(ChemPur 99.9%)、 0.0118giHfF4(AlfaAesar99.9%)&5.4314giSi3N4(UBE 99.99%)於排除氧氣及水分之手套箱中彼此密切混合並隨 後移入内襯有鉬之剛玉坩堝中。隨後將坩堝移入經成形氣 體(N2/H2=90/10)沖洗之管狀爐中並在關閉該爐後,在 1400°C下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分 類。 實例2c :製備經0.1% Zr共摻雜之Sr2Si5N8:Eu(2%) 將4.4118§之81'31^2、0.1942 §之丑1^3(〇16111?1^99.9°/〇)、
0.0078 g之ZrF4(Alfa Aesar 99.9%)及 5.4336 g之 Si3N4(UBE 99.99%)於排除氧氣及水分之手套箱中彼此密切混合並隨 後移入内襯有鉬之剛玉坩堝中。隨後將坩堝移入經成形氣 體(N2/H2=90/10)沖洗之管狀爐中並在關閉該爐後,在 1400°C下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分 類。 3.製備共摻雜之Ba2Si5N8:Eu(其包括2%之Eu) 實例3a :製備作為參考磷光體之Ba2Si5N8:Eu(2%) 將 5.4472 g之Ba3N2、0.1584 g之EuF3(ChemPur 99.9%)及 146469.doc -25- 201038718 4.4305 g之Si3N4(UBE 99_99%)於排除氧氣及水分之手套箱 中彼此密切混合並隨後移入内襯有鉬之剛玉坩堝中。隨後 將坩堝移入經成形氣體(N2/H2=90/10)沖洗之管狀爐中並在 關閉該爐後,在1 400°C下煅燒1 4 h。最終,將所得燒結餅 磨碎、過筛並分類。 實例3b :製備經〇·ΐ% Hf共摻雜之Ba2Si5N8:Eu(2%) 將 5.4408 g之 Ba3N2、0.1584 g之 EuF3(ChemPur 99.9%)、 0.0096 giHfF4(AlfaAesar99.9%)&4.4298 giSi3N4(UBE 99.99%)於排除氧氣及水分之手套箱中彼此密切混合並隨 後移入内襯有鉬之剛玉坩堝中。隨後將坩堝移入經成形氣 體(N2/H2=90/10)沖洗之管狀爐中並在關閉該爐後,在 1400°C下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分 類。 實例3c :製備經0.1% Zr共摻雜之Ba2Si5N8:Eu(2%) 將 5.4426 g之 Ba〗N2、0.1584 g之 EuF3(ChemPur 99.9%)、 0.0063 g^ZrF4(Alfa Aesar 99.9%)^. 4.43 13 g^Si3N4(UBE 99.99%)於排除氧氣及水分之手套箱中彼此密切混合並隨 後移入内襯有鉬之剛玉坩堝中。隨後將坩堝移入經成形氣 體(N2/H2=90/10)沖洗之管狀爐中並關閉該爐後,在1400°C 下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分類。 實例 4:製備經 0.1% Zr 共摻雜之 NaiCao.wZro.cmSU.wNv Ειι0.〇2(其包括 2% 之 Eu) 將 0.81469 g 之 CaH2(Alfa Aesar 99.8%)、0.9288 g 之 NaH(95%,Sigma Aldrich)、0.2479 g之EuF3(ChemPur 99.9%)、 146469.doc -26- 201038718 0.0099 g之 ZrF4(Alfa Aesar 98%)及 6.9335 g之 Si3N4(UBE 99.99%)於排除氧氣及水分之手套箱中彼此密切混合並隨 後移入内襯有鉬之剛玉坩堝中。隨後將坩堝移入經成形氣 體(N2/H2=90/10)沖洗之管狀爐中並在關閉該爐後,在 1400°C下烺燒14 h。最終,將所得燒結餅磨碎、過篩並分 類。 實例 5:製備經 0.1% Zr 共摻雜之 NaiwCao.wZro.oGiSU.wNy Eu〇.〇2Ce〇.〇i(其包括 2% 之 Eu 及 1% 之 Ce) 將 0.7897 g 之 CaH2(Alfa Aesar 99.8%)、0.9146 g 之 NaH(95%,Sigma Aldrich)、0.2479 g 之 EuF3(ChemPur 99.9%) ' 0.1169 g 之 CeF3(ChemPur 99.9%)、0.0099 g 之 ZrF4(Alfa Aesar 98%)^6.9335 g^Si3N4(UBE 99.99%)^# 除氧氣及水分之手套箱中彼此密切混合並隨後移入内襯有 鉬之剛玉坩堝中。隨後將坩堝移入經成形氣體 (N2/H2=90/10)沖洗之管狀爐中並在關閉該爐後,在1400°C 下煅燒14 h。最終,將所得燒結餅磨碎、過篩並分類。 組合物 發射最大值於 「nml 在450 nm之QY Γ%1 CIE 1931 x,y Ca2Si5N8:Eu2+(2.0%) 609 79 0.601 0.397 Ca2Si5N8:Eu2+(2.0%), 608 84 0.600 H^CO.l%) 0.399 Ca2Si5N8:Eu2+(2.0%) > 608 86 0.600 Zr4+(0.1%) 0.398 Sr2Si5N8:Eu2+(2.0%) 619 71 0.629 0.369 146469.doc -27- 201038718
Sr2Si5N8:Eu2+(2.0%) 617 87 0.621 H^CO.l%) 0.372 Sr2Si5N8:Eu2+(2.0%) 617 80 0.629 Zr4+(0.1%) 0.376 Ba2Si5N8:Eu2+(2.0%) 583 76 0.540 0.458 Ba2Si5N8:Eu2+(2.0%) 581 84 0.535 0.462 Ba2Si5N8:Eu2+(2.0%) 581 88 卜 琴---- 0.532 Zr4+(0.1%) 0.466 表 1 ·· MusSisNyEuo.oMMNCa、Sr、Ba)相較於根據本發明 共摻雜之磷光體之光學特性(QY=量子產率) 【圖式簡單說明】 參考諸多工作實例將本發明更詳細地說明於上。圖式顯 示於下。 圖1 :顯示在450 nm之激發波長下’ Cai.98Si5N8:EU〇.02& 共摻雜之磷光體之發射光譜。在此: a)表示非共摻雜之鱗光體, ^表不經⑴:^之汾共摻雜之^^丨心:如㈣^及 c)表示經 〇·ι%之Hf^ 摻雜之 Cai 98Si5N8:EuQ 〇2。 圖2 .顯不圖1之細節放大以更好區別。…及c)之發射光 譜大約相同。 圖3 :顯示在450㈣之激發波長下,Sr] 98_8:Ειι〇 及 共摻雜之磷光體之發射光譜。在此: 幻表示非共摻雜之磷光體, 丁、·工〇.1/q之心共摻雜之SrusSisNyEuow,及 丁、.工 0· 1 /。之 Hf共摻雜之 Sr! 98Si5N8:Eu。们。 146469.doc •28- 201038718 圖4 ··顯示在450 nm之激發波長下,根據本發明之 BausSisNyEuG·。2及共摻雜之磷光體之發射光譜。a)表示非 共摻雜之磷光體,b)表示經〇.1%之Zr共摻雜之 BausSisNyEuo.o2,及c)表示經〇·ι。/。之Hf共摻雜之
BausSisNyEuo.o〗。 圖5 :顯示圖4之細節放大以更好區別發射光譜,。 圖6 ··顯示a)非共摻雜之磷光體,b)經〇_1%之Zr共摻雜之 〇 Cai 98Si5N8:Eu。·。2,c)經 0.1% 之 Hf 共摻雜之 Cah98Si5N8:Eu〇 〇2 之X-射線粉末繞射圖。 圖7 :顯示a)非共摻雜之磷光體,1%之2^共穆雜之
Sr 丨.98Si5N8:EUG.G2,c)經 0.1% 之 Hf 共摻雜之 X-射線粉末繞射圖。 圖8 :顯示a)非共摻雜之磷光體,…經⑴丨^之心共摻雜之 BamSisNvEuow,c)經 〇.1%之财共摻雜之Bai 98Si5N8:Eu〇 ()2 之X-射線粉末繞射圖。 〇 圖9:顯示具有含磷光體之塗層之發光二極體之示意 圖。该組件包括類似晶片之LED 1作為輻射源。該LED係 女裝於一杯狀反射器内,其係藉由調整架2支持。該晶片1 係經由扁面電纜7連接至第一接點6並直接連接至第二電接 -點6 °包括根據本發明之轉換磷光體之塗層塗覆於反射器 杯之内側曲面上。該等磷光體係彼此分開或以混合物形式 使用。(組件編號列:1發光二極體、2反射器、3樹脂、4 轉換磷光體' 5散射器、ό電極、7扁平電纜) 圖10 :顯示一InGaN型之COB(晶片直接黏附在電路板 146469.doc -29- 201038718 上)封裝物’其係用作為白光之光源(LED)(1=半導體晶 片;2、3 =電接點;4 =轉換磷光體;7=電路板)。該磷光體 係分佈於一黏合劑鏡片中,其同時表示第二光學元件且如 鏡片影響光發射特性。 圖11 :顯示一 InGaN型之COB(晶片直接黏附在電路板 上)封裝物,其係用作為白光之光源(LED)( 1 ==半導體晶 片,2、3 =電接點;4 =轉換填光體;7=電路板)。該鱗光體 係位於一直接分佈於該LED晶片上之黏合劑薄層内。其上 可放置由透明材料組成之第二光學元件。 圖12 :顯示用作為白光之光源(LED)之封裝物(1 =半導體 曰曰片,2、3 =電接點;4 =於具有反射器之空腔中之轉換磷 光體)。該轉換磷光體係分散於黏合劑中並以該混合物充 填該空腔。 圖13 :顯示一封裝物,其中1 =罩殼;2 =電接點;4=半導 體曰a片,且s亥空腔底部之該鏡片係經根據本發明之轉換磷 光體完全充填。此封裝物具有可使用較大量之轉換磷光體 之優點。此亦可用作為遠端磷光體。 圖14 :顯示一SMD(表面黏著型裝置)封裝物,其中卜罩 殼;2、3=電接點;4=轉換麟光體。該半導體晶片係藉由 根據本發明之磷光體完全轉換。該SMD設計具有其具有小 物理形狀且因此剛好放入習知燈中之優點。 其中1 =轉換磷光體;2=晶片
圖15 :顯示一T5封裝物, 3、4=電接點;5 = 於該LED晶片之背 146469.doc -30- 201038718 卻之優點。 圖16 :顯示—發光二極體之示意圖,其中1 =半導體晶 片,2、3 =電接點;4=轉換磷光體;5 =接合線,其中該磷 光體係塗覆於黏合劑中以作為頂端球狀物。此形式之磷光 體/黏合劑層可作為第二光學元件並影響(例如)光傳播。 圖17 :顯示一發光二極體之示意圖,其中卜半導體晶 片;2、3=電接點;4=轉換磷光體;5 =接合線,其中該磷 ❹ 光體係以分散於黏合劑中之薄層形式塗覆。作為第二光學 疋件(如(例如)鏡片)之另一組分可容易塗覆於此層。 圖18 ·顯不另一應用如自US-B 6,700,322原則上已知之 實例。根據本發明之磷光體係與〇LED 一起用於此。該光 源係有機發光二極體3丨,其係由實際有機膜3〇及一透明基 板32組成。該膜30發射,尤其係(例如)藉由香豆 素(PVK係聚(N-乙烯基咔唑)之縮寫;卩81)係2_(4_聯苯基)_ 5-(4-第二丁基苯基噁二唑之縮寫)所產生之藍光一 〇 纟光。該發射係部分轉換成黃光,其次藉由自根據本發明 之鱗光體層33所形成之轉換層發射光,使得白光發射整個 係、.丄由'人及一次發射光之色彩混合而實現。該〇LED基 • I上係由至少-個發光聚合物層或所謂兩個電極間之小分 子組成,其係由本身已知之材料組成,如(例如)ιτ〇(氧化 銦錫之縮寫)作為陽極,及高活性金屬(如(例如如或叫作 為陰極。在電極之間亦經常使用複數個層,其係用作為電 洞傳輸層或在小分子領域内,亦作為電子傳輸層。所用發 射聚合物係(例如)聚苐類或聚螺材料。 146469.doc -31 - 201038718 【主要元件符號說明】 圖9 1 發光二極體 2 反射器 3 樹脂 4 轉換磷光體 5 散射器 6 電極 7 扁平電纜 圖10及11 1 半導體晶片 2 電接點 3 電接點 4 轉換磷光體 7 電路板 圖12 1 半導體晶片 2 電接點 3 電接點 4 於具有反射 圖13 1 罩殼 2 電接點 4 半導體晶片 器之空腔中之轉換磷光體 146469.doc 32- 201038718
圖14 1 罩殼 2 電接點 3 電接點 4 轉換磷光體 圖15 1 轉換磷光體 2 晶片 3 電接點 4 電接點 5 用透明樹脂之鏡片 圖16及17 1 半導體晶片 2 電接點 3 電接點 4 轉換磷光體 5 接合線 圖18 30 有機膜 31 有機發光二極體 32 透明基板 33 磷光體層 146469.doc -33-
Claims (1)
- 201038718 七、申請專利範圍: 1. 一種具銪及/或鈽摻雜之2-5-8鹼土金屬矽氮化物型之化 合物’其另外包括姶、銼、鋰、鈉及/或鉀作為共摻雜 劑。 • 2 ·如請求項1之化合物,其特徵在於式I Ma2.y(Ca,Sr,Ba),.x.ySi5.zMezN8:EuxCey (I) 其中 Ma=Li、Na及/或 K ^ Me=Hf4+及/或心“ x=〇.〇015 至 0.20,且 y=〇 至 0.15 z<4 ° ζ<1,較佳 3·如清求項丨或2之化合物,其特徵在於 z<0.1 ’ 更佳係 z=〇 〇〇〇2至〇 〇2。 4·:咕求項!或2之化合物,其可藉由以固態擴散方法使含 ❹ =化砂、销、鈽及約及/或銘及/或鋇之起始材料盘至少 二=、結、链、納及/或钟之共換雜劑混合並隨後進 仃熟後處理獲得。 5. -種製備如請求項!至4中任一項之 有以下製程步驟: 物之方法,其具 a)藉由混合至少4種選自含氮化石夕 鋇、铪、杜 ^ 月鈽、鈣、鋰、 ,"、鋰、鈉及/或鉀之材料之起始枒祖制 铪、鲒、钿h 巧始材枓製備經含 鋰、鈉及/或鉀之材料共摻雜 之2-5-8於+ a ” 銪及/或鈽摻雜 8鹼土金屬矽氮化物化合物, Ί心雜 146469.doc 201038718 b)熱後處理該共摻雜化合物。 6. —種包含如請求項1至4中任一項之化合物之成形主體’ 其特徵在於:其具有載有包含Si02、Ti〇2、Al2〇3、 ZnO、Zr02及/或Y203或其混合氧化物之奈米微粒及/或 包含如請求項1至4中任一項之化合物且含或不含選自 銪、鈽、铪、鍅、鋰、鈉及/或鉀系列之摻雜劑的微粒之 粗糙表面。 7. —種包含如請求項1至4中任一項之化合物 其特徵在於:其具有一由si〇2、Ti〇2、Al2〇3、ZnO、 Zr〇2及/或Y2〇3或其混合氧化物及/或不含活化劑銪之如 請求項1至4中任一項之化合物所組成之連續表面塗層。 8. 一種包含如請求項1至4中任一項之化合物之成形主體, 其特徵在於:其具有一由Si〇2、Ti〇2、Al2〇3、Ζη〇、 Zr〇2及/或ίο;或其混合氧化物及/或含或不含選自銪、 鈽铪、鍅、鋰、鈉及/或鉀系列之摻雜劑的如請求項玉 至4中任項之化合物所組成之多孔表面塗層。 9. 10 一種包含如請求項1至4中任-項之化合物之成形主體, =特徵在於:該表面具有利於化學或物理鍵結至土 環氧樹脂或聚石夕氧樹脂組成之環境之官能基。 土 ::製備如請求項6至9中任一項之成形主體之方 具有下列製程步驟: 其 a)藉由處合至少4錄、阳&人〆 4目仏 種避自含氮化矽、銪、鈽、鈣、热 領、給、jiL、如. 』 鄉、 … 納及/或鉀之材料之起始材料夢備 給及/或锆之材料共換 1備麵含 雜之2-5-8銪摻雜之驗土金屬砂氮 146469.doc 201038718 化物化合物, b) 熱後處理该共換雜之化合物並形成具有粗链表面之成 形主體, c) 利用包括 Si02、Ti〇2、a1203、ZnO、Zr02&/或 γ2〇3 或 . 其混合的氧化物之奈米微粒或利用包含如請求項1至4中 任一項之化合物且含或不含摻雜劑之奈米微粒塗佈該粗 糖表面。 ❹ U. 一種發光單元,其具有至少一種發射最大值在250 nm至 530 nm之範圍内,較佳在390 nm與4 8 0 nm之間的一次光 源’其中此輻射係藉由如請求項1至5中任一項之化合物 或如請求項6至10中任一項之成形主體部分或完全轉換 成較長波長之輻射。 12. 如請求項1丨之發光單元,其特徵在於··該光源係發光氮 化鋁鎵銦’尤其係式IniGajAlkN者,其中〇$i,〇$j, 〇分,及i+j+k=l,或基於Zn〇、TC〇(透明傳導氧化物)、 Q ZnSe或SiC之發光化合物。 13. 如請求項11之發光單元,其特徵在於:該光源係有機發 光配置或電漿或放電燈。 ,14·如請求項11至13中任一項之發光單元,其特徵在於:該 - 磷光體係直接配置於一次光源上及/或其遠端處。 15. 如請求項14之發光單元,其特徵在於:該磷光體與該一 次光源間之光學耦合係藉由光傳導配置實現。 16. 種至少—種如請求項1至4中任一項之化合物作為磷光 體或轉換磷光體之用途,其係用於部分或完全轉換來自 146469.doc 201038718 發光 二極體之藍光或IJV發射。 17. 種如請求項】至41任一項之化合物作為轉換 Q光體之用途,其制於根據隨選色彩概念將—次輕射 轉換成某一色點。 18. 一種如請求項6至9中任一項之成带 之用途。 主體作為磷光體元件 146469.doc -4.
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2009
- 2009-02-27 DE DE102009010705A patent/DE102009010705A1/de not_active Withdrawn
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2010
- 2010-02-01 CN CN2010800093824A patent/CN102333844B/zh not_active Expired - Fee Related
- 2010-02-01 SG SG2011059805A patent/SG173767A1/en unknown
- 2010-02-01 US US13/203,288 patent/US9028716B2/en not_active Expired - Fee Related
- 2010-02-01 EP EP10703006.6A patent/EP2401342B1/de not_active Not-in-force
- 2010-02-01 JP JP2011551427A patent/JP2012519216A/ja active Pending
- 2010-02-01 KR KR1020117022592A patent/KR20110126725A/ko not_active Application Discontinuation
- 2010-02-01 WO PCT/EP2010/000592 patent/WO2010097157A1/de active Application Filing
- 2010-02-26 TW TW099105745A patent/TWI464240B/zh not_active IP Right Cessation
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TWI510599B (zh) * | 2010-05-14 | 2015-12-01 | Lightscape Materials Inc | 以碳氮化物為主之磷光體及利用其之發光裝置 |
TWI572065B (zh) * | 2012-02-09 | 2017-02-21 | 電化股份有限公司 | 螢光體及發光裝置 |
TWI755340B (zh) * | 2017-09-20 | 2022-02-11 | 美商通用電機股份有限公司 | 綠色發光磷光體及其裝置 |
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KR20110126725A (ko) | 2011-11-23 |
US20110304261A1 (en) | 2011-12-15 |
JP2012519216A (ja) | 2012-08-23 |
WO2010097157A1 (de) | 2010-09-02 |
US9028716B2 (en) | 2015-05-12 |
TWI464240B (zh) | 2014-12-11 |
CN102333844B (zh) | 2013-07-31 |
DE102009010705A1 (de) | 2010-09-02 |
SG173767A1 (en) | 2011-09-29 |
CN102333844A (zh) | 2012-01-25 |
EP2401342B1 (de) | 2013-06-12 |
EP2401342A1 (de) | 2012-01-04 |
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