TW200932704A - Ceramic material for LEDs with reduced scattering and method of making the same - Google Patents
Ceramic material for LEDs with reduced scattering and method of making the same Download PDFInfo
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- TW200932704A TW200932704A TW097146966A TW97146966A TW200932704A TW 200932704 A TW200932704 A TW 200932704A TW 097146966 A TW097146966 A TW 097146966A TW 97146966 A TW97146966 A TW 97146966A TW 200932704 A TW200932704 A TW 200932704A
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Description
200932704 九、發明說明: 【發明所屬之技術領域】 本發明係關於用於發光裝置之冷光材料,尤其係LED。 【先前技術】 破光體廣為人知,其包含矽酸鹽、磷酸鹽(例如磷灰石) . 及鋁酸鹽作為主體材料,添加過渡金屬或稀土金屬作為活 . 化材料至該等主體材料。特別隨著近年來藍光LED投入應 用,正積極進行與此類磷光體材料組合來利用此類藍光 © led的白光光源之研發。伴隨陶瓷冷光材料的出現,藍光 led也可幾乎完全地轉換成綠色及紅色。 尤其,基於所謂”SiAlON”系統的冷光材料由於其較佳光 學特徵而正成為此領域内的關注焦點。 然而,仍不斷需要可用於廣泛應用範圍内並尤其允許製 把具有最佳發光效率與演色性之磷光體暖白光pcLED的冷 光材料。 【發明内容】 本發明之一目的係提供一種發光裝置,#包含一冷光材 料,該冷光材料具有改良光學特徵以及一較佳可生產性及 穩定性。 • 此目的係藉由依據本發明之請求項1之一發光裝置來實 現。據此,提供一種發光裝置,尤其為LED,該發光裝置 匕3至'第—冷光材料,其發射一第一波長;及至少一 陶究轉換器材料,其至少部分地吸收該第一波長並隨後發 射-第二波長之光,該第二波長係大於該第一波長,該陶 136524.doc 200932704 瓷轉換器材料具有一 20。散射強度SI(20)與一 40。散射強度 SI(40) ’ SI(20)/SI(40) >1.5。 術語"Y。散射強度SI (γ)”係定義如下: 拋光一 100 μπι晶圓至光學品質(Ra<20 nm)。在該陶瓷轉 換器材料上的法線入射(==垂直於該晶圓)下發射一波長入的 • 單色光,在可見光譜之一區域内選取λ,其中吸收係數&係 . <30 cm-1。 在〇°角(=垂直於該晶圓)下測量的散射強度(=在一散射角 ® 的透射光)為100%(亦參考圖3)。接著在Y。角下測量Y。散射 強度SI(Y)。 在本發明之意義上的術語"陶瓷轉換器材料"尤其意指及/ 或包括一晶體或多晶壓實材料或複合材料,其具有一控制 數量的細孔或無細孔。 在本發明之意義上的術語"多晶材料"尤其意指及/或包括 具有主要組分之大於90百分比之一體積密度的一材料該 ❹ 主要組成由超過80百分比的單晶域所組成,每一域直徑大 於0.5 pm,且該材料可能具有不同的結晶定向。該等^晶 域可藉由非晶或玻璃材料或藉由額外晶體組分加以連接。 ' 已發現依據本發明之轉換器材料,其對於許多應 用具有下列優點之至少一或多者: 所發現的光學散射增強該裝置之轉換效率,因為散射可 能引起吸收損失。 所發現的光學散射增強轉換光與透射未轉換光之混合並 提供一較高封裝效率。 136524.doc 200932704 較佳的係,該陶瓷轉換器材料具有一 20。散射強度SI(20) 與一 4〇。散射強度 SI(40),SI(20)/SI(40)>1.6,較佳的係 SI(20)/SI(40)>1.8。 依據本發明之一較佳具體實施例,該陶瓷轉換器材料具 有一 30。散射強度SI(30)與一 60。散射強度SI(60), SI(30)/SI(60)>1.9。此更進一步增加用於本發明内許多應 • 用之轉換效率。 較佳的係,該陶瓷轉換器材料具有一散射強度比
IP SI(3 0)/SI(60) >2.5,較佳的係 SI(30)/SI(60) >2.9。 依據本發明之一較佳具體實施例,該陶瓷轉換器材料顯 示其構成微晶粒之一較佳定向,其係定義為其紋理。 為了偵測一優先定向,可應用X射線繞射技術。不具有 優先定向的陶瓷展現其相對峰値強度與針對對應材料所計 算的該等者相同的X射線繞射圖案。計算X射線圖案要求 瞭解材料的晶體結構,但不一定需要關於晶體形態的資 _ 訊。與理論圖案相比,紋理化陶瓷之X射線繞射圖案顯示 峰值強度的明顯偏差,即一些反射顯示增強的強度而其他 則可能展現甚至低於偵測限制的強度。由其米勒指數 (Miller indice)特徵化的該等反射顯示增加或減少的強度一 • 般取決於測量幾何學(即相對於X射線束之陶瓷樣本對 齊)、該形態以及在樣本内該等顆粒之定向。 較佳的係’該陶瓷轉換器材料顯示其構成微晶粒之一較 佳疋向,使付Intpeak A :Intpeak B>3,較佳的係>5 ,更佳的係 Η且最佳的係29,其中Intpeak a :lntpeak B係定義如下: 136524.doc 200932704 對於一般成分Sr〗-x-yMxEuySi2〇2N2的化合物,M=Ca、 Ba、Mg或其混合物,該等化合物係與主體化合物 SrSi202N2同形,intpeak A係由(〇 2 〇)反射之強度(以一方式 選取結晶設定使得(〇 k 0)晶格平面平行於晶體結構内的 [ShC^N2]2·層)或藉由(0 2 〇)與(1 2 〇)反射之強度之和(若該 等峰值在XRD粉末圖案中不充分分離以致無法決定(〇 2 〇) • 反射之強度)來給出,而IntPeak b係藉由(2 2 0)反射之強度 鲁 或藉由(2 2 0)與(2 -1 〇)反射之強度之和(若該等峰值在 XRD粉末圖案中不充分分離以致無法決定(2 2 0)反射之強 度)來給出。 依據本發明之一較佳具體實施例,該陶瓷轉換器材料基 本上係由具有一 25 μηι之dso的顆粒來製成。已顯示此在廣 泛應用範圍内進一步減少散射。 在本發明之背景下的術語”基本上"尤其意指>75 %,較 佳的係> 80 %且最佳的係> 9〇 %的材料具有所需成分及/或 ⑩ 結構。 在本發明之意義上的術語"Ιο"係用於平均顆粒大小的— 測量且定義如下:在對應樣本内微粒(例如顆粒)數目之 5〇°/°的大小等於或小於給定dso值。術語"微粒大小"尤其表 . 不一球體之直徑,該球體的體積與在具有一任意形狀之考 量之下之微粒之體積相同。 較佳的係’該陶瓷轉換器材料基本上係由具有一y pm 之dSG的顆粒來製成。 依據本發明之一較佳具體實施例,該材料基本上具有成分 136524.doc 200932704
Sr1.y.zMySi2〇2N2:Euz 其中M係選自包含Ca、Ba、Mg及其混合物之群組中, 且y係20至<1 ’而z係2 0.0001至切.5 出於下列原因,已顯不此·一材料有利地用於廣泛應用範 圍: 與先前技術的材料相比’該材料之穩定性通常得到改 良。該材料通常具有一極高熱(尤其光熱)穩定性。 此材料之光譜通常相當銳利,從而允許使用於本發明内 ® 料多應用中。 依據本發明之一較佳具體實施例,在一光功率強度1〇 W/cm2與一平均光子能量2.75 eV下在2〇〇χ:下持續曝光該 陶瓷轉換器材料達1000小時之後該陶瓷轉換器材料之光熱 穩定性為初始強度之之8〇%至si 1 〇〇/〇。 在本發明之意義上的術語"光熱穩定性"尤其意指及/或包 括在同時施加熱及高強度激發下冷光強度之保存,即一 〇 1〇0%的光熱穩定性指示該材料實際上不受同時曝露於輻 射及熱的影響。 ' 依據本發明之-較佳具體實施例,該陶㈣換器材料之 光熱穩定性在一光功率強度10 w/em2與一平均光子能量 . 2.75 eV下在200t下持續曝光該陶竟轉換器材料達_〇小 時之後為>82.5%至幻05%,較佳的係乏85%至幻〇〇%。 、依據本發明之—較佳具體實施例,該陶£轉換器材料之 導熱性為之1 W rn-iiC1至s 20 W n^K·1。 依據本發明之一具體實施例’該陶瓷轉換器材料顯示對 136524.doc 200932704 於在從2 550 nm至乞1000 nm之波長範圍内的光在空氣法線 入射下210 %至<85 %的一透明度。 較佳的係,在空氣法線入射下的透明度對於在從^55〇 nm至S 1〇〇〇 nm之波長範圍内的光為22〇 %至$ 80 %,對於 在從2550 nm至S1 〇〇〇 nm之波長範圍内的光更佳的係^30% 至<75°/。且最佳的係>4〇%至<70%。 ' 在本發明之意義上的術語”透明度"尤其意指 210%,較佳的係220%,更佳的係230%,最佳的係 240%且<85%的不被該材料吸收的一波長之入射光在空氣 法線入射(=垂直於表面)下透過樣本透射。此波長較佳的 係在2 550 nm且幺1〇〇〇 nm之範圍内。 依據本發明之一較佳具體實施例中,該陶瓷轉換器材料 具有理論密度之295%且S 101%的一密度。 依據本發明之一較佳具體實施例中,該陶瓷轉換器材料 具有理論密度之297%且g 1〇〇%的一密度。 Φ 依據本發明之所說明較佳具體實施例低於100%的密度 較佳的係藉由燒結該陶瓷至其中細孔仍存在於陶瓷基材内 的階段來加以獲得。更佳的係在298.0%且<99.8%範圍内 的雄、度’在陶瓷基材内的總細孔體積在^〇 2至之範圍 内。一較佳平均細孔直徑係在21〇〇〇至<5〇〇〇11111範圍内。 本發明更進一步關於一種產生一獨創材料之方法,其包 3單軸熱壓至少一先驅化合物,該壓製步驟係在 至幺1800°C的一溫度下執行。 7人%驚的係,已顯示藉由如此操作,可對於許多應用 136524.doc 200932704 容易且有效地產生具有所需且獨創特徵的一材料。 較佳的係,在一之130〇1至<170(rc的溫度下執行該壓製 步驟。 令人吃驚的係,已發現’對於在本發明内的許多應用, 可藉由單軸熱壓來引發該多晶陶瓷轉換器材料之紋理。在 單軸熱壓期間,優先定向板狀陶瓷顆粒,其表面在單轴熱 壓方向上垂直。 依據本發明之一較佳具體實施例,該至少一先驅化合物 基本上係由顯示一 2 2:1縱橫比之晶粒所組成。 術語"縱橫比"尤其意指該等微粒顆粒之最長與最短尺寸 之比率。對於(例如)板狀及針狀微粒發現一較大縱橫比。 對於在本發明内的許多應用已顯示,藉由按如上所聲明 操作’可進一步增強本獨創方法所製造之陶瓷轉換器材料 之所需特徵’尤其可減低回到入射方向上的光散射。 較佳的係,至少一先驅化合物基本上具有一 2 3:1的縱橫 比’更佳的係之4:1。 依據本發明之一較佳具體實施例,至少一先驅化合物基 本上係由具有一>5〇〇 nm直徑之板及/或薄片來製成。 對於許多應用,已顯示還促進製程並降低所產生陶瓷轉 換器材料之散射。 較佳的係’至少一先驅化合物基本上由具有一 WOO ’較佳的係u μΐΏ之直徑之板及/或薄片來製成。 依據本發明之一較佳具體實施例,該壓製步驟係在一 MO MPa之壓力下執行。 136524.doc -12- 200932704 包含依據本發明之一陶瓷轉換器材料之一發光裝置以及 使用本方法所產生之一陶瓷轉換器材料可用於各式各樣系 統及/或應用,諸如下列之一或多者: 辦公室照明系統、 家庭應用系統、 商店照明系統、 住宅照明系統、 重點照明系統、 聚光照明系統、 劇院照明系統、 光纖應用系統、 投影系統、 自我照明顯示系統、 像素化顯示系統、 分段顯示系統、 警告標魏系統、 醫學照明應用系統、 指示燈標誌系統、以及 裝飾照明系'統、 可攜式系統、 汽車應用、 溫室照明系統。 前述組件以及所聲明組件及在所說明具體實施例中欲依 據本發明使用之組件在其大小、形狀、材料選擇及技術方 136524.doc 13 200932704 面不受任何特殊例外影響,使得可無限制地應用在所屬領 域内習知的選擇準則。 【實施方式】 從範例I之下列詳細說明將會更清楚地明白本發明,該 範例僅以一解說性方式作為一獨創陶瓷轉換器材料之一範 例。獨創範例I與比較範例I兩者均參考SrSi2〇2N2:Eu陶 瓷。
範例I 標稱化學成分Sr〇,98EuQ.()2Si2〇2N2之一先驅物粉末係藉由 碾磨混合Eu摻雜正矽酸锶(SrQ.98EuQ Q2)2Si〇4與氮化矽,在 N2/H2大乾内在1400C下燒製該混合物,並最後礙磨並筛 選原始產物來加以合成。 將大約4 g先驅物粉末填裝入一石墨壓製工具内, 預先壓實,且最後在一氮大氣内在15〇(rc&7〇 Mpa下單 軸熱壓達5小時。 切割、研磨並拋光所得陶瓷體至1〇〇 μιη的一最終厚度。 比較範例1(傳統燒結) 標稱化學成分SrowEuo.^ShC^N2之一先驅物粉末係藉由 在惰性氣體大氣内碾磨混合Eu摻雜正矽酸鳃 (Sro.wEuo.QASiO4與氮化矽,在乂⑴2大氣内在12〇(Γ(:下燒 製該混合物,並最後碾磨並篩選原始產物來加以合成。 該粉末係單軸並均衡冷壓且所得碟狀小球在一氮大氣内 在環境壓力下在155(TC下燒結達5小時。 研磨並拋光所得陶瓷體至100 ^爪的一最終厚度。 136524.doc •14- 200932704 圖1及2分別顯示獨創範例j與比較範例丨之XRD圖案。該 等XRD圖案係對於0=〇。使X射線束垂直於板法線定位來獲 得,板法線係(a)平行於範例j之單軸熱壓方向且(b)平行於 比較範例I之單軸冷壓方向。 圖3顯不依據獨創範例丨(粗線)與比較範例〗(虛線)針對丨〇〇 μηι厚度的晶圓對於一法線入射66〇 nm雷射束透射光之正 規化角散射強度分佈。該等晶圓之表面係拋光至光學品質 (Ra<20 nm)。因此光散射僅由於在該等晶圓内的散射事件 而引起。 可清楚看出,該獨創材料之散射清楚地不同於該比較範 例之散射。即,20。散射強度81(20)係4〇。散射強度SI(4〇)的 >2倍,而30。散射強度SI(30)係6〇。散射強度81(6〇)的>3倍, 而在該比較範例中,該些比率要小得多。 圖4顯示在獨創範例〗(粗線)與比較範例〖(虛線)之一藍光 LED上的發射光譜。由於出色散射特徵,該獨創範例之發 射率特性優於該比較範例之該等者。 圖5顯示在研磨及拋光之後依據範例j之陶瓷轉換器材料 之結構之一光學顯微圖。可看見’該陶瓷轉換器材料包含 許多較大顆粒及/或板,其中一些者具有5〇 μηι或以上的一 直徑。平均dw為大約4 μηι。未束缚於任何理論,本發明 者相信此非正統結構至少部分地引起本發明之材料之獨創 且所需優點。 在下文中,論述依據範例I之材料之結構以及用於測量 依據本發明之較佳應用之材料之蚊理的一般構造。 136524.doc •15- 200932704 纟該陶錢#器材料内部的構成微晶粒之較佳定向可藉 由X射線繞射來加以量化。 圖6顯示用於測量該陶瓷轉換器材料之紋理的一極示意 性實驗構造。在陶究樣本3中,指示兩個板狀陶竟微晶、!及 2 ’其晶格平面分職+冑直或(如高度紋理化陶竟所需)垂 直於板法線。欲檢查的陶瓷板3經受一入射X射線束6。繞 射束5係使用一X射線偵測器7來加以測量。θ為繞射角。該 陶瓷板之表面法線與在單軸熱壓期間的壓製方向—致,該 壓製方向由箭頭4來加以指示。 量化決定結晶紋理可藉由在一較佳定向反射峰值上組合 = Θ-2Θ掃描與一θ掃描來進行,如非專利文獻1^ D, %udin 等人、J. Mater. Res. 13 (1998) 291〇中所說明其係以引 用的方式完全併入本文内。 在以一方式實施X射線繞射實驗,使得對於θ=〇。垂直於 該陶究之單軸熱壓方向來定位入射乂射線光束的情況下,、 〇 針對垂直於該壓製方向的該等板狀微晶粒之倒易晶格平面 優先觀察到引起X射線輻射之繞射極限的建設性干涉。若 在布喇格-布倫塔諾(Bragg-Brentano)幾何學中一χ射線偵 . 測器之一對稱掃描係以一方式實施,使得對於β=9〇。 ' 該谓測器係平行於該陶瓷樣本之平面而定位,則較強地增 強源自垂直或近乎垂直於該壓製方向而定向之晶格平面處 繞射的反射,同時較強地減弱源自平行或近乎平行於該壓 製方向定向之晶格平面處繞射的反射。 進一步檢查範例I之材料給出下列結果: 136524.doc •16· 200932704 依據晶體結構決定結果,例如如O. Oeckler、F.
Stadler、T. Rosenthal、W. Schnick,Solid State Sci., 2007, 9(2),205-212中所說明’其以引用方式完全併入本文内, SrSizChN2係藉由具有末端氧離子之邊角共享[Si〇N3]四面 體片來加以構造’該等末端氧離子形成Sr或摻雜離子之 配位環境’該等Sr或摻雜離子位於該等[8丨2〇以2]片之 間。因此’可針對該SrSizOzN2先驅化合物觀察到一板狀 形態。
❷ 對於由板狀顆粒所組成之熱壓SrSi2〇2N2:Eu型陶究,在 範例章節中解釋細節。在下列章節中解釋用於碟狀陶瓷樣 本的--般適當測量幾何學(如在下面所說明之所有測量 中所應用)。 關於該結構,(0 k 0)倒易晶格平面係平行於該等 [ShC^N2]片而定向並因此也垂直於該等SrSi2〇2N2板法線。 對於具有一明顯優先定向之樣本,與其他反射相比,具有 米勒指數(0 k 0)的反射尤其顧示增加的強度。81>812〇2^之 (〇 1 0)反射係在2Θ〜12,6。下發現,而(〇 2 〇)峰值在2θ〜 25·4。下與U 2 _值重叠(兩個峰值之和將會稱為峰值 Α)。具有最大理論強度(2 2 0)峰值的反射係在2θ〜318。下 發現並與(2 -1 0)反射重疊(兩個峰值之和將會稱為峰值 Β)。 比較熱壓(獨創範例I)與傳統燒結(比較範例^材料之該 XRD圖案,顯然熱壓導致具有該等微晶之—較強優先定 的陶瓷。甚至在2Θ〜12.6。下的峰值顯示高於峰值Β的2 136524.doc -17- 200932704 度。 依據比較範例I之陶瓷不會展現一明顯優先定向並顯示 強度比Intpeak A : Intpeak B<1(亦參見圖7),而一優先定向之 存在係由Intpeak A : Intpeak B > 1來加以指示。 具有一較強優先定向之樣本應展現Intpeak a : IntpeakB >3 的一比率,較佳的係>5。對於以上所說明之熱壓陶瓷(獨 創範例I) ’觀察到Intpeak a : Intpeak B~9.4的一強度比(基於
❹ 在背景校正之後的峰值高度)’顯示可觀察到一極強優先 定向。 在以上詳細說明之具體實施例中的元件及特徵之特定組 合僅為範例性;還明確預期使用此專利案及以引用形式併 入之該等專利案/申請案中的其他教導來互換及代替該些 教導。習知此項技術者應認識到,熟習此項技術者可想到 本文所說明内容之變更、修改及其他實施方案而不脫離所 聲明之本發明之精神及料。據此,前述僅藉由範例方式 而並非意在限制。本發明之範疇係定義於隨附申請專利範 圍及其等效内容内。此外’於說明書與中請專利範圍中使 用之參考符號不限制所聲明的本發明之範疇。 【圖式簡單說明】 在該等附屬項、該等圖式及該等各別圖式及範例之以上 說明中已揭示本發明之目的之額外細節'特徵、特性及優 點’該等㈣及範例僅以-範例性方式顯㈣於依據本發 明之-發光裝置内的-材料之數個具體實施例及範例。 圖!顯示用於依據本發明之範船之―材料之—細圖案 136524.doc -18- 200932704 圖2顯示用於依據比較範例I之一材料之一 xRD圖案 圖3顯示獨創範例I及比較範例I之散射強度之一角度解 析測量 圖4顯示獨創範例I及比較範例I之一發射光譜 圖5顯示在研磨及拋光之後依據範例I之陶免轉換器 之結構之一光學顯微圖,以及 盗材料 極示意 圖6顯示用於測量該陶瓷轉換器材料之紋理的 性實驗構造。
【主要元件符號說明】 1 板狀陶瓷微晶 2 板狀陶瓷微晶 3 陶瓷板 4 箭頭 5 繞射束 6 入射X射線束 7 X射線偵測器 136524.doc • 19_
Claims (1)
- 200932704 十、申請專利範圍: 1. 一種用於發光裝置之陶瓷轉換器材料,該發光裝置尤其 係LED,該陶瓷轉換器材料具有一 2〇。散射強度SI(2〇)與 一 4〇°散射強度SI(40),SI(2〇)/SI(40) y.6。 2. 如請求項丨之陶瓷轉換器材料,其具有一 3〇。散射強度 SI(3〇)與一 60°散射強度叫6〇),SI(30)/SI(60) >1.9。 3. 如响求項1或2之陶瓷轉換器材料,其中該陶瓷轉換器材 料顯示其構成微晶粒之一較佳定向。 4·如請求項1或2之陶瓷轉換器材料,其中該材料基本上係 由具有一>5 μπι之d5〇的顆粒所製成。 5·如請求項丨或2之陶瓷轉換器材料,其中該材料基本上具 有成分 Sr】 _y.zMy S i2〇2N2:Euz 其中Μ係選自包含Ca、Ba、Mg&其混合物之群組中, 且y係>〇至si,而2係》〇.0001至5〇 5。 6. Ο 一種產生如請求項丨或2之材料之方法,其包含單轴熱壓 至少—先驅化合物,該壓製步驟係在一 °c之溫度下執行。 如凊求項6之方法,其中該至少—先驅化合物基本上具 有一 2 2:1的縱橫比。 8. 如請求項6之方法,纟中該至少一先驅化合物基本上係 由具有一2500 nm直徑之板及/或片所製成。 9. 如請求項6之方法,其中該壓製步驟係在Μρ&的一壓 力下執行。 136524.doc 200932704 1 0. —種包含如請求項1或2之陶瓷轉換器材料之系統,該系 統係用於下列應用之一或多者: 辦公室照明系統、 家庭應用系統、 商店照明系統、 住宅照明系統、 重點照明系統、 聚光照明系統、 劇院照明系統、 光纖應用系統、 投影系統、 自我照明顯示系統、 像素化顯示系統、 分段顯示系統、 警告標誌系統、 醫學照明應用系統、 指示燈標誌系統、以及 裝飾照明系統、 可攜式系統、 汽車應用、 溫室照明系統。 136524.doc
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