TW200811078A - YAG-based ceramic garnet material comprising at least one multi-site element - Google Patents
YAG-based ceramic garnet material comprising at least one multi-site element Download PDFInfo
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Description
200811078 九、發明說明: 【發明所屬之技術領域】 本發明係關於陶瓷石榴石材料,尤其彼等用於發光裝置 (尤其LED)中之材料。 【先前技術】 ^ 當今之發光裝置(尤其LED)在很大程度上包括摻雜
Ce(III)之以YAG為主之材料,此乃因YAG具有優異的材料 性質。在這方面,可參考(例如)美國專利第2003 /0078156 ^ A1號,其以引用的方式倂入本文中。 然而,尤其對於使用呈陶瓷及/或結晶型式之摻雜 Ce(III)之以YAG為主的材料的發光裝置,已顯示製造彼等 YAG-陶瓷通常很困難,尤其因為材料組合物須嚴格保持 有序以避免於YAG中存在次要相,尤其係YAP(鈣鈦礦) 相。 可自(例如)J.S· Abell,I.R· Harris,B. Cockayne及 B. Lent, J· Mater· Sci,9 (1974) 527中瞭解到在氧化鋁-氧化釔系統 _ 中相之關係。在固態下,若偏離理想的化學計量比,則 y3ai5o12(yag)結晶為線性化合物,而氧化鋁即ai2o3或 • YAP即YA103結晶為形成於多晶石榴石YAG材料中之鄰近 自 Μ· M. Kuklja及 R. Pandey,J. Am. Ceram. Soc· 82 (1999) 2881瞭解到,固有的錯置無序係容納自理想化學計 量比偏離(即在Y3A15012(YAG)石榴石化合物中,Y203或 Α1203過量)之主要機制。該錯置無序可導致圍繞線性化合 122713.doc 200811078 物化學計量纟卜$ g 4 θ 早相存在區域擴展,尤其對於顯示氧化釔 過量之組合物而^ 物而口,因為在八面體鋁位點上納入釔比在十 二面體釔位點納入鋁在能量上更有利。 然而,尤其在工業生產摻雜Ce(III)之yag-陶瓷範圍 内,常由於稱量誤差或生產過程中之波動而不能保持完全 正確之組成。 【發明内容】
本發明之一目的係提供一種具有改進'1·生質之以YAG為主 之陶£石權石材料’其尤其使得多種應用具有更大生產公
〜目的由本發明請求項i之以Yag4r陶曼石榴石材 料及/或本發明之請求項9之方法而達成。因此,本發明提 供-種以YAG為主之陶瓷石榴石材料,#包括可在該以 YAG為主之陶瓷石榴石材料中佔據八面體及/或十二面體 配位陽離子晶格點之至少一個多位成份。 吾人已驚奇地發現,在本發明内之大部分應用中,藉由 使用此一以YAG為主之陶瓷石榴石材料可極大地提高生產 公差而不會影響該以YAG為主之陶瓷之性質。在一2應用 中,該以YAG為主之陶瓷石榴石材料之性質甚至可得:改 進。雖然尚未確定為某一理論,但本發明之發明者相信至 少一個多位成份為YAG材料中之其他離子(尤其係丫及/或 A1離子)充當佔位者之功能有助於擴大該yag材料之處理 窗口。 【實施方式】 122713.doc 200811078 術語”以YAG為主,,尤其意指及/或包含一種包括作為主要 組份之Μΐ3Μΐί2(ΜίπΧ4)3材料,其中M1選自由Mg、ca、Y、
Na、Sr、Gd、La、Ce、Pr、Nd、Sm、Eu、Dy、Tb、
Ho ' Er、Tm、Yb、Lu或其混合物組成之群,mii選自由 A卜 Ga、Mg、Zn、γ、Ge、Sc、Zr、丁i、Hf、Lu 或其混 合物組成之群,Min選自由a卜si、b、Ge、Ga、v、As、 Zn或其混合物組成之群,χ選自由〇、s、n、f、^、h、 I =〇H及其混合物組成之群,且構造為mII\八面體及 ΜΠΙχ4四面體’其中任-八面體藉由共享頂點之四面體與 八個其他八面體相接合。任一四面體與四個八面體共享其 頂點’因此該構架之組成為(Μηχ3)2(Μ„Ιχ2)3。較大離子 Μ1佔據該構架間隙中之8配位體位置(十二面體的),由此 產生終組成 Ml3Mll2(MlI%)3。 術浯主要組份"尤其意指該材料由295%、較佳>97%且 最佳頻之以YAG為主之陶究石權石材料組成,-不包括 至少-個多位成份及可能添加之摻雜材料。 應注意,在本發明之一 & ~ ί田石材料中,M1與μιπ位置 至少部分地由相同元素原子佔據。 ^ 應注意,該以YAG為主之陶竟材+ ’克材枓可摻雜選自由Lu、
Pr、Sm、Tb、Dy、Ho、E” Tm、γ ,, b、La、Ce或其混合物 組成之群之物質。 σ π 本發明中之術語"以ΥΑ 立托、 為主之陶瓷石榴石材料,,尤其還 思才日及/或包括上述材# I 八 加兩^人物^ 製作陶:光過程中添加之添 加剤之混合物。該等添加劑入 疋王或α卩分地納入最終材料 122713.doc 200811078 中,因此最終材料亦可係數種不同化學物之組合物且尤其 包括彼等為業内所知用作溶劑之物質。適宜之熔劑包括驗 土或鹼金屬氧化物及鹵化物、硼酸鹽、Si02及諸如此類。 本發明中術語”陶瓷材料”尤其意指及/或包括帶有受控數 量之小孔或無孔的晶體或多晶緻密材料或複合材料。 本發明之”多晶材料”尤其意指及/或包括一種體積密度大 於主要組份(其由超過80%之單晶域組成,且任一域之直徑 皆大於0.5微米)之90%的材料,並且可具有不同之結晶定 向。該等單晶域可由非晶形或玻璃狀物質或由額外的晶體 組份相連接。 根據本發明之一較佳實施例,該至少一個多位成份之六 重配位離子半徑係WO pm至£104 pm及/或該至少一個多位 成份之八重配位離子半徑係>85 pm至$116 pm。此已於本 發明之許多應用中證明係最有效的。 應注意幾個不同多位成份存在時,尤其較佳的係所有多 位成份具有上述之離子半徑;此作必要修正後適用於本發 明中之所有其他實施例。 根據本發明之—較佳實施例,該至少—個多位成份之六 重配位離子半徑係>75 Pm至侧Pm,更佳⑽pm至養 pm 〇 根據本發明之—較佳實施例,該至少—個多位成份之八 重配位離子半控係’ Pm5^114 Pm’更佳292 pm至$112 pm 〇 據本I明之一實施例’該至少一個多位成份相對於以 122713.doc 200811078 YAG為主之石權石結構之濃度係· 5莫耳%至<5莫耳%。 已顯示此係在本發明之多種應用内可獲得最寬處理窗而不 有損YAG材料之性質的最佳適宜範圍。 根據本發明之一實施例,該至少一個多位成份相對於單 元式中陽離子總和之濃度係20.1原子%至20.7原子%,較佳 地20.2原子%至$〇.4原子%。 根據本發明之一實施例,在該陶瓷石梅石材料中,(Y、
Lu、Gd、Pr、Sm、Tb、Dy、Ho、Er、Tm、Yb、La、
Ce、Ca)之總和與(A卜 B、Si、Mg、Ge、Zr、Hf、Ga、 Sc)之總和之商數係a.590至S0.610。藉此,對於多種應 用,可獲得最適宜YAG陶瓷材料。在該陶瓷石榴石材料 中,較佳地(Y、Lu、Gd、Pr、Sm、Tb、Dy、Ho、&、
Tm、Yb、La、Ce、Ca)之總和與(A1、B、Si、Mg、Ge、
Zr、Hf)之總和之商數係20.593至$〇·6〇7,更佳係20.595至 S0.605。 根據本發明之一較佳實施例,在以YAG為主之陶曼石權 石材料中,該主要相與該(等)可能的次要相之比率係 210 : 1,較佳地>20 : 1且最佳24〇 : 1。 本發明之術語"次要相’’尤其意指及/或包括展示不同化學 組成及/或結晶結構之最終混合物之較少組份。 根據本發明之一車父佳實施例’該至少一個多位成份係選 自包括Se、Ga、Yb、Lu、Mg及其混合物之群。在實踐 中,已證實該等材料可用於許多應用中。 根據本發明之一較佳實施例,將該陶瓷材料於2〇〇〇c下 122713.doc -10- 200811078 暴露於10 W/cm2之光功率密度及2.75 eV之平均光子能量下 1000小時後,摻雜Ce(III)之以YAG為主之陶瓷石榴石材料 的光熱穩定性係280%至U 00%。 本發明中術語’’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發米強度之保守性,亦即100%之光 熱穩定性指材料實質上不受同時照射與加熱之影響。 根據本發明之一較佳實施例,將該陶瓷材料於200°c下 暴露於10 W/cm2之光功率密度及2.75 eV之平均光子能量下 1000小時後,摻雜Ce(III)之以YAG為主之陶瓷石榴石材料 的光熱穩定性係282.5%至$95%,較佳地285%至$97%。 根據本發明之一較佳實施例,該以YAG為主之陶瓷石榴 石材料之導熱率係2〇·〇7 W cn^K·1至$0.15 W cn^K·1。 根據本發明之一較佳實施例,摻雜Ce(III)之以YAG[PS1] 為主之陶瓷石榴石材料的量子產率係290%至$99%。 本發明之術語”量子產率"尤其意指及/或包括發射光子數 與吸收光子數之比例。 根據本發明之一較佳實施例,該以YAG為主之陶瓷石榴 石材料之光子產率係293%至$99%,較佳地仝95%至£98%。 根據本發明之一實施例,該以YAG為主之陶瓷石榴石材 料在空氣中對垂直入射之波長範圍在2550奈米至£1000奈 米之光線的透光率為210%至$85%。 較佳地,在空氣中對垂直入射之波長範圍在2550奈米至 $1000奈米之光線的透光率為220%至$80%,對波長範圍在 2550奈米至$1000奈米之光線,更佳地為230%至$75%且最 122713.doc -11 - 200811078 佳為>40%至<70%。 本發明之術語’’透光率"尤其意指對於空氣中之垂直入 射,210%、較佳地220%、更佳地仝30%、最佳240%且 $85%的一不能為材料所吸收的波長之入射光以任意角度 透射穿過樣品。該波長較佳係在範圍255〇奈米及$1000奈 米内。 根據本發明之一較佳實施例,該以YAG為主之陶瓷石榴 石材料之密度為化學劑量石榴石結構之理論密度的》95〇/〇 且 $101%。 根據本發明之一較佳實施例,該以YAg為主之陶瓷石榴 石材料之密度為理論密度之297%且^ 100%。 根據本發明所述之較佳實施例,低於1 〇〇Q/。之密度較佳 係藉由將陶兗燒結至陶瓷基質中仍存在小孔之程度而獲 得。最佳地’密度係在298 0%且£99 8%之範圍内,且陶究 基質中之總孔容積在2〇·2_$2%範圍内。一較佳之平均小孔 直徑係在2400-S1500奈米範圍内。 本發明進一步係關於一種生產本發明之以YAG為主之陶 瓷石榴石材料之方法,其包括燒結步驟。 本發明之術語"燒結步驟,,尤其意指前體粉末在熱作用(可 組合施用單軸或等靜壓力)下緻密化但不使被燒結材料主 要組份達到液態。 根據本發明之一較佳實施例,燒結步驟係無壓的,較佳 地係在還原或惰性氣氛中實施。 根據本發明之-較佳實施例,該方法進-步包括在燒結 122713.doc -12 - 200811078 前將陶瓷石榴石前體材料壓縮至其理論密度之>50%至 $70%,較佳地255%至S65%之步驟。在實際應用中,已顯 示此可改進用於本發明所闡述之大部分以YAG為主之陶究 石榴石材料之燒結步驟。 根據本發明之一較佳實施例’生產本發明之以YAG為主 之陶瓷石榴石材料之方法包括以下步驟: (a) 將用於以YAG為主之陶瓷石榴石材料之前體材料混合 (b) 視情況烘培該等前體材料,較佳在> 1300°C至 S1700 C溫度下,以移除揮發性物質(例如在使用碳酸 鹽情況下之C02)。 (°) 視情況粉碎並洗滌 (d) 第一壓製步驟,較佳地係一單軸壓製步驟,其使用 帶有期望形狀(例如,桿形或丸形)之模具之適宜的粉 末壓實工具,及/或一冷均壓壓製步驟,較佳在23〇〇〇 巴(bar)至$5000巴下。 (e) 燒結步驟,係在21500。(:至$2200。〇下於惰性、還原 性或輕微氧化氣氛中及21 〇_7毫巴至S104毫巴之壓力 下。 (0 視情況之熱壓步驟,較佳地係一熱均壓壓製步驟, 車乂 L在>30巴至$25〇〇巴且較佳地溫度為>15〇〇。〇至 S2000 C及/或一熱單軸壓製步驟,較佳在h〇〇巴至 ^2500巴且較佳溫度為21500°C至£2000。〇。 (g)視一况一後退火步驟,係在>1〇〇〇。〇至<1700°C下於 惰性氣氛或於含氧氣氣氛中。 122713.doc -13- 200811078 根據該方法,對大多數之期望材料組合物,該生產方法 已生產出用於本發明之最佳的以YAG為主之陶瓷石榴石材 料。 本發明亦係關於一種發光裝置,尤其一種包括本發明之 以YAG為主之陶瓷石權石材料之led。 本發明之以YAG為主之陶瓷石榴石材料、一種包括本發 明之以YAG為主之陶瓷石榴石材料之發光裝置及/或以本 發明方法生產之以YAG為主之陶瓷石榴石材料可用於多種 系統及/或應用中,其中包括以下之一或多種: - 辦公室照明系統 - 家用糸統 - 商場照明系統, - 家庭照明系統, - 重點照明系統, - 聚光照明系統, " 劇院照明糸統, - 光纖應用系統, • 投影系統, - 自發光顯示系統, - 像素化顯示系統, - 分段顯示系統, - 警報信號系統, - 醫療照明應用系統, 指示信號系統,及 122713.doc -14- 200811078 - 裝飾照明系統, - 便攜式系統, - 汽車應用 • 溫室照明系統, - 門窗材料及門窗應用 - 雷射(laser)應用系統,尤其用於具有 石榴石主晶格之多晶雷射材料 ' 發光裝置外殼,尤其用於HID燈 - 光學透鏡或高折射率元件 上述組件、及所主張組件及根據本發明用於所述實施例 中之組件在其尺寸、形狀、材料選擇及技術概念等方面無 任何特定例外,因此相關領域中習知之選擇標準可不受限 地施用。 本發明目的之更多細節、性質、特徵及優點揭示於隨附 申請專利範圍、附圖及下文對各圖及實例之闡釋中,該等 以示例形式展示了本發明之以YAG為主之陶瓷石榴石材料 的一些實施例及實例。
實例I至IV 結合僅僅舉例說明形式之實例1至IV可更好地理解本發 明,實例I至IV係本發明之以YAG為主之陶瓷石榴石材料 的四個實例。 该石權石材料以如下途徑製備: 百先’稱入合適量之 Y2〇3(99.99%,Rhodia)、Gd2〇3 (99.99%5 Rhodia) ^ Sc2〇3(99.9%) > Al203(99599%? Baikowski) 122713.doc -15- 200811078 及Ce〇2(>99%,Rhodi a)粉末並在添加1000 ppm石夕石作為水 解的四乙氧基矽烷下在異丙醇中以高密度氧化鋁研磨介質 實施研磨。隨後,將陶瓷漿液過篩以移除粗粒子,並在添 加以聚乙烯縮丁醛為主之黏結劑系統後進行乾燥。然後將 該粉末混合物造粒,且藉由冷等壓壓製形成陶瓷生坯。在 空氣氣氛中移除黏結劑後,在H2/N2(5%/95%)氣氛中於 1600-1750°C之溫度範圍内燒結該陶瓷生坯。機械加工 後,在空氣氣氛中於12〇0°C-1400°C下對該陶瓷部分實施後 退火。 表I展示四個本發明實例I至IV之材料組成: 表1 :實例I至IV之組成 本發明 實例 金屬比例 燒結後相對密度 I (Y0.9Gd0.1)2.994 Ce0.06 A14.96 Sc0.02 100.00% II (Y0.9Gd0.1)2.994 Ce0.06 A14.98 Sc0.02 99.89% III (Y0.9Gd0.1)2.994 CeG.06 A15.00 Sc0.02 99.96% IV (Y0.9Gd0.1)2.994 Ce0.06 A15.02 ScO.02 100.00% 多位陽離子Sc之數量選擇為化學計量石榴石組合物之單 元式中陽離子之總和之0.25%。
術語”相對密度”意指將兩個最大密度陶瓷(其具有相同密 度)任意設定為具有100%之相對密度。可發現所有陶瓷實 質上具有相同密度。比較實例I至IV 和本發明之實例一起,亦完全按上述方式製備四個比較 實例,僅不含至少一個多位成份(亦即,無Sc)。 122713.doc -16- 200811078 表II展示四個本發明實例I至IV之材料組成: 表II :陶瓷丫八0:〇6樣品之組成 組合物 實例 金屬比例 燒結後相對密度 I (Y0.9Gd0.1)2.994 Ce0.06 A14.96 100.00% II (Y0.9Gd0.1)2.994 Ce0.06 A14.98 98.92% III (Y0.9Gd0.1)2.994 Ce0.06 A15.00 99.34% IV (Y0.9Gd0.1)2.994 Ce0.06 A15.02 99.55% 此處術語"相對密度”亦意指將最大密度之陶瓷任意設定 為具有100%之相對密度。可看出密度偏差較表I中略大, 且因此可觀察到光學性質有大的不同,例如散射。 圖1至8展示本發明實例I至IV(分別為圖1至4)及比較實例 I至IV(分別為圖5至8)之微結構(SEM顯微照片)。 可發現所有本發明之實例均展示均勻結構且未發現次要 相,而在所有比較實例中均存在次要相。 應稍加注意,最佳比較實例係實例II,雖然在起始材料 混合物中A1含量稍低。由於以氧化鋁研磨時可發生一些小 磨損,因此會略微提高A1含量。 實例III及IV展示在陶瓷中充當散射中心之氧化鋁次要相 顆粒(掃描式電子顯微鏡圖像中係可見之黑色顆粒)。 然而,很明顯比較實例II係密度最小之陶瓷,乃因其存 在内部孔隙。已顯示在許多應用中,若不具有至少一個多 位成份,則組成精確之材料通常係最難燒結之材料,此極 可能係由於缺少充當燒結輔助物之共熔次要相。若添加至 122713.doc -17- 200811078 少一個多位成份,此可得以解決;所有本發明之實例均顯 示優良的燒結特性。 上文詳述實施例中成份及性質之具體組合僅係例示性; 本發明亦明確涵蓋該等教義與本文及以引用之方式倂入之 專利/申請案中之教義之間的互換及替代。熟習此項技術 - 者會認識到,一般技術者可想到本文所述方法之變化、改 進、及其他實施方式而不違背本發明所主張之主旨及範 _。因此’上文僅以實例方式闡述而並非意欲施加限制。 _ 本發明之範圍由以下申請專利範圍及其等效項界定。而 且,說明書及申請專利範圍中使用之參考符號並不限制所 主張之本發明之範圍。 【圖式簡單說明】 圖1展示本發明實例I之以YAG為主之陶瓷石榴石材料之 微結構。 圖2展示本發明實例II之以YAG為主之陶兗石權石材料 之微結構。 • 圖3展示本發明實例111之以YAG為主之陶瓷石權石材料 之微結構。 , 圖4展示本發明實例1V之以YAG為主之陶瓷石梅石材料 - 之微結構。 圖5展示比較實例I之YAG陶瓷石榴石材料之微龄構 圖6展示比較實例II之YAG陶瓷石榴石材料之微钟構 圖7展示比較實例III之YAG陶瓷石榴石材料之微結構 圖8展示比較實例IV之YAG陶瓷石榴石材料之微結構 122713.doc -18-
Claims (1)
- 200811078 十、申請專利範圍: 其包括至少一個可 内之八面體及/或十 1. 一種以YAG為主之陶瓷石榴石材料, 佔據該以YAG為主之陶甍石權石材料 二面體位點之多位成份。 2. 如請求項1之以YAG為主之陶瓷石榴石材料,其中,納 入該掺雜Ce⑽之以YAG為主之㈣石權石材料中的在 六重配位陽離子晶格點上之該至少—個多位成份之離子 半徑係270 pm至$ 104 pm。3. 如請求項丨或2之以YAG為主之陶兗石榴石材料,其中該 至少-個多位成份之濃度係該石權石結構之陽離子總和 之2〇·1原子%至£〇.7原子%。 4. 如請求.項1至3中任一項之以YAG為主之陶究石權石材 料,其中在該陶瓷石榴石材料中,(γ、Lu、Gd、ρι>、 Sm'Tb'Dy'H()'Er、Tm、”、。、。、^之總和 與(Sc、Ga、A卜 B、Mg、Si、Ge、Zr、Hf)之總和之商 數係2〇.590至$〇.61〇。 5.如請求項1至4中任一項之以YAG為主之陶瓷石榴石材 料,其中該以YAG為主之陶瓷石榴石材料中之該主要相 與該(等)可能的次要相之比例係Si 〇:1。 6·如請求項1至5中任一項之以YAG為主之陶瓷石榴石材 料’其中該至少一種多位成份係選自包括Sc、Ga、Yb、 Lu、Mg及其混合物之群。 7·如請求項1至6中任一項之以YAG為主之陶瓷石榴石材 料’其中在將該陶瓷材料於20(rCT暴露於10 w/cm2之光 122713.doc 200811078 功率密度及2.75 eV之平均光子能量η·小時後,該以 YAG為主之陶瓷石榴石材料之光熱穩定性係y〇%至 £100%。 一種發光裝置,尤其係一種LED,其包括如請求項丨至7 中任一項之以YAG為主之陶瓷石榴石材料。 9. 10.一種生產如請求項1至7中任一項之用於發光裝置之以 YAG為主之陶£石權石材料之方法,其包括燒結步驟。 種系統,其包括如請求項1至7中任一項之以YAG為主 =陶究石權石材料、如請求項8之發光裝置及/或根據如 明求項9之方法生產之以yag為主之陶瓷石 該系統侈田认丨夕 田材枓, 1糸用於一或多種以下應用中·· _ 辦公室照明系統 豕用糸統 ~ 商場照明系統, ^ _ 家庭照明系統, ' - 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, 、 自發光顯示系統, ' 像素化顯示系統, 分段顯示系統, ' 警報信號系統, 122713.doc 200811078 醫療照明應用系統, 指示信號系統,及 裝飾照明系統, 便攜式系統, 汽車應用 溫室照明系統, 門窗材料及門窗應用 雷射應用系統,尤其用於具有石榴石 主晶格之多晶雷射材料 發光裝置外殼,尤其用於HID燈 光學透鏡或高折射率元件。122713.doc 200811078 七、指定代表圖: (一) 本案指定代表圖為:第(1)圖。 (二) 本代表圖之元件符號簡單說明: (無元件符號說明) 八、本案若有化學式時,請揭示最能顯示發明特徵的化學式: (無) 122713.doc
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