TW200848494A - Red emitting luminescent materials - Google Patents

Red emitting luminescent materials Download PDF

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Publication number
TW200848494A
TW200848494A TW097104326A TW97104326A TW200848494A TW 200848494 A TW200848494 A TW 200848494A TW 097104326 A TW097104326 A TW 097104326A TW 97104326 A TW97104326 A TW 97104326A TW 200848494 A TW200848494 A TW 200848494A
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Taiwan
Prior art keywords
lighting systems
systems
present
materials
illuminating device
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TW097104326A
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English (en)
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Peter J Schmidt
Florian Stadler
Wolfgang Schnick
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Koninkl Philips Electronics Nv
Philips Lumileds Lighting Co
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Publication of TW200848494A publication Critical patent/TW200848494A/zh

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Description

200848494 九、發明說明： 【發明所屬之技術領域】 本發明係關於發光裝置之新賴發光材料，尤其係關於 L E D之新賴發光材料領域。 【先前技術】 包含石夕酸鹽、雄酸鹽（例如磷灰石）及銘酸鹽作為主體材 料且具有作為活化材料添加至該等主體材料中之過渡金屬 或稀土金屬的磷光體已廣泛為吾人所知。詳言之，隨著近 1 年來UVA至藍色發光LED變得實用，現正積極探求使用該 UVA至藍色發光LED以及該等磷光體材料來研發白色光 源。 尤其關注白色發光材料且已提出數種材料（例如 US6522065 B1)。所主張之磷光體為 Ca2NaMg2V3〇i2:Eu 組 成之釩酸鹽石榴石材料，其展示來自釩酸鹽主體晶格群之 黃光發射及Ειι (III)摻雜物之紅線發射。 然而，仍持續需要發光材料，尤其白色發光材料，其可 用於各種應用且尤其允許製造具有最佳發光效率及色彩再 現之麟光體暖白光pCLED。 【發明内容】 本發明之目標為提供可用於各種應用且尤其允許製造具 有最佳發光效率及色彩再現之麟光體暖白光pcLED之材 料。 如本發明請求項1之材料解決了此目標。因此，提供材 料 M'.xMHxSQNwxOh， 128440.doc 200848494 由广Μ1係選自二價鹼土金屬、銪或其混合物之群， Μ係選自三價稀土金屬、釔、鑭、銃或其混合物之 群， 且 x>0 JL <1。 應’主思，術語，，尤其及/或另外意謂 及/或包括基本上具有此組成之任何材料。 ^ 基本上尤其意謂295重量％，較佳地a?重量％且 最佳39重量％。然而，在一些應用中，在總組成中亦可存 在；艮里添加知]此專添加劑特別包括諸如此項技術中稱為 溶劑之物質。合適之炼劑包括驗土金屬或驗金屬氧化物及 氟化物、Si〇2及其類似物及其混合物。 該材料已展示在本發明之各種應用中具有以下優勢中之 至少一者： -將該材料用作發光材料可構建白色發光led，其展示改 良士光特徵尤其熱穩定性及良好Ra值，此等Ra值在各 種應用中290，有時甚至>94或>96。 -將該材料用作發光材料，已發現在本發明之各種應用中 LED之顏色溫度基本上與所用電流及咖温度無關。 4材料在本發明之各種應用巾均為穩定的且在曝露於高 溫時尤其不展示或僅展示較少的發光降級。 不受任何理論束缚，本發明者咸信本發明材料之改良特 性至少部分係由該材料之結構引起的。 咸信本發明材料基本上具有立方結構，其包含共享⑴ (Ν’ 〇)4四面體之所有棱，由此產生具有兩個結晶學不同^ 128440.doc 200848494 位點之延伸三維網路。 對單位晶胞中本發明材料之各種結構而言，存在可經不 同大小及價數之陽離子填充的4個不同金屬位置（M1、 M2、M3及M4)(亦參看隨後描述之圖〗至圖4)。 在M1包含Ba及/或Ca之狀況下，對本發明材料之各種結 構而吕’ Ml位點僅由Ba(最大位點）佔據，m2及M3由Ba及 Ca佔據，且M4僅由Ca(最小位點）佔據。 f 咸信Eu2+可摻入所有可用晶格位點上，而Ce3+或Eu3 +最 可能摻入至M3位點上。因為在同型化合物 BUiiuYbShNH中，三價陽離子Yb3+僅嵌入至以3位點 上’所以可作此假定。 總而言之，對於本發明材料之各種結構而言，該結構會 引起所明之4-6-11相。本發明材料之各種結構中一般可見 之陽離子（若存在）分布列於表I中：
表I : 4-6-11結構中可用位點上陽離子之分布：
根據本發明 體結構。 之一較佳實施例，該材料基本上具有立方 晶 已展 下此會導致對本發明之各種應用而言具有進一步 改良之發光特徵的材料。 此已 根據本發明之_較佳實施例，該材料包含銷及飾 128440.doc 200848494 展示出對於本發明之各種應用均為有利的，且便於白光發 光材料之積聚。 根據本發明之一較佳實施例，銪與鈽之關係（以莫耳··莫 耳計）為21:0.5且$1:10，較佳地21:1且9:3，更佳>1:1 5且 :3。此已展示出對本發明之各種應用均為有利的。 在不文任何理論約束下，本發明者咸信摻入Ce(In)至少 部分地減少因為材料中存在之Eu (11)而可能產生的任何Eu (III)。因為Ειι (III)與Eu (II)之光譜特徵極為不同，所以該 材料之光學參數另外有所增加。 根據本發明之一較佳實施例，x^O.25且$〇·75，較佳>0.4 且S0.6。已發現此對本發明之各種結構均為有利的。 根據本發明之一較佳實施例，立方晶格常數&3〇2且 106 nm。已展示，具有此晶袼常數之結構尤其符合對於 本發明各種結構内的白色發光材料之需求。 本發明另外係關於本發明材料作為發光材料之用途。 本發明另外係關於尤其為LED之發光材料，其包含至少 一種如上所述之材料。 較佳地，該至少一種材料係以粉末及/或陶瓷材料形式 提供。 若該至少一種材料係至少部分地以粉末形式提供，則粉 末尤其較佳地具有3 已證實此有利於 本發明之廣泛應用。 右该至少一種材料係至少部分地以粉末形式提供，則Ce 之濃度（以莫耳計）尤其較佳地^〇 5%且^4%，較佳地^^/〇且 128440.doc 200848494 53%(Ml原子）。已發現此對本發明之各種材料均為有利 的。 根據本發明之一較佳實施例，該至少一種材料係至少部 分地以至少一種陶瓷材料之形式提供。 術語，才料，，在本發明之意義上尤其意謂及/或包括具 有又控里之孔或無孔的結晶或多晶緻密材料或複合材料。 —術語”多晶材料，，在本發明之意義上尤其意謂及/或包括體 ㈤度大於主成份的9〇%，由8〇%以上之單晶疇組成且其中 C 各晶嘴直徑大於0.5 _且具有不同結晶取向之材料。該等 單晶疇可藉由非晶形或玻璃質材料連接，或藉由其他結晶 成份連接。 ％ 根據一較佳實施例，該至少一種陶究材料之密度>理於 密度的90%且侧％。已證實此有利於本發明之廣泛: 用’因為隨後該至少一種陶瓷材料之發光特性可增加。 更佳地，該至少一種陶瓷材料之密度2理論密度的97%且 5100% ’更佳298%且別〇%，甚至更佳挪5%且2〇〇%且 最佳 299.0% 且 $100%。 右4至夕一種材料係至少部分地作為陶瓷提供，則G之 濃度（以莫耳計）尤其較佳地20.05%且2%，較佳地a 2%且 3.5%，更佳地μμ_<1%(μΙ原子）。已發現此對本發明 之各種材料均為有利的。 根據本發明之-較佳實施例，該至少一種陶竟材料表面 之表⑲較度RMS(表面平坦度之中斷；以最高表面特徵 與最深表面特徵之間的差異之幾何平均值來量測泣0·001 128440.doc 200848494 μηι且 S5 μιη 〇 根據本發明之一實施例，該至少一種陶瓷材料表面之表 面粗糙度20.005 μιη且;^0.8 μιη，根據本發明之一實施例 20.01 μιη且$〇·5 μηι，根據本發明之一實施例20.02 μη^ 50.2 μπι ’且根據本發明之一實施例M M 且$〇. 15 μηι。 根據本發明之一較佳實施例，該至少一種陶瓷材料之比 表面積210·7 m2/g且迎」m2/g 〇 本發明之材料及/或發光裝置可用於各種系統及/或應 用，以下各項為其中—或多種系統及/或應用： -辦公照明系統， -家用系統， -商鋪照明系統， -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， -像素顯示系統， -區段顯示系統， -警告標誌系統， -醫用照明應用系統， -指示標該系統，及 128440.doc -11- 200848494 裝飾照明系統， -攜帶型系統， -汽車應用， -溫室照明系統。 前述組份以及所主張之組份及根據本發明待用於所述實 施例中之組份關於其大小、形狀、材料選擇及技術概念並 無任何特定例外，因此可無限制地應用相關領域中已知之 選擇標準。 【實施方式】 本發明目標之其他細節、特徵、特性及優勢揭示於子申 請專利範圍、圖式及各別圖式及實例之以下說明中，其 (以例示方式）展示用於本發明之發光裝置的至少一種陶兗 材料之若干實施例及實例以及本發明之發光裝置的若干實 施例及實例。 圖1至圖4為本發明材料之咸信結構中1)至M(4)位點之 示意圖。此等圖僅應理解為說明性的且為平均值，且可因 本發明之不同實際組合物而變化。 如圖1中可見，咸信M(l)位點僅由Ba(若結構中存在）佔 據。然而，M(2)位點可由所有不同鹼土金屬佔據，咸信實 際位置視大小而定稍有不同，例如”Ca，，位置與”Ba，，位置略 微偏移。 M(3)位點可由多種原子佔據，而M(4)位點僅由(若結 構中存在）佔據。 將藉由以下實例I至V進一步瞭解本發明，其以僅供說明 128440.doc -12- 200848494 方式展示本發明之若干材料。 實例I : 圖5係指（Bai.8Ca2.2)Si6N1()〇:EiKl%)(實例I)且展示其發射 光譜（3 70 nm激發）。 此材料僅換雜有Eu。 實例II : 圖 6係指（Bai.8Ca2.2)Si6N10〇:Ce(l%)(實例 II)且展示其激 發光谱（虛線）及發射光譜。 此實例之材料展示在390 nm處具有強吸收帶，從而使該
材料適於由在370-400 nm光譜區域内發射之AunGaN UV-A LED激發。佔據晶格中m(3)位置之Ce (III)的發射位於藍色 光譜區域中，其肩部在綠色光譜區域中，此可解釋為m(4) 位點上亦嵌有一些Ce (III)。由於極小斯托克位移，摻雜有
Ce (III)之4-6-11相可在370-400 nm光譜區域内有效激發。 實例III及IV : 圖7係指叫1.8〇&2.2冲6>110〇:£11(1%)，〇6為1〇/0〇6(實例 III)及2% Ce(實例IV)，其展示發射光譜（實例m :下方曲 線，實例IV :上方曲線）。 可見，較回Ce(m)含量會抑制紅色光譜區域内之(m) 發射譜線，此導致總效率增強且因此為如上所述之本發明 之較佳實施例。 實例V : 圖 8係指 Ba"46Ca2 134Si6Nl〇 〇8〇〇 92:Eu〇 〇4Ce。⑽（實例 ^且 展示其發射光譜（3 90 nm激發）。 128440.doc -13 - 200848494 經發射之磷光體的光展示3760 K之相關顏色溫度及為96 之演色性指數，從而導致暖白光發射（X = 0.398，y = 0.402) 〇 為進一步說明本發明，下文描述實例IV之材料之製備： 用於合成（BauCarDSLNwOzEuUo/OCeG%)之起始材料 及溫度程式列於表II中·· 表II : 溫度程式 25ΐ 4 145〇ΐ(3 h) 1450〇C -> 1450〇C(10h) 1450〇C -> 800〇C(35h) 800°C -^25〇C(lh) 0.59 mol = 81.5 g 0.73 mol = 29.1 g 0.013 mol = 2.8 g 0.026 mol = 5.2 g 0.17 mol = 10.0 g 1.54 mol = 91.0 起始材料：
__丨丨丨丨 III
Ba:
Ca:
EuF3:
CeF3:
Si02 (Aerosil A380): Si(NH)2: 在氬氣氛下’藉由研磨將Ba&Ca金屬粉末與EuF3及CeF, 混合。接著，添加Si〇2及Si(NH)2且將由前軀物材料形成之 批料精細混合。混合後，將前軀物批料轉移至鉬坩堝中且 接著在A或H2/N2(5/95)氣氛下以表！中給出之溫度程式燒 製。燒製後，研磨發光粉末材料且將其以水洗滌。乾燥 後，對磷光粉進行篩檢以獲得具有所要粒徑分布之粉末。 類似於此程序製備其他實例之材料。 圖9為展示本發明各種材料之晶袼常數與仏含量之間的 關係之圖表。在此圖表中，量測淨式叫办⑻办。。之各 種材料的晶格常數（如圖表中所示，以為1()至2.2)。 根據Veegart定律，較大主體陽離子（Ba)之摻入會導致單 位晶胞擴大，而較小主體陽離子心)之摻人會導致單位晶 128440.doc -14- 200848494 胞收縮。 意外地發現，在第一種狀況下，摻雜有Ce (ιπ)及Eu (ιι) 的材料之寬帶發射略微朝藍光偏移，而在後一種狀況下， 發射略微朝紅光偏移。因此’具有淨式(Bai為 zSuNw+zOuEiiyCezi材料的磷光體發射之相關顏色溫度 可藉由改變Ba/Ca比率而調|皆。
上文詳述實施例中之元件及特徵之特定組合僅為例示性 的；亦明確預期以本申請案及以引用方式併入之專利/申 請案中之其他教示交換及替代該等教示。熟習此項技術者 將瞭解，-般技術者可不偏離所主張之本發明精神及範疇 而2行本文所述内容之改變、修正及其他實施例。因此， 先鈉描述僅舉例而§且並非意欲加以限制。本發明之範疇 限定於以下申請專利範圍及其等效物中。此外，用於說明 書及申請專利範圍中之參考標諸並不限制所主張之本發明 範疇。 【圖式簡單說明】 圖1為本發明材料之咸信結構中M(l)位點之示意圖； 圖2為本^明材料之咸信結構中m⑴位點之示意圖； 圖為本^明材料之咸信、结構中M( 1)位點之示意圖； 圖為本么明材料之咸信結構中M( 1)位點之示意圖； 圖5為本發明第一實例之材料的發射光譜（370 nm激 發）； 圖6為本發明篦-鲁 、 I 一貢例之材料的激發光譜及發射光譜； 圖7為本發明繁： 一&第四實例之兩種材料的兩個發射光 128440.doc 200848494 譜（370 nm激發）； 圖8為本發明第五實例之材料的發射光譜（370 nm激 發）；且 圖9為展示本發明各種材料之晶格常數與Ba含量之間的 關係之圖表。
128440.doc -16-

Claims (1)

  1. 200848494 十、申請專利範圍： 1· -種 MYxM'Si^+xObx， 由此Μ1係選自二價鹼土金廛 1貝鹼上至屬、銪或其混合物之群， Μ係選自三價稀土金屬、 纪、鑭、銃或其混合物之 群 且χ>0且$1。 2·如請求項1之材料，由此該枒4 衬枓基本上具有立方晶體結 構。 3·如請求項1或2之材料’由此該材料包含销及鈽。 4·如請求項⑴中任一項之材料，由此銷及飾之含量（以 mol:mol 計）2ΐ:0·5 且 。 5. -種如請求項⑴中任一項之材料之用途，其係用作發 光材料。 6. 一種發光裝置，其尤其為包含至少一種如請求項⑴中 任一項之材料之led。 7. 如請求項6之發光裝置，由此提供至少一種粉末及/或陶 瓷材料形式之結構Μΐ4-χΜΠχΜ6Νΐ()+χ〇ι·χ的材料。 8. 如請求項6至7中任一項之發光裝置，其另外包含至少一 種UVA發光材料及/或至少一個uva發光源。 9. 如請求項6至8中任一項之發光裝置，由此該陶瓷具有 2理論密度的90%的密度。 ίο. 一種包含如請求項丨至4中任一項之材料及/或如請求項6 至9中任一項之發光裝置及/或如請求項5之製造用途的系 統’該系統係用於以下應用中之一或多種： 128440.doc 200848494 -辦公照明系統， -家用系統， -商鋪照明系統， 家庭照明系統， -重點照明系統， -聚光照明系統， -劇院照明系統， -光纖應用糸統’ -投影系統， -自發光顯示系統 -像素顯不糸統’ -區段顯不糸統， -警告標諸系統， 統， 及 -醫用照明應用系 -指示標誌、系統， -裝飾照明系統， -攜帶型系統， -汽車應用， -溫室照明系統。 128440.doc
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