TWI453277B - 具有多相矽鋁氮氧化物為基的陶瓷材料之發光裝置 - Google Patents

具有多相矽鋁氮氧化物為基的陶瓷材料之發光裝置 Download PDF

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TWI453277B
TWI453277B TW097139240A TW97139240A TWI453277B TW I453277 B TWI453277 B TW I453277B TW 097139240 A TW097139240 A TW 097139240A TW 97139240 A TW97139240 A TW 97139240A TW I453277 B TWI453277 B TW I453277B
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lighting
phase
illuminating device
multiphase
ceramic
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TW200932886A (en
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Peter J Schmidt
Baby-Seriyati Schreinemacher
Andreas Tuecks
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Koninkl Philips Electronics Nv
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Description

具有多相矽鋁氮氧化物為基的陶瓷材料之發光裝置
本發明係關於發光裝置，尤其係關於LED領域。
磷光體的材料(或磷光體)係使用作為波長轉換器(或磷光體轉換器=pc)，其吸收自光源發出的第一波長及再發出長於第一波長的第二波長(螢光材料)。普遍已知包含作為主體材料的矽酸鹽、磷酸鹽(例如，磷灰石)磷光體及鋁酸鹽，與以主體材料的活化材料添加的過渡金屬或稀土金屬的磷光體。尤其，近年來，隨著藍色LED光源已變得實用，正積極實行利用結合此磷光體材料之此藍色LED發展白光源。
尤其，以稱為"鋁氮氧化物(SiAlON)"系統為基的螢光材料因其良好的光特徵，在該領域已引起注意。
但，仍需要在大範圍應用中可用及尤其可製造具有較佳發光效率與現色性的磷光體暖白光pcLED之螢光材料。
本發明之目的係提供一種具有螢光材料可改善光特徵及具有良好可製造性的發光裝置。
該目的係由如本發明技術方案1之發光裝置解決。是以，本發明之一種發光裝置，其包含尤其是LED之光源，與主要為M2-z Cez Si5-x-y-(z-z1) Ay＋(z-z1) N8-4x-y＋z1 O4x＋y-z1 組合物的陶瓷多相材料的螢光材料。
其中M係選自包含Sr、Ca、Ba、Mg、Eu或其混合物之群。
A係選自包含Al、B、Ga或其混合物之群，及x係至，y係至，z係至及z1 係至。
術語"多相"尤指及/或包含材料由形成所述總組合物的至少兩種不同結晶圖可識別相構成。這些相可為不同組合物，但在本發明中非必需。
術語"主要"尤指，較佳及最佳材料具有所需組合物。
術語"陶瓷材料"在本發明中意指及/或尤包含一種具有控制含量孔或無孔之晶體或多晶緻密材料或複合材料。
術語"多晶材料"在本發明中意指及/或尤包含一種具有大於90%主要成分之體積密度，包含大於80%單晶範圍，每個範圍直徑係大於0.5μm之材料且可具有不同結晶取向。單晶範圍可由非晶或玻璃狀材料或另一些結晶成分連接。
對於本發明內大範圍應用，此材料顯示具有至少以下益處中至少一個：
-該材料量子效率通常相對於先前技術的多種"單相"材料極大改善；
-該材料通常利用極佳轉換效率；
-該材料通常具有極高熱安定性，尤其光熱安定性。
認為初始組合物中x的增加可增加燒結後多相陶瓷中第二相含量，從而增加螢光陶瓷光散射。但是，適當調整名義組合物M2-z Cez Si5-x-y-(z-z1) Ay＋(z-z1) N8-4x-y＋z1 O4x＋y-z1 陶瓷(其顯示因富氧相助熔作用的高密度)中x值(如上述)，則可達到高光透射。根據較佳實施例，x為與，較佳係與。
進一步認為隨著本發明材料中A含量的增加，第二相含量通常減少及O於材料中溶解度增加。在A包含硼或鋁之情況下，亦通常發現相(如稍後描述)顆粒生長增加。根據較佳實施例，y＋(z-z1 )係與，較佳係與。
發明者亦發現隨著Ba含量增加，活化劑發射(Eu及/或Ce)通常向較短波長移動，而Ca及/或Sr可向更長波長移動。較佳是，Ba含量(以"M"原子數%)係，較佳係。
根據較佳實施例，本發明材料包含Eu。如果存在Eu，尤其較佳是其含量(以"M"原子數%)係與，較佳係與。
但，如果本發明材料包含Eu與Ce，尤其較佳是Eu與Ce的添加量(以總材料莫耳%)為，較佳係。
根據本發明較佳實施例，多相材料包含至少一種組合物M2-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 之相，M、A、z與z1 如上定義及a係至。
對於本發明內多種應用，顯示其為有利的。更確切的說，多相材料包含至少一種組合物Bab MI 2-b-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 之相，MI 係選自包含Sr、Ca、Mg、Eu或其混合物之群及A、z與z1 如以上定義及a係至及b係至。
材料中M2-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 及/或Bab MI 2-b-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 相之體積含量係，較佳係及最佳係。
根據本發明較佳實施例，多相材料包含至少一種組合物MSi7 N10 之相，M如上定義。
對於本發明內多種應用，顯示其為有利的，尤其發現如果此相存在於本發明材料中，該材料可行性極大簡化(如稍後說明)。
較佳是，MSi7 N10 相體積含量係，較佳係及最佳係。
根據本發明較佳實施例，多相材料包含至少一種組合物M2 SiO4 之相，M如上定義。
對於本發明內多種應用，顯示其為有利的，尤其發現如果此相存在於本發明材料中，該材料可行性極大簡化(如稍後說明)。
較佳是，M2 SiO4 相體積含量係，較佳係及最佳係。
根據本發明較佳實施例，本發明相中至少一種主要以顆粒形式存在於多相材料中。
根據本發明較佳實施例，顆粒中至少一部分的d50 係μm至。藉此，對於多種應用，可改善光特徵與本發明多相陶瓷安定性。
術語"d50 "在本發明中為一種用於平均粒徑的測量方法及如下定義：相應樣品中50%粒子(例如顆粒)大小係等於或小於已定d50 值。
根據本發明另一及/或較佳實施例，至少一部分顆粒的d50 係至。藉此，對於多種應用，可改善光特徵與本發明多相陶瓷安定性。
應了解根據本發明，最佳係粒度係"相當低"或"相當高"。因此，很明顯的是，如果顆粒中一些係小的(即具有0.5至4μm之d50 )及一些係大的(即具有5至30μm之d50 )，則顆粒混合物亦為本發明較佳實施例。
根據本發明較佳實施例，在陶瓷材料於260℃，10W/cm2 光功率密度與2.75eV平均光子能暴露10小時後，陶瓷多相材料的光熱安定性係至。
術語"光熱安定性"在本發明中尤指及/或包含在同時施加熱與高強度激發後，發光強度不變，即100%光熱安定性指材料幾乎不受同時輻射與受熱影響。術語不受影響尤指發射光強度保持不變。
根據本發明較佳實施例，在陶瓷材料於260℃，10W/cm2 光功率密度與2.75eV平均光子能暴露10小時後，陶瓷多相材料的光熱安定性係至，較佳係至。
根據本發明較佳實施例，陶瓷多相材料的熱傳導率為至。
根據本發明一實施例，陶瓷多相材料顯示對於波長 至之光在空氣中正入射的透明度係至。
對於波長至之光在空氣中正入射的透明度係至，更佳係至及最佳係對於波長至之光為>40%至<70%。
術語"透明度"在本發明中尤指該波長，較佳，更佳，最佳與入射光不能由材料吸收，穿透空氣中正入射的樣品(以任意角)。此波長較佳於與範圍內。
根據本發明較佳實施例，陶瓷多相材料具有理論密度與之密度。在全文中，多相陶瓷的所有相對密度尤其指常用組合物M2-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 及/或Bab MI 2-b-z Cez Si5-a-(z-z1) Aa＋(z-z1) N8-a＋z1 Oa-z1 較佳主要組分的理論密度。
根據本發明較佳實施例，陶瓷多相材料具有理論密度與之密度。
根據本發明所述較佳實施例，小於100%的密度較佳係經燒結陶瓷至在陶瓷基質中仍存在孔之階段得到。最佳係範圍與之密度，陶瓷基質中總孔體積於至之間。較佳平均孔直徑係於之間。
本發明進一步係關於一種自包含M2 Si5-y Ay N8-y Oy -材料與矽-前驅體-材料的至少兩種前驅體材料的陶瓷多相材料製造用於根據本發明之發光裝置之方法。
術語"矽-前驅體-材料"尤意指或包含一種包含矽酸鹽或經取代的矽酸鹽之材料。尤佳係矽酸鹽及/或氧-氮-矽酸鹽。最佳係MSi2 O2 N2 及/或M2 SiO4 。
本方法較佳包含低溫壓縮階段，較佳在<100℃溫度下，最佳在周圍溫度下。
令人吃驚的係發現根據本發明之材料可無高溫壓縮步驟經製造。
術語"壓縮步驟"尤意指及/或包含具有前驅體材料(及，若必要，進一步佐劑或補充材料)之混合物經>50bar壓力至少>30分鐘。
根據本發明另一實施例，該方法包含燒結步驟，其較佳在壓縮步驟後進行。
術語"燒結步驟"在本發明中尤意指在熱量作用下壓緊前驅體粉末，其結合施加同軸或均衡壓力，未達到燒結材料主要成分的液態。
根據本發明較佳實施例，燒結步驟係無壓的，較佳是在還原性或惰性大氣下。
根據本發明較佳實施例，該方法另包含在燒結前，壓縮陶瓷前驅體材料至為材料主要成分的相應單晶相的至，較佳至理論密度之步驟。實際顯示此改善用於本發明所述的大多數陶瓷多相材料之燒結步驟。
根據本發明較佳實施例，製造用於根據本發明之發光裝置的陶瓷多相材料之方法包含以下步驟：
(a)　混合陶瓷多相材料的前驅體材料
(b)　視需要焙燒前驅體材料，較佳在至溫度下，以移除揮發性材料(例如CO2 ，在使用碳酸鹽情況下)
(c)　視需要研磨與沖洗
(d)　第一次壓縮步驟，較佳係利用適宜的具有所需形狀(如桿狀或顆粒狀)模具的粉末壓製工具之同軸壓縮步驟及/或較佳在至的冷均壓步驟
(e)　在至壓力的惰性、還原性或微氧化大氣中，於至下的燒結步驟
(f)　在>1000℃至<1700℃下，於惰性大氣或包含氫氣的大氣中視需要的後退火步驟。
根據該方法，對於最需材料組合物，此製造方法已製造用於本發明的最佳陶瓷多相材料。
根據本發明之發光裝置與根據本發明製造的陶瓷多相材料可用於多種系統及/或應用，以下為其中一種或多種：
-　辦公室照明系統
-　家庭應用系統
-　商店照明系統
-　家庭照明系統
-　效果照明系統
-　局部照明系統
-　劇場照明系統
-　光纖應用系統
-　投影系統
-　自點亮顯示系統
-　像素顯示系統
-　分段式顯示系統
-　警告標誌系統
-　醫學燈光應用系統
-　指示符號系統，及
-　裝飾照明系統
-　可攜式系統
-　汽車應用
-　溫室照明系統
上述組分，及請求之組分與可根據本發明用於所述實施例之組分，不受與其大小、形狀、材料選擇與技術概念相關的任意特定例外限制，使相關領域已知的選擇標準可無限制應用。
本發明目標的其他細節、特徵、特點與益處於隨附請求項、圖式及以實例方式，分別顯示用於根據本發明之發光裝置的陶瓷多相材料多個實施例與實例的隨後圖式與實例的描述中揭示。
實例I與II
結合僅以闡述形式，為本發明陶瓷多相材料二實例的實例I與II將更易理解本發明。
實例I有關於Ba1.454 Sr0.536 Eu0.01 Si4.967 N7.868 O0.132 ，其由以下方式製造：
首先，製造二前驅體材料(a)與(b)：
(a)　製備Ba1.5 Sr0.49 Eu0.01 Si5 N8 粉末
(Ba0.75 Sr0.245 Eu0.005 )2 Si5 N8 粉末可根據以下反應製備：
1.5 BaH2 ＋0.49 SrH2 ＋5 SiN4/3 ＋0.005 Eu2 O3 ＋2/3 N2 →Ba1.5 Sr0.49 Eu0.01 Si5 N8 ＋0.015 H2 O＋1.975 H2
所有前驅體粉末於乾燥大氣中，由球磨研磨混合，然後在1450℃下，於合成氣體中焙燒。焙燒後，粉末經磨碎及由鹽酸沖洗且乾燥：粉末A
(b)製備SrSi2 O2 N2
根據以下反應製備SrSi2 O2 N2
SrO＋0.5 SiO2 ＋3/2 SiN4/3 →SrSi2 O2 N2
所有前驅體粉末於乾燥大氣中，由球磨研磨混合，然後在1300℃下，於氮氣中焙燒：粉末B
(c)陶瓷加工
95重量%粉末A與5重量%粉末B由球磨研磨於無水乙醇中混合。添加聚乙烯醇縮丁醛粘合劑與粒化後，混合物經冷均壓以得到綠色陶瓷盤。該等盤於600℃在氮氣中脫脂，並於1650℃在氮氣中焙燒4-8小時。
結果：具有4.32g/cm3 密度(相對於相純(Ba0.75 Sr0.25 )2 Si5 N8 陶瓷的理論密度為97.3%相對密度)的密實複合陶瓷。
圖1顯示實例I材料的XRD模式。圖2顯示(由上而下)M2 SiO4 (斜方晶)、MSi7 N10 與M2 Si5 N8 (斜方晶)的三個XRD模式。
由圖1與2的重合，明顯係根據實例I的材料包含作為主相(>90%)的斜方晶M2 Si5 N8 相與作為額外相的斜方晶M2 SiO4 與MSi7 N10 。
實例II
實例II指Ba1.404 Sr0.582 Eu0.014 Si4.936 N7.744 O0.256
類似於實例I材料製造該材料，除步驟a)中製造具有0.7at%Eu摻雜含量(相對於M-型原子)的粉末及在步驟c)陶瓷加工中，90重量%粉末A與10重量%粉末B混合。
因此，得到具有相對於相純(Ba0.75 Sr0.25 )2 Si5 N8 陶瓷的理論密度為96.7%相對密度的密實複合陶瓷。
圖3顯示實例I材料的XRD模式。圖4顯示(自上而下)M2 SiO4 (斜方晶)、MSi7 N10 與M2 Si5 N8 (斜方晶)的三個XRD模式。
由圖3與4的重合，明顯係根據實例I的材料包含作為主相(>85%)的斜方晶M2 Si5 N8 相與作為額外相的斜方晶M2 SiO4 與MSi7 N10 。
圖5顯示較綜合性圖表，其中顯示如本發明一些實例中所發現的SrSi2 O2 N2 前驅體材料含量與三相相對含量的關係。一般而言，M2 SiO4 與MSi7 N10 含量隨SrSi2 O2 N2 前驅體材料的添加量增加而增加，藉此當SrSi2 O2 N2 前驅體材料含量在初始混合物中超過5重量%時，M2 SiO4 相通常更顯著。
圖6顯示實例I與II材料的發射光譜。
為此，實例I與II厚度200μm陶瓷磨光試樣由450nm發射的發藍光LED光源激發。該陶瓷在淡黃色光譜範圍內顯示有效發射。實例II(虛線)顯示相對於實例I因較高Sr與Eu濃度的紅移顏色點。
實例III
實例II指M2-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 及/或Bab M2-b-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1
材料中M2-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 及/或Bab M2-b-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 相的體積含量係70%及/或M2 Si7 N10 相及/或M2 SiO4 相的體積含量係15%。
上述具體實施例中要素與特徵的特定組合僅為實例性；亦具體假定在本案及以引用的方式併入的專利/申請案中此等指示與其他指示的相互交換與替代。如擅長該技術者了解，文中所述的變化、修改、及其他實施可在未脫離如請求之本發明主旨與範圍下由擅長該技術者進行。因此，上述描述僅以實例方式且不具限制性。本發明範圍在以下請求項及其同等物中定義。而且，說明與請求項中使用的參考符號不限制如請求之本發明範圍。
圖1顯示根據本發明實例I之材料的XRD模式。
圖2顯示存在於根據實例I之材料中三種主要相的三個XRD模式。
圖3顯示根據本發明實例II之材料的XRD模式。
圖4顯示存在於根據實例II之材料中三種主要相的三個XRD模式。
圖5顯示主相相對含量與在製造材料前添加的前驅體含量的關係圖。
圖6分別顯示實例I與II之材料的兩個發射光譜。
(無元件符號說明)

Claims (9)

  1. 一種發光裝置，包含尤其是一LED之一光源，及一主要為以下組合物的陶瓷多相材料之一螢光材料：M2-z Cez Si5-x-y-(z-z1) Ay+(z-z1) N8-4x-y+z1 O4x+y-z1 其中M係選自包含Sr、Ca、Ba、Mg、Eu或其混合物之群，A係選自包含Al、B、Ga或其混合物之群，及x係0.0005與0.25，y係0至4，z係0至1及z1 係0至z。
  2. 如請求項1之發光裝置，其中y+(z-z1 )係0.05與0.8。
  3. 如請求項1或2之發光裝置，其中該Ba含量(以"M"原子數%)係30%。
  4. 如請求項1或2之發光裝置，其中該Eu含量(以"M"原子數%)係0.02%與5%。
  5. 如請求項1或2之發光裝置，其中該Eu與Ce添加含量(以總材料莫耳%)係3%。
  6. 如請求項1或2之發光裝置，其中該多相材料包含至少一組合物M2-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 相，M、A、z與z1 如上定義及a係0至4。
  7. 如請求項1或2之發光裝置，其中該多相材料包含至少一組合物MSi7 N10 及/或M2 SiO4 相。
  8. 如請求項1或2之發光裝置，材料中M2-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 及/或Bab M2-b-z Cez Si5-a-(z-z1) Aa+(z-z1) N8-a+z1 Oa-z1 相的體積含量係70%及/或M2 Si7 N10 相及/或M2 SiO4 相 的體積含量係15%。
  9. 一種包含如請求項1至8中任一項之發光裝置的系統，該系統可用於以下應用中一或多者：- 辦公室照明系統- 家庭應用系統- 商店照明系統- 家庭照明系統- 效果照明系統- 局部照明系統- 劇場照明系統- 光纖應用系統- 投影系統- 自點亮顯示系統- 像素顯示系統- 分段式顯示系統- 警告標誌系統- 醫學燈光應用系統- 指示符號系統，及- 裝飾照明系統- 可攜式系統- 汽車應用- 溫室照明系統。
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