TWI520923B - A wavelength conversion member, a light emitting device, and a wavelength conversion member - Google Patents

A wavelength conversion member, a light emitting device, and a wavelength conversion member Download PDF

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TWI520923B
TWI520923B TW100115783A TW100115783A TWI520923B TW I520923 B TWI520923 B TW I520923B TW 100115783 A TW100115783 A TW 100115783A TW 100115783 A TW100115783 A TW 100115783A TW I520923 B TWI520923 B TW I520923B
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phase
wavelength conversion
conversion member
light
rare earth
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TW100115783A
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TW201213272A (en
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Kazuhiro Wataya
Toshihiko Tsukatani
Yasushi Takai
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Shinetsu Chemical Co
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Description

波長變換構件、發光裝置、及波長變換構件之製造方法
本發明，係與使由光源所發光之光的一部分透射，並對一部分實施波長變換之波長變換構件、利用其之發光裝置、以及波長變換構件之製造方法相關。
發光二極體，係現在可利用之光源當中，最有效率的光源之一。近年來，積極地針對組合著藍色發光LED及螢光體之白色LED進行開發。例如，日本特開2007-150331號公報(專利文獻1)中，就提出了將發光元件所釋出之光進行波長變換而具透光性且均質之波長變換構件當作含柘榴石等之波長變換構件、及具備該波長變換構件之發光裝置。並且，該波長變換構件，相較於傳統之組合著螢光體及用以使其分散之樹脂的波長變換層，可以期待高耐熱性及高機械強度，相對於隨著發光元件之輸出的變大而增大之發熱，可期待高耐久性。
將柘榴石使用於波長變換構件時、透光性且均質之波長變換構件時、從光源發光之光透射波長變換構件之透射光時，於波長變換構件中直線前進，另一方面，為波長變換構件所吸收而為經過波長變換之波長變換光時，因為全部方向為等向發光，透射光及波長變換光之配光模式不同。所以，由具備此種波長變換構件之發光裝置所發光之光，其色澤不均一，此種發光裝置，只能得到色澤不均一之照明面。其對策，可以利用於發光裝置之外周部設置不透明或半透明之光擴散構件，來謀求緩和照明面之色澤不均，然而，因為使用光擴散構件，光的一部分因為光擴散構件而損失，因而導致光之利用效率降低。
[專利文獻1]　日本特開2007-150331號公報
本發明，係以解決上述問題點為目的者，其目的在於提供：於使由光源所發光之光的一部分透射並對一部分實施波長變換之波長變換構件，可以減輕透射光及波長變換光之配光不同所造成之色澤不均，於照明面，可以賦予均一色澤之波長變換構件、利用其之發光裝置、以及波長變換構件之製造方法。
於使用波長變換構件之發光裝置，為了減輕如上所述之透射光及波長變換光之配光不同所造成的色澤不均，儘可能抑制透射光之損失，並使透射光於波長變換構件中散射是有效的方法。
例如，為了使透射波長變換構件之光產生散射，於燒結體之波長變換構件，可以考慮使其含有氣泡來刻意降低燒結密度，而降低由發光裝置發光之光的色澤不均，然而，此時，因為波長變換構件及氣泡之折射率的差太大，因為波長變換構件與氣泡之界面之光的反射、散射等，而有發光裝置之發光效率降低的缺點。
所以，本發明者，為了解決上述課題而重複進行審慎檢討，發現以下之結果，亦即，構成發光裝置之波長變換構件，含有：(A)柘榴石相、及(B)從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相，(A)相中含有而分散著由(B)相所構成之微細結晶之多晶體的燒結陶瓷，使透射波長變換構件之光於柘榴石相、及鈣鈦礦相、單斜晶相、或矽酸鹽相之界面適度散射，可以抑制發光裝置之發光效率的降低且可以減輕發光裝置所發光之光的色澤不均，而完成本發明。
因此，本發明，係提供下述之波長變換構件、發光裝置、及波長變換構件之製造方法。
申請專利範圍第1項：一種波長變換構件，係包含著：(A)以下述組成式(1)
(A1-xBx)3C5O12　(1)
(式中，A係從Y、Gd及Lu所選取之1種類以上之稀土元素，B係從Ce、Nd及Tb所選取之1種類以上之稀土元素，C係從Al及Ga所選取之1種類以上之元素，x為0.002≦x≦0.2)所示之柘榴石相；及(B)從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相之多晶體的燒結陶瓷；其特徵為：(A)相中含有而分散著由(B)相所構成之微細結晶。
申請專利範圍第2項：係如申請專利範圍第1項所述之波長變換構件，其中上述鈣鈦礦相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素：以及氧。
申請專利範圍第3項：係如申請專利範圍第1或2項所述之波長變換構件，其中上述單斜晶相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；以及氧。
申請專利範圍第4項：係如申請專利範圍第1至3項中任一項所述之波長變換構件，其中上述矽酸鹽相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；矽；以及氧。
申請專利範圍第5項：係如申請專利範圍第1至4項中任一項所述之波長變換構件，其中由上述(B)相所構成之微細結晶的平均粒徑為0.1μm以上。
申請專利範圍第6項：係如申請專利範圍第1至5項中任一項所述之波長變換構件，其中燒結陶瓷之氣孔率為0.1體積%以下。
申請專利範圍第7項：係一種發光裝置，係利用如申請專利範圍第1至6項中任一項所述之波長變換構件的發光裝置，其特徵為：來自光源之光的一部分透射上述波長變換構件，且來自光源之光的一部分由上述波長變換構件進行波長變換並發光。
申請專利範圍第8項：係一種波長變換構件之製造方法，係用以製造如申請專利範圍第1項所述之波長變換構件的方法，其特徵為：將以賦予(A)相之組成而含有(A)相所含有之各元素的原料粉末、及以賦予(B)相之組成而含有(B)相所含有之各元素的原料粉末進行混合，對所得到之混合粉末實施成形，且對所得到之成形體進行加熱並燒結。
透射本發明之波長變換構件的光，因為於在波長變換構件中之柘榴石相、與鈣鈦礦相、單斜晶相、或矽酸鹽相之界面散射，利用此波長變換構件之發光裝置，光的損失較少，此外，發光色之均一性良好。亦即，使用此種波長變換構件之發光裝置，透射波長變換構件之光及被波長變換之光的配光均一性，相較於傳統者，獲得改善，而得到色澤不均獲得改善之照明面。
以下，針對本發明進行詳細說明。
本發明之波長變換構件，係包含(A)相之柘榴石相、及(B)相之從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相的多晶體之燒結陶瓷。此外，本發明之波長變換構件，係以(A)相作為主相，而由(B)相所形成之微細結晶係包含分散於由主相之(A)相所形成之結晶中。
該等相之狀態，具體而言，例如，係如第1圖所示之波長變換構件的剖面示意圖所示，係於柘榴石相((A)相)之結晶1中，分散分佈著從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相((B)相)之微細結晶2的構造，係不同之2種相所形成之所謂海島構造的狀態。
若波長變換構件為此種相構造之多晶體的燒結陶瓷，將其使用於使來自光源之光的一部分透射波長變換構件且以波長變換構件對來自光源之光的一部分進行波長變換來發光之發光裝置的話，透射波長變換構件之光、及經由波長變換構件進行變換之光，皆可於柘榴石相、與鈣鈦礦相、單斜晶相或矽酸鹽相之界面進行適度散射，而抑制發光裝置之發光效率的降低，並減少發光裝置所發光之光的色澤不均。
(A)相及(B)相之比率((B)相/(A)相)，以0.001～0.2、尤其是，0.001～0.1為佳。該比率若超過上述範圍的話，發光效率可能降低，於上述範圍以下，則散射所造成之色澤不均的改善效果可能降低。該比率，可以藉由製造燒結體時之賦予兩相之原料粉末比率的調整來設定。
由(B)相所構成之微細結晶的平均粒徑以0.1μm以上為佳，此外，以1mm以下為佳。0.1μm以下的話，透射光之散射效果可能降低，超過1mm的話，因為(B)相之結晶粒徑過大，而可能導致透射光之透射率的降低。
此外，燒結陶瓷之氣孔率為0.5體積%以下，尤其是，以0.1體積%以下為佳。氣孔率高於上述範圍的話，透射波長變換構件中之光，尤其是，為波長變換構件所吸收而經過波長變換之光，因為於波長變換構件中之氣孔散射而造成損失，可能導致發光效率的降低。
本發明之波長變換構件，(A)相之柘榴石相，以下述組成式(1)
(A1-xBx)3C5O12　(1)
(式中，A係從Y、Gd及Lu所選取之1種類以上之稀土元素，B係從Ce、Nd及Tb所選取之1種類以上之稀土元素，C係從Al及Ga所選取之1種類以上之元素，x為0.002≦x≦0.2)所示之柘榴石相為佳。
另一方面，(B)相之鈣鈦礦相，係含有從Ce、Nd及Tb所選取之1種類以上之稀土元素的氧化物鈣鈦礦相，尤其是，以含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；以及氧之鈣鈦礦相為佳。此種鈣鈦礦相，具體而言，例如，以下述組成式(2)
(A1-yBy)CO3　(2)
(式中，A、B及C與上述相同，y係0.002≦y≦0.98)所示者。
此外，(B)相之單斜晶相(單斜相)，係含有：從Ce、Nd及Tb所選取之1種類以上之稀土元素的氧化物單斜晶相，尤其是，以含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；以及氧之單斜晶相為佳。此種單斜晶相，具體而言，例如，以下述組成式(3)
(A1-zBz)4C2O9　(3)
(式中，A、B及C與上述相同，z係0.002≦z≦0.98)所示者。
此外，(B)相之矽酸鹽相，係含有：從Ce、Nd及Tb所選取之1種類以上之稀土元素的矽酸鹽相，尤其是，以含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；矽；以及氧之矽酸鹽相為佳。
此種多晶體陶瓷之波長變換構件的製造，可以減少波長變換構件內之氣泡，此外，從使(B)相均一分散於(A)相中之觀點而言，以燒結法來製造為佳，然而，也可以其他方法來製造。
以燒結法來製造時，具體而言，首先，以賦予(A)相之組合含有(A)相所含有之各元素的原料粉末，來製造具有柘榴石相或接近其之組成之含有比率的陶瓷粉末。於該製造時，係以如上述特定之含有比率，混合柘榴石相所含有之各元素的氧化物、氫氧化物等之粉末，於大氣環境中、或真空中，藉由900～1500℃之溫度、10分鐘～8小時的燒結，可以得到柘榴石相單相組成的原料粉末。
以賦予(B)相之組成含有(B)相所含有之各元素的原料粉末，為鈣鈦礦相及單斜晶相時，與柘榴石相相同，以上述特定之含有比率將具有鈣鈦礦相或接近其之組成之含有比率的陶瓷粉末或具有單斜晶相或接近其之組成之含有比率的陶瓷粉末，與各相所含有之各元素之氧化物等粉末進行混合，於大氣環境中、真空中，藉由900～1500℃之溫度、10分鐘～8小時的燒結，可以得到各相單相組成之原料粉末。
另一方面，矽酸鹽相時，含有矽之化合物，例如，以氧化矽、矽樹脂等之粉末作為(B)相之原料粉末即可。(A)相採用上述組成式(1)所示之柘榴石相時，添加之矽化合物的一部分或全部，係於燒結過程，用以形成由組成式(1)中之A、B及C所表示之元素及矽及氧所構成之矽酸鹽相。
其次，將以構成該等(A)相為目的之原料粉末、以形成(B)相為目的之原料粉末，以如上述之((B)相/(A)相)之比率進行混合，將所得到之混合粉末，以衝壓法、注漿法、全張成形法等實施成形，再將所得到之成形體，於大氣環境中、還原環境中、或真空中實施加熱燒結，而得到緻密之陶瓷燒結體的波長變換構件。尤其是，因為可以儘量減少波長變換構件中之氣泡，故以真空燒結為佳。
此外，為了提高波長變換構件之密度，燒結溫度應為1700℃以上，尤其是，以1750℃以上為佳。此外，燒結溫度以2000℃以下為佳。燒結溫度，超過上述範圍的話，於經濟面較為不利。燒結時間，通常為4～24小時程度。於該燒結過程，可以形成主相之(A)相且同時形成(B)相，而使(B)相分散存在於(A)相中。
[實施例]
以下，係以實施例及比較例，針對本發明進行具體說明，然而，本發明並未受限於下述實施例。
[實施例1]
將純度99.9%、平均粒徑1.0μm之氧化釔(Y2O3)粉末、純度99.0%、平均粒徑0.5μm之氧化鋁(Al2O3)粉末、以及純度99.9%、平均粒徑0.2μm之氧化鈰(CeO2)粉末，以分別為Y：Al：Ce=2.98：5：0.02之莫耳比，利用攪拌器進行30分鐘混合，而得到500g之混合粉末。其次，將該混合粉末，於大氣環境中實施1400℃、4小時之燒結，而得到柘榴石相單相組成之原料粉末(1-1)500g。
另一方面，將純度99.9%、平均粒徑1.0μm之氧化釔(Y2O3)粉末、純度99.0%、平均粒徑0.5μm之氧化鋁(Al2O3)粉末、以及純度99.9%、平均粒徑0.2μm之氧化鈰(CeO2)粉末，以分別為Y：Al：Ce=2.98：3.00：0.02之莫耳比進行混合，而得到1g之混合粉末。其次，將該混合粉末，於大氣環境中實施1400℃、4小時之燒結，而得到鈣鈦礦相單相組成之原料粉末(1-2)1g。
將該等原料粉末(1-1)及(1-2)，以攪拌器實施1小時之混合，得到燒結用之原料粉末(1)。其次，將所得到之原料粉末(1)以單軸衝壓機實施衝壓成形後，以1750℃進行真空燒結，得到緻密之燒結體。從所得到之燒結體切取長1.5mm、寬2.0mm、厚200μm之薄板狀之燒結體，並作為波長變換構件。
測定該波長變換構件之燒結密度時，係4.55g/cm3，氣孔率為0.1體積%。觀察該波長變換構件之剖面時，為氣泡較少之緻密的燒結體。此外，對該波長變換構件以XRD實施定性分析時，確認主相為YAG相(柘榴石相)而其餘為YAP相(鈣鈦礦相)。更進一步，以電子顯微鏡觀察該波長變換構件之組織來進行EPMA分析時，確認平均粒徑約3μm之YAP相係以包含分散於YAG相之狀態存在於YAG相中。第2圖，係電子顯微鏡像及EPMA像。
以470nm之光激發所得到之波長變換構件時，波長變換構件之內部量子效率為0.90。此外，以470nm之點光源照射該波長變換構件時，在光源之照射面的相反側之面，得到無色澤不均一之發光。
[實施例2]
以與實施例1相同之方法，得到原料粉末(1-1)500g。另一方面，將純度99.9%、平均粒徑1.0μm之氧化釔(Y2O3)粉末、純度99.0%、平均粒徑0.5μm之氧化鋁(Al2O3)粉末、以及純度99.9%、平均粒徑0.2μm之氧化鈰(CeO2)粉末，以分別為Y：Al：Ce=3.98：2.00：0.02之莫耳比進行混合，得到1g之混合粉末。其次，將該混合粉末，在大氣環境中實施1400℃之4小時的燒結，得到單斜晶相單相組成之原料粉末(2-2)1g。
將該等原料粉末(1-1)及(2-2)，以攪拌器進行1小時混合，得到燒結用之原料粉末(2)。其次，將所得到之原料粉末(2)以1軸衝壓機實施衝壓成形後，以1750℃進行真空燒結，而得到緻密之燒結體。從所得到之燒結體切取長1.5mm、寬2.0mm、厚200μm之薄板狀之燒結體，並作為波長變換構件。
測定該波長變換構件之燒結密度時，係4.55g/cm3，氣孔率為0.1體積%。觀察該波長變換構件之剖面時，為氣泡較少之緻密的燒結體。此外，對該波長變換構件以XRD實施定性分析時，確認主相為YAG相(柘榴石相)而其餘為YAM相(單斜晶相)。更進一步，以電子顯微鏡觀察該波長變換構件之組織來進行EPMA分析時，確認平均粒徑約5μm之YAM相係以包含分散於YAG相之狀態存在於YAG相中。第3圖，係電子顯微鏡像及EPMA像。
以470nm之光激發所得到之波長變換構件時，波長變換構件之內部量子效率為0.92。此外，以470nm之點光源照射該波長變換構件時，在光源之照射面的相反側之面，得到無色澤不均一之發光。
[實施例3]
將純度99.9%、平均粒徑1.0μm之氧化釔(Y2O3)粉末、純度99.0%、平均粒徑0.5μm之氧化鋁(Al2O3)粉末、以及純度99.9%、平均粒徑0.2μm之氧化鈰(CeO2)粉末，以分別為Y：Al：Ce=2.99：5：0.01之莫耳比，利用攪拌器進行30分鐘混合，而得到混合粉末。其次，將此混合粉末，於大氣環境中實施1400℃、4小時之燒結，而得到柘榴石相單相組成之原料粉末(1-1)。
於該原料粉末(1-1)，以成為2000ppm之方式添加氧化矽粉末，以攪拌器進行1小時混合，得到燒結用之原料粉末(3)100g。其次，將所得到之原料粉末(3)以1軸衝壓機實施衝壓成形後，以1780℃進行真空燒結，得到緻密之燒結體。從所得到之燒結體切取長1.5mm、寬2.0mm、厚200μm之薄板狀之燒結體，並作為波長變換構件。
測定該波長變換構件之燒結密度時，係4.54g/cm3，氣孔率為0.2體積%。觀察該波長變換構件之剖面時，為氣泡較少之緻密的燒結體。此外，對該波長變換構件以XRD實施定性分析時，確認主相為YAG相(柘榴石相)而其餘為矽酸鹽相。更進一步，以電子顯微鏡觀察該波長變換構件之組織來進行EPMA分析時，確認平均粒徑約5μm之矽酸鹽相係以包含分散於YAG相之狀態存在於YAG相中。第4圖，係電子顯微鏡像及EPMA像。
以470nm之光激發所得到之波長變換構件時，波長變換構件之內部量子效率為0.92。此外，以470nm之點光源照射該波長變換構件時，在光源之照射面的相反側之面，得到無色澤不均一之發光。
[比較例1]
以與實施例1相同之方法，得到原料粉末(1-1)500g。其次，將所得到之原料粉末(2)以單軸衝壓機衝壓成形後，以1750℃進行真空燒結，而得到緻密之燒結體。從所得到之燒結體切取長1.5mm、寬2.0mm、厚200μm之薄板狀之燒結體，並作為波長變換構件。
測定該波長變換構件之燒結密度時，係4.55g/cm3，氣孔率為0.1體積%。此外，對該波長變換構件以XRD實施定性分析時，係柘榴石相。更進一步，以電子顯微鏡觀察該波長變換構件之組織來進行EPMA分析時，未觀察到柘榴石相以外之相。第5圖，係電子顯微鏡像及EPMA像。
以470nm之光激發所得到之波長變換構件時，波長變換構件之內部量子效率為0.90。此外，以470nm之點光源照射該波長變換構件時，在光源之照射面的相反側之面，只能得到色澤不均勻之發光。
第1圖係波長變換構件中，(B)相包含分散於(A)相之狀態的示意圖。
第2圖係實施例1所得到之波長變換構件之電子顯微鏡像及EPMA像。
第3圖係實施例2所得到之波長變換構件之電子顯微鏡像及EPMA像。
第4圖係實施例3所得到之波長變換構件之電子顯微鏡像及EPMA像。
第5圖係比較例1所得到之波長變換構件之電子顯微鏡像及EPMA像。

Claims (8)

  1. 一種波長變換構件，係包含著：(A)以下述組成式(1)(A1-xBx)3C5O12 (1)(式中，A係從Y、Gd及Lu所選取之1種類以上之稀土元素，B係從Ce、Nd及Tb所選取之1種類以上之稀土元素，C係從Al及Ga所選取之1種類以上之元素，x為0.002≦x≦0.2)所示之柘榴石相；及(B)從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相之多晶體的燒結陶瓷；其特徵為：(A)相中含有而分散著由(B)相所構成之微細結晶；該等相之狀態，係於柘榴石相((A)相)之結晶中，分散分佈著從鈣鈦礦相、單斜晶相及矽酸鹽相所選取之1種類以上之相((B)相)之微細結晶的構造，係不同之2種相所形成之海島構造的狀態。
  2. 如申請專利範圍第1項所述之波長變換構件，其中上述鈣鈦礦相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；以及氧。
  3. 如申請專利範圍第1或2項所述之波長變換構件 ，其中上述單斜晶相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；以及氧。
  4. 如申請專利範圍第1或2項所述之波長變換構件，其中上述矽酸鹽相，係含有：從Y、Gd及Lu所選取之1種類以上之稀土元素；從Ce、Nd及Tb所選取之1種類以上之稀土元素；從Al及Ga所選取之1種類以上之元素；矽；以及氧。
  5. 如申請專利範圍第1或2項所述之波長變換構件，其中由上述(B)相所構成之微細結晶的平均粒徑為0.1μm以上。
  6. 如申請專利範圍第1或2項所述之波長變換構件，其中燒結陶瓷之氣孔率為0.1體積%以下。
  7. 一種發光裝置，係利用如申請專利範圍第1至6項中任一項所述之波長變換構件的發光裝置，其特徵為：來自光源之光的一部分透射上述波長變換構件，且來自光源之光的一部分由上述波長變換構件進行波長變換並發光。
  8. 一種波長變換構件之製造方法，係用以製造如申 請專利範圍第1項所述之波長變換構件的方法，其特徵為：將以賦予(A)相之組成而含有(A)相所含有之各元素的原料粉末、及以賦予(B)相之組成而含有(B)相所含有之各元素的原料粉末進行混合，對所得到之混合粉末實施成形，且對所得到之成形體進行加熱並燒結。
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