TW201406929A - 波長轉換構件,其製法,及發光裝置 - Google Patents
波長轉換構件,其製法,及發光裝置 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 13
- 239000000758 substrate Substances 0.000 claims abstract description 77
- 239000012190 activator Substances 0.000 claims abstract description 76
- 239000000919 ceramic Substances 0.000 claims abstract description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910052727 yttrium Inorganic materials 0.000 claims description 12
- 229910052684 Cerium Inorganic materials 0.000 claims description 11
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910052765 Lutetium Inorganic materials 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 230000007423 decrease Effects 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 5
- 238000010304 firing Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 15
- 229910000420 cerium oxide Inorganic materials 0.000 description 13
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 13
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 11
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012764 semi-quantitative analysis Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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Abstract
一種波長轉換構件係藉由以下方式製備:將多晶體透明陶瓷基板的表面以活化劑塗佈及將經活化劑塗佈之陶瓷基板燃燒,為讓該活化劑從陶瓷基板的表面擴散至陶瓷基板中。
Description
本發明關於用於光源之波長轉換構件,使來自光源之光的一部分進行波長轉換,而使光的另一部分透射,使用該構件之發光裝置,及製備該構件之方法。
發光二極體為目前可取得之最有效率的光源之一。近年來藉由組合藍色LED與磷光體而積極致力於發展白色發光裝置。例如,JP-A 2007-150331揭示包含柘榴石或類似者的波長轉換構件,尤其為能夠使發光組件所發射之光進行波長轉換的均勻透光之波長轉換構件,及包含波長轉換構件之發光裝置。波長轉換構件被預期具有比包含磷光體和磷光體分散於其中的樹脂之先前技術的波長轉換層更高的耐熱性和更高的機械強度,且亦被預期具有對抗隨著發光組件輸出增加而增加的熱之耐久性。
一種製造此一波長轉換構件之已知方法為調配具有與波長轉換構件相同的成分元素組成之原料、成形、機械施
工及在高溫下燒結。
專利文件1:JP-A 2007-150331
(US 7514721、EP 1958269)
本發明的目的係提供一種與先前技術方法不同的方式製造波長轉換構件之方法,所製得之波長轉換構件,及使用該構件之發光裝置。
根據本發明,用於使光源所發射之光進行波長轉換的構件(亦即波長轉換器)係由以下方式製造:預先製備具有與最終構件相同的組成(除了活化劑以外)之透光基板,將基板表面以活化劑塗佈及使基板持續在熱氛圍中,為讓活化劑擴散至基板中。
建構波長轉換構件之基板或基質可為透光之氧化鋁、透光之釔鋁柘榴石(YAG)、透光之鎦鋁柘榴石或類似者。此等基板比較容易取得。而且通常使用Tb、Eu和Ce之氧化物作為使該等材料轉變成螢光材料之活化劑,該等氧化物亦比較容易取得。然而,具有特定含量之活化劑的波長轉換構件不容易取得。
本發明者發現波長轉換構件的製造可以比較容易取得的透明陶瓷基板開始,以活化劑塗佈基板及讓活化劑在高溫下擴散。
在一個態樣中,本發明提供一種製備波長轉換構件之方法,其包含以下步驟:將多晶體透光陶瓷基板的表面以活化劑塗佈,及將經活化劑塗佈之陶瓷基板燃燒,為讓活化劑從陶瓷基板的表面擴散至陶瓷基板中。
多晶體透明陶瓷基板通常具有Y3Al5O12、Lu3Al5O12、(Y,Lu)3Al5O12、(Y,Gd)3Al5O12或Al2O3之組成。活化劑亦通常為鈰、銪或鋱之氧化物。
燃燒步驟較佳地在1,000至1,800℃之溫度下。
在另一態樣中,本發明提供一種包含多晶體透光陶瓷基板之波長轉換構件,其中有一活化劑已從陶瓷基板的表面擴散,陶瓷基板係由多晶體粒建構,且活化劑之濃度分配係以晶粒邊界附近比晶粒中心高。
在較佳的具體例中,圍繞各晶粒之活化劑具有使得濃度從晶粒邊界向晶粒中心減少的濃度分配。
在更佳的具體例中,在陶瓷基板內部之活化劑具有使得在厚度方向的濃度從基板表面至深度逐漸減少的濃度分配。
多晶體透明陶瓷基板通常具有Y3Al5O12、Lu3Al5O12、(Y,Lu)3Al5O12、(Y,Gd)3Al5O12或Al2O3之組成。活化劑亦通常為鈰、銪或鋱之氧化物。
本文亦涵蓋包含上文定義之波長轉換構件的發光裝置。
根據本發明,具有任意的活化劑添加於其中的波長轉換構件可使用比較容易取得的透明陶瓷基板製造。
在本文所使用之透明陶瓷基板較佳地選自Y3Al5O12、Lu3Al5O12、(Y,Lu)3Al5O12、(Y,Gd)3Al5O12及Al2O3之中。該等透明陶瓷比較容易取得,因為該等被廣泛地用作為除了本文涵蓋的波長轉換器應用以外的光學和結構材料。以先前技術的方法,當該等材料被用作為波長轉換構件之基板時,其中活化劑類型和濃度受到限制的特定尺寸之透明陶瓷基板係以順從特別的應用而製備。從此方法所製備之波長轉換構件來產生所欲發射特性之嘗試失敗了,即使尺寸和活化劑濃度僅稍微偏離指定的值。因此有必要嚴格控制活化劑濃度和波長轉換構件尺寸。
在用於部分或全部可見光或紫外光之波長轉換的構件範圍內,如所涉及之白色LED的情況中,希望製造具有不同濃度的活化劑之構件。為此目的,必須在成形及燒結之前調配具有特定濃度的活化劑之混合原料。為了符合此需求,必須提供許多具有不同濃度的活化劑之原料。為了從此波長轉換構件獲得所欲特性,波長轉換構件必須以精確的機械施工技術加工成特定尺寸。為了避免這些製造難度,可能希望是否可以控制透明陶瓷中的活化劑量而不受基板類型及機械施工尺寸的支配。本發明提供在此方面超
越先前技術方法之製造方法。
因為透明陶瓷材料(諸如Y3Al5O12、Lu3Al5O12、(Y,Lu)3Al5O12、(Y,Gd)3Al5O12及Al2O3)具有固定的組成,所以比較容易由其製備單一尺寸的基板。關於該等陶瓷材料之製法,例如JP 2866891詳細說明Y3AI5O12陶瓷材料之製法。根據吾等的發明,活化劑係藉由以活化劑塗佈陶瓷基板的表面及讓活化劑擴散至陶瓷基板中而引入此透明陶瓷材料中。在本文所使用之透明陶瓷基板必須由多晶體粒建構。這是因為活化劑係沿著晶粒邊界擴散至內部及進一步擴散至晶體粒中。若陶瓷基板為單晶體,則活化劑不可能以足夠行使波長轉換器功能的量引入陶瓷基板中。使活化劑擴散至透明陶瓷基板的所欲措施係將經活化劑塗佈之陶瓷基板表面在高溫下徐冷。
在本文所使用之活化劑典型地選自稀土元素及/或其稀土氧化物之中,尤其為鈰、銪和鋱之氧化物。
當活化劑塗覆於陶瓷基板時,活化劑可為任何形式之氧化物粒子、金屬箔、經蒸氣沉積之氧化物、無機鹽、有機鹽、複合物或類似者,只要可在陶瓷基板上形成均勻的塗層。一種較佳的塗佈程序如下:將氧化物粒子或類似者分散在溶劑(諸如水或醇)中,將分散液塗覆於陶瓷基板及經由蒸發或類似者移除溶劑。另一選擇地,可將活化劑以噴濺或真空蒸發而沉積或塗覆於陶瓷基板。
作為活化劑的塗佈重量較佳地在3×10-6莫耳/平方公分至3×10-5莫耳/平方公分之範圍內。若塗佈重量少於3×
10-6莫耳/平方公分,則有效擴散的活化劑量太少而不能提供作為發光陶瓷材料的所欲性能。若塗佈重量超過3×10-5莫耳/平方公分,則在高溫燃燒期間可能發生活化劑單獨在表面上燒結或活化劑與基板表面附近反應,產生阻礙活化劑擴散至基板中的複合物,無法達成有效的活化劑擴散。
當活化劑的塗佈重量係在上述範圍內改變時,可控制陶瓷的螢光效率,甚至當以相同的藍色LED照射時。例如,假設光轉換構件係藉由以氧化鈰均勻地塗佈透光之YAG及接著徐冷而製造,以較少的氧化鈰塗佈重量所製得之光轉換構件在以藍色LED照射時供給較低比例的黃色光轉換及因此供給具有高色溫的發光。當氧化鈰塗佈重量增加時,則發光整個轉變為暖色。根據本發明,波長轉換構件的發光色可藉由改變活化劑的塗佈重量而變化。此有利於消除波長轉換構件進行精確的機械施工之必要性。
可將塗佈於陶瓷基板之活化劑乾燥,在或低於800℃下煅燒或在塗佈後以其他方式處理,其係取決於活化劑的形式而定。
接著將以活化劑塗佈之透明陶瓷基板在高溫下加熱,為讓活化劑從陶瓷基板的表面擴散至陶瓷基板中。雖然適合於活化劑擴散的燃燒溫度係隨陶瓷和活化劑二者的類型而改變,但是燃燒溫度較佳地在1,000至1,800℃之範圍內,更佳為1,500至1,700℃,而甚至更佳為1,600至1,700℃。低於1,000℃之溫度可能不足以讓活化劑擴散至
陶瓷基板中,而超過1,800℃之溫度可能引起陶瓷基板本身變形。在上述任一情況中,獲得滿意的波長轉換構件之難度可能提高。燃燒氛圍可為空氣、減壓氛圍或真空氛圍,雖然此選擇係取決於活化劑類型而定。可在燃燒後再於高溫下進行熱處理。燃燒時間通常為1至24小時,較佳為3至15小時,而更佳為5至12小時。
活化劑擴散至透明陶瓷基板中首先係沿著陶瓷基板內的晶粒邊界發生。隨後活化劑進一步從晶粒邊界擴散至晶粒內部。因為活化劑係沿著陶瓷基板內的晶粒邊界擴散,所以晶粒邊界附近的濃度比晶粒中心高。圍繞各晶粒之活化劑亦具有使得濃度可從晶粒邊界向晶粒中心減少的濃度分配。
活化劑的擴散深度通常在50至600微米之範圍內,雖然其係取決於陶瓷類型、晶體粒尺寸、活化劑類型、燃燒溫度和燃燒時間而定。在陶瓷基板內,活化劑具有使得在厚度方向的濃度可從基板表面至深度逐漸減少的濃度分配。
具有活化劑擴散於其中的透明陶瓷基板可以移除未擴散之活化劑為目的而在經活化劑塗佈之表面進行研磨,或以增加粗糙度來改進光擴散或透光率為目的而以噴砂或類似者進行粗糙化。
因此製造之波長轉換構件具有高的透明度及螢光效率。
如此徐冷之陶瓷基板具有平坦且光滑的表面。在以
BEI觀察的橫截面上,使活化劑沿著基板內的晶粒邊界擴散之區域被證實從表面穿越有限的狹窄範圍。此活化劑擴散區域的厚度及活化劑擴散狀態在陶瓷基板表面上的每個地區皆為均勻的。經證實從藍色LED之光激發出螢光。
圖1為在活化劑(氧化鈰)之擴散處理後的透光之YAG陶瓷板的橫截面顯微照片。
圖2例示在擴散處理後的表面附近之元素分配。
在下文以例示方式而非限制方式提出本發明的實例。
將1公克具有200奈米平均粒徑之氧化鈰粒子加入20公克丙烯酸乳液(Daido Chemical Corp.之Vinyzol 1020)中,將其在35kHz下經超音波處理30分鐘,獲得氧化鈰分散液。
將具有99.99%之純度及在450奈米波長下具有75%之線性透光率的透光之YAG陶瓷板(50.8×50.8×1毫米)製備成基板。將氧化鈰分散液噴霧塗佈在基板表面上及在120℃之烘箱中乾燥,以形成在基板表面上的氧化鈰塗層。測量經塗佈之基板重量,測得81.3毫克的增重,其相當於3.15毫克/平方公分之每單位表面積的氧化鈰塗佈
重量。將塗佈之基板在空氣中於600℃下煅燒且在1,650℃下於98%之Ar與2%之氫氣的混合氣體氛圍中燃燒5小時,完成波長轉換構件。
以SEM觀察依此燃燒的波長轉換構件之橫截面,發現鈰係沿著晶粒邊界擴散。擴散距離為從表面至約100微米深度。
當以450奈米波長之光照射時,波長轉換構件發射具有在~552奈米波長之波峰的光。
圖1例示以SEM(BEI×2000)所觀察在活化劑(氧化鈰)的擴散處理後的透光之YAG陶瓷板的橫截面。表1顯示在圖1中的表面白色部位P1和灰色部位P2及YAG陶瓷(燒結體)之半定量測定值。
應注意與定量分析不同的半定量分析包含從光譜數據的定量校正。特定言之,半定量測定值係由以下方式獲得:以定性分析軟體鑑定元素,以經鑑定之元素為基準從定性光譜測定波峰背景強度,計算強度對純元素之特性X-射線強度之比,及由此進行校正。
圖2例示在擴散處理後的表面附近之元素分配。
將氧化鈰粒子使用磁控管噴濺系統塗佈在具有99.99%之純度及在450奈米波長下具有75%之線性透光率的透光之YAG陶瓷板(1毫米厚度)表面上。以SEM觀察板的橫截面,發現在表面上形成15微米氧化鈰塗層。將經氧化鈰塗佈之YAG陶瓷板在1,650℃下於98%之Ar與2%之氫氣的混合氣體氛圍中燃燒5小時。將依此燃燒的經氧化鈰塗佈之陶瓷板表面以膠態氧化矽磨光,完成波長轉換構件。
以SEM觀察波長轉換構件之橫截面,發現鈰係沿著晶粒邊界於整個表面上擴散,如實例1。當以450奈米波長之光照射時,波長轉換構件發射具有在~552奈米波長之波峰的光。
將1公克具有200奈米平均粒徑之氧化鈰粒子插入20公克去離子水及丙烯酸乳液(Daido Chemical Corp.之Vinyzol 1020)中,將其在35kHz下經超音波處理30分鐘,獲得氧化鈰分散液。
將具有99.99%之純度及在450奈米波長下具有75%之線性透光率的透光之YAG陶瓷板(50.8×50.8×1毫米)製備成基板。將氧化鈰分散液噴霧塗佈在基板表面上及在120℃之烘箱中乾燥,以形成在基板表面上的氧化鈰塗
層。測量經塗佈之基板重量,測得105毫克的增重,其相當於4.01毫克/平方公分之每單位表面積的氧化鈰塗佈重量。當以450奈米波長之光照射時,所得構件不產生螢光。
Claims (10)
- 一種製備波長轉換構件之方法,其包含以下步驟:將多晶體透明陶瓷基板的表面以活化劑塗佈,及將經活化劑塗佈之陶瓷基板燃燒,為讓該活化劑從陶瓷基板的表面擴散至陶瓷基板中。
- 根據申請專利範圍第1項之方法,其中該多晶體透明陶瓷基板具有Y3Al5O12、Lu3Al5O12、(Y,Lu)3Al5O12、(Y,Gd)3Al5O12或Al2O3之組成。
- 根據申請專利範圍第1項之方法,其中該活化劑為鈰、銪或鋱之氧化物。
- 根據申請專利範圍第1項之方法,其中該燃燒步驟係在1,000至1,800℃之溫度下。
- 一種包含多晶體透明陶瓷基板之波長轉換構件,其中有一活化劑已從該陶瓷基板的表面擴散,該陶瓷基板係由多晶體粒建構,且該活化劑之濃度分配係以晶粒邊界附近比晶粒中心高。
- 根據申請專利範圍第5項之波長轉換構件,其中圍繞各晶粒之該活化劑具有使得濃度從晶粒邊界向晶粒中心減少的濃度分配。
- 根據申請專利範圍第5項之波長轉換構件,其中在陶瓷基板內部之該活化劑具有使得在厚度方向的濃度從基板表面至深度逐漸減少的濃度分配。
- 根據申請專利範圍第5項之波長轉換構件,其中該多晶體透明陶瓷基板具有Y3Al5O12、Lu3Al5O12、 (Y,Lu)3Al5O12、(Y,Gd)3Al5O12或Al2O3之組成。
- 根據申請專利範圍第5項之波長轉換構件,其中該活化劑為鈰、銪或鋱之氧化物。
- 一種發光裝置,其包含根據申請專利範圍第5項之波長轉換構件。
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