TW201608007A - 近紅外光發光二極體及其製造方法 - Google Patents
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Abstract
本發明係關於一種近紅外光發光二極體及其製造方法,其在製備近紅外光發光二極體之發光層時,係將CsSnXX’2
溶液塗布於具有電洞傳輸層之基板上,然後經乾燥處理而使溶劑脫離,讓CsSnXX’2
溶液固化並結晶為具鈣鈦礦結構之CsSnXX’2
,以作為近紅外光發光二極體之發光層,得發出近紅外光;其中,X以及X’係為相同或不相同之鹵素元素。另外,本發明也可使用鉛替換部分之錫,利用調整鉛/錫之比例或是使用不同之鹵素元素組合,而使產生的近紅外光波長有所變化。
Description
本發明係關於一種發光二極體及其製造方法,尤指一種可不使用複雜之化學合成方法或是稀有元素,而得透過簡易的方法形成,並且可發出近紅外光之近紅外光發光二極體及其製造方法。
近紅外光技術在國防工業、地質探測、光纖通信、環境監控、生物成像、食品醫藥、農業檢測等領域都扮演著重要角色。而近紅外光技術發展關鍵的係在於材料的研製與發光元件之製作。由於近紅外發光二極體具有體積小、耗能低、穩定性高以及壽命長等優點,因此是近紅外技術於落實應用時的重要媒介。
在一般應用上,近紅外光發光二極體隨處可見,例如遙控器、商店的自動門之外,在資訊的傳輸與儲存、光纖通訊等領域也有近紅外光發光二極體的身影。而在夜間監視器上的近紅外光光源也是近紅外光發光二極體的應用,雖然人眼無法感受到近紅外光,但其可以被相機或攝影機所感測到,也因此常用於夜間或亮度不足之場所的補充光源,使監視器攝影機可以拍到影像。
而除了上述之夜視或光通訊等應用之外,近紅外光發光二極體也可應用於生醫領域,例如將近紅外光發光二極體所發出的近紅外光照射於使用者的皮膚,再利用光譜偵測儀接收反射光,經過計算以評估使用者的血糖值,作為非侵入式血糖儀之應用,或是用於治療皮膚疾病。
不過近紅外光發光二極體在製作上,其發光材料只有極少具有可溶解性,且大多需要透過複雜的化學方法合成,或者是透過複雜的方法合成不同粒徑之量子點材料,而其中還多含有金屬鉛,不符合環保的要求。另外,其製程中大多需要高昂的真空製程設備,製程門檻可說相當高。
中國專利申請號CN 200780017078.2曾揭露一種在可見區或近紅外區中發光的發光材料,其係將無水之SnI2
與CsI在標準罐模機中混合,然後碾磨1~24小時,兩者之比例配製為1wt%~99wt%,其碾磨後的成品經測試可作為近紅外區之光致發光材料。對此,其所採用之材料係為一種具潛力之近紅外光發光二極體之發光層材料,但其技術內容距離作為可行之發光二極體發光層尚遠,也還需要在發光層的製作方法上進行進一步的研究。
因此,基於近紅外光發光二極體應用範圍廣泛但製作不易之背景條件,本發明針對近紅外光發光二極體之發光層之組成及製作方法進行創新開發和改良。
本發明之主要目的,係提供一種近紅外光發光二極體之製造方法,其在使用相關材料進行溶液配製並塗布後,直接透過抽乾、烘乾等乾燥方式就形成固態之膜層,以作為發光層,方法簡單且有效。
本發明之次要目的,係提供一種近紅外光發光二極體之製造方法,其可將所配製之溶液經由稀釋之手段進行濃度調整,因而在乾燥後形成不同厚度之發光層,係為調控發光層特性之新穎手段。
本發明之另一目的,係提供一種近紅外光發光二極體之製造方法,其透過配製特定之溶液後再進行抽乾,其經固化結晶而形成之發光層在結構上具有鈣鈦礦結構(perovskite),係為讓電子與電洞於此複合而發出波長約710~950nm之近紅外光之關鍵。
本發明之再一目的,係提供一種近紅外光發光二極體,其發光層之材質不含有汞、鎘、鉻、鈷、鎳或砷等重金屬,且可選擇性地使用鉛作為調整發光波長之技術手段,較具有環保性質。而除了使用鉛,也可利用不同之鹵素元素之組合而改變光色。
為了達到上述之目的,本發明揭示了一種近紅外光發光二極體之製造方法,若以不含鉛的方法為一典型之實施例,該近紅外光發光二極體係包含一發光層,其特徵在於該發光層之形成係包含步驟:混合一第一粉末、一第二粉末以及一溶劑,形成CsSnXX’2
溶液,該第一粉末係為CsX,該第二粉末係為SnX’2
,X以及X’係為鹵素元素;塗布該CsSnXX’2
溶液於一基板上;以及乾燥該CsSnXX’2
溶液,使該CsSnXX’2
溶液固化並結晶為具鈣鈦礦結構之CsSnXX’2
,其係為該發光層。
10‧‧‧基板
20‧‧‧電洞傳輸層
30‧‧‧發光層
40‧‧‧電子傳輸層
50‧‧‧電極層
S1~S3‧‧‧步驟
A‧‧‧Cs
B‧‧‧Sn
C‧‧‧I
20‧‧‧電洞傳輸層
30‧‧‧發光層
40‧‧‧電子傳輸層
50‧‧‧電極層
S1~S3‧‧‧步驟
A‧‧‧Cs
B‧‧‧Sn
C‧‧‧I
第1圖:其係為本發明一較佳實施例之結構示意圖;
第2圖:其係為本發明一較佳實施例之步驟流程圖;
第3圖:其係為本發明一較佳實施例中,發光層之鈣鈦礦結構示意圖;以及
第4A~4C圖:其係為本發明一較佳實施例之發光層之顯微鏡視圖,用以表示不同濃度之CsSnI3 溶液經抽乾而乾燥後所形成之發光層。
為使本發明之特徵及所達成之功效有更進一步之瞭解與認識,謹佐以較佳之實施例及配合詳細之說明,說明如後:
首先請參考第1圖,本發明所製造之近紅外光發光二極體在結構上係包含了:基板10、電洞傳輸層20、發光層30、電子傳輸層40以及電極層50。其中,電洞傳輸層20係設置於基板10之上,發光層30係設置於電洞傳輸層20之上,電子傳輸層40係設置於發光層30之上,而電極層50則係設置於電子傳輸層40之上。
基於上述的結構,本發明之近紅外光發光二極體於運作時,電洞可以經由電洞傳輸層20注入發光層30材料的價電帶,而電子則可以經由電極層50注入電子傳輸層40材料的導電帶。由於電子傳輸層40材料的導電帶的能階較發光層30材料的導電帶為高,因此電子傳輸層40中的電子可以再傳輸到發光層30的導電帶。而當發光層30當中發生電子與電洞複合時,則基於其材料係為具鈣鈦礦結構之Cs(Sny
Pb1-y
)X3-Z
X’z
,其中X以及X’係為相同或不相同之鹵素元素,而0<y≦1,0≦z≦3。若所形成之發光層係為CsSnI3
,其發光波長約為950 nm;但由於CsPbI3
的發光波長約為710~720 nm之紅光,因此鉛的加入得以作為調整光色的媒介,可透過控制鉛的摻入量來調整本發明之近紅外光發光二極體的發光波長是落於710~950nm之範圍,隨著鉛的摻入量增加,其波長越偏向710nm,接近近紅外光之波長下限。而除了利用錫/鉛之比例改變光色,本發明在使用之不同之鹵素元素,或者是改變鹵素元素之組合,也可讓近紅外光之波長產生改變,達到調整光色之目的。
而在製造本發明之近紅外光發光二極體之方法上,其係先準備具有已圖案化銦錫氧化物(Indium Tin Oxide,ITO)之基板。這種具有已圖案化ITO之玻璃基板因為於保存和蝕刻的過程有殘留油漬、灰塵、光阻和水分於其表面,因此在設置電洞傳輸層之前,需先將之表面清洗乾淨。其清洗流程係包含:(1)將具有已圖案化ITO之玻璃基板浸泡至丙酮溶劑當中,並且置放在超音波震盪機震盪10分鐘。(2)將步驟(1)的基板改浸泡於異丙醇中,並放置在超音波震盪機震盪10分鐘。(3)將步驟(2)的基板改浸泡於去離子水中,並放置在超音波震盪機震盪10分鐘。(4)將基板取出並在無塵室工作臺以氮***吹乾,並放置於紫外線-臭氧機當中曝照30分鐘,以再進行後續之層面塗布處理。
基板上之電洞傳輸層係透過旋轉塗布的方式,將導電高分子聚(3,4-乙烯二氧噻吩)(PEDOT)以及聚苯乙烯磺酸(PSS)之混合物塗布於基板之上,並以120℃烘烤20分鐘。
接著,再於電洞傳輸層上設置發光層,請參考第2圖,本發明於形成發光層時,以製作不含鉛的發光層為例,係包含步驟:
步驟S1:混合第一粉末、第二粉末以及溶劑,形成CsSnXX’2 溶液,該第一粉末係為CsX,該第二粉末係為SnX’2 ,X以及X’係為鹵素元素;
步驟S2:塗布前述之CsSnXX’2 溶液於電洞傳輸層上;以及
步驟S3:乾燥前述之CsSnXX’2 溶液,使前述之CsSnXX’2 溶液固化並結晶為具鈣鈦礦結構之CsSnXX’2 ,其係為發光層。
步驟S1:混合第一粉末、第二粉末以及溶劑,形成CsSnXX’2 溶液,該第一粉末係為CsX,該第二粉末係為SnX’2 ,X以及X’係為鹵素元素;
步驟S2:塗布前述之CsSnXX’2 溶液於電洞傳輸層上;以及
步驟S3:乾燥前述之CsSnXX’2 溶液,使前述之CsSnXX’2 溶液固化並結晶為具鈣鈦礦結構之CsSnXX’2 ,其係為發光層。
在本發明的一較佳實施例中,係使用CsI為第一粉末,SnI2
為第二粉末,而實際操作之用量則為0.2054g之CsI以及0.2946g之SnI2
,也就是兩者皆約為0.0008莫耳的量,與溶劑進行混合。本發明所使用之溶劑係為多個溶劑的混合物,此混合物中含有甲氧基乙腈(methoxyactonitrile,MOAN)、二甲基甲醯胺(dimethylformamide,DMF)以及乙腈(acetonitrile,AN),三者的比例係為1:3:2。經混合第一粉末、第二粉末以及溶劑後,此操作實例係得到濃度約為330mg/ml之CsSnI3
溶液。
前述操作實例係以CsI為第一粉末、SnI2
為第二粉末,而若將碘替換為其他鹵素元素,例如氟、氯、溴以及砈也是可行,而錫則是可用鉛取代,並且兩者可同時混用,例如將部分之第二粉末SnI2
以第三粉末PbI2
取代,但第一粉末之莫耳數仍與第二粉末以及第三粉末之莫耳數和相同。以使用相同之鹵素元素X為例,當第一粉末為CsX,第二粉末為SnX2
,第三粉末為PbX2
時,經前述步驟將第一粉末、第二粉末、第三粉末以及溶劑混合後,可形成Cs(Sny
Pb1-y
)X3
溶液,其中0<y<1。而若使用不同的鹵素元素,例如第一粉末為CsX,第二粉末為SnX2
或SnX’2
,第三粉末為PbX2
或PbX’2
,X以及X’係為不相同之鹵素元素,則可在與溶劑混合後,形成Cs(Sny
Pb1-y
)X3-Z
X’z
溶液,其中0<y<1,0<z<2。而無論是形成CsSnXX’2
溶液、Cs(Sny
Pb1-y
)X3
溶液或Cs(Sny
Pb1-y
)X3-Z
X’z
溶液,其主要差異僅在於所用以製備之具鈣鈦礦結構之發光層係具有不同的發光波長,但皆為近紅外光,使用者可依鉛的摻入量對波長值進行調整。
經前述列舉之步驟S1操作而形成CsSnXX’2
溶液(下以實際操作之CsSnI3
溶液為例)後,其在塗布於電洞傳輸層上之前,可先將CsSnI3
溶液進行稀釋處理,使其濃度降低至15~70mg/ml,然後再利用旋轉塗布(2500~3500rpm)、刮刀塗布或澆注(drop cast)的方式,將CsSnI3
溶液均勻地塗布在電洞傳輸層之上。接著以抽乾或是烘乾等乾燥方式促使溶劑脫離,使CsSnI3
溶液固化並結晶為具有鈣鈦礦結構之CsSnI3
,此即為本發明之發光層。請參考第3圖,其係為本發明之發光層於此實施例形成立方晶系之鈣鈦礦結構之示意圖,其中的元素A、B、C分別代表Cs、Sn以及I。
另請參考第4A~4C圖,其係分別將調配之CsSnI3
溶液稀釋為16.6mg/ml、33mg/ml、66mg/ml等濃度後,以澆注法塗布於電洞傳輸層之上之顯微鏡視圖,可見發光層之厚度係受CsSnI3
溶液之濃度影響而在抽乾後有所不同。
待形成具鈣鈦礦結構之CsSnI3
作為發光層之後,接著將2-(4-biphenylyl)-5-(4-tert-butylphenyl)1,3,4-oxadiazole (PBD)溶液以旋轉塗布的方式均勻覆蓋成膜於發光層之上,作為電子傳輸層。
最後,再將氟化鋰/鋁蒸鍍於電子傳輸層之上,作為電極層,其係為本發明之近紅外光發光二極體的陰極。
經上述步驟處理而形成之膜層堆疊即為本發明之近紅外光發光二極體,其透過具鈣鈦礦結構之CsSnI3
或是上述其他可行之化學組成作為發光層,可讓在此層面複合之電子電洞對視鉛之摻入比例而發出波長約為710~950nm之近紅外光。利用這種方法所製備之近紅外光發光二極體可進一步作為夜視、光通訊、生醫領域等應用。綜上所述,本發明詳細揭露了一種近紅外光發光二極體及其製造方法,基於其低成本特質以及操控條件上的簡易性的,本發明無疑是一種兼具經濟和實用價值之近紅外光發光二極體及其製造方法。
惟以上所述者,僅為本發明之較佳實施例而已,並非用來限定本發明實施之範圍,舉凡依本發明申請專利範圍所述之形狀、構造、特徵及精神所為之均等變化與修飾,均應包括於本發明之申請專利範圍內。
S1~S3‧‧‧步驟
Claims (16)
- 【第1項】一種近紅外光發光二極體之製造方法,該近紅外光發光二極體係包含一發光層,其特徵在於該發光層之形成係包含步驟:
混合一第一粉末、一第二粉末以及一溶劑,形成CsSnXX’2 溶液,該第一粉末係為CsX,該第二粉末係為SnX’2 ,X以及X’係為鹵素元素;
塗布該CsSnXX’2 溶液於一基板上;以及
乾燥該CsSnXX’2 溶液,使該CsSnXX’2 溶液固化並結晶為具鈣鈦礦結構之CsSnXX’2 ,其係為該發光層。 - 【第2項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中X以及X’係為相同之鹵素元素。
- 【第3項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中X以及X’係為不同之鹵素元素。
- 【第4項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中該溶劑係為甲氧基乙腈、二甲基甲醯胺以及乙腈之混合物。
- 【第5項】如申請專利範圍第4項所述之近紅外光發光二極體之製造方法,其中該溶劑之甲氧基乙腈、二甲基甲醯胺以及乙腈之比例係為1:3:2。
- 【第6項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中該第一粉末以及該第二粉末之莫耳數係為相同。
- 【第7項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中於塗布該CsSnXX’2 溶液於該基板上之步驟之前,更包含步驟:
稀釋該CsSnXX’2 溶液。 - 【第8項】如申請專利範圍第7項所述之近紅外光發光二極體之製造方法,其中於稀釋該CsSnXX’2 溶液之步驟中,係將該CsSnXX’2 溶液濃度稀釋至15~70mg/ml。
- 【第9項】如申請專利範圍第1項所述之近紅外光發光二極體之製造方法,其中於塗布該CsSnXX’2 溶液於該基板上之步驟中,係使用旋轉塗布法、刮刀塗佈法或澆注法。
- 【第10項】如申請專利範圍第9項所述之近紅外光發光二極體之製造方法,其中該旋轉塗布法之轉速係為2500~3500rpm。
- 【第11項】一種近紅外光發光二極體之製造方法,該近紅外光發光二極體係包含一發光層,其特徵在於該發光層之形成係包含步驟:
混合一第一粉末、一第二粉末、一第三粉末以及一溶劑,形成Cs(Sny Pb1-y )X3 溶液,該第一粉末係為CsX,該第二粉末係為SnX2 ,該第三粉末係為PbX2 ,X係為鹵素元素,0<y<1;
塗布該Cs(Sny Pb1-y )X3 溶液於一基板上;以及
乾燥該Cs(Sny Pb1-y )X3 溶液,使該Cs(Sny Pb1-y )X3 溶液固化並結晶為具鈣鈦礦結構之Cs(Sny Pb1-y )X3 ,其係為該發光層。 - 【第12項】如申請專利範圍第11項所述之近紅外光發光二極體之製造方法,其中該第一粉末之莫耳數係與該第二粉末與該第三粉末之莫耳數和相同。
- 【第13項】一種近紅外光發光二極體之製造方法,該近紅外光發光二極體係包含一發光層,其特徵在於該發光層之形成係包含步驟:
混合一第一粉末、一第二粉末、一第三粉末以及一溶劑,形成Cs(Sny Pb1-y )X3-Z X’z 溶液,該第一粉末係為CsX,該第二粉末係為SnX2 或SnX’2 ,該第三粉末係為PbX2 或PbX’2 ,X以及X’係為不相同之鹵素元素,0<y<1,0<z<2;
塗布該Cs(Sny Pb1-y )X3-Z X’z 溶液於一基板上;以及
乾燥該Cs(Sny Pb1-y )X3-Z X’z 溶液,使該Cs(Sny Pb1-y )X3-Z X’z 溶液固化並結晶為具鈣鈦礦結構之Cs(Sny Pb1-y )X3-Z X’z ,其係為該發光層。 - 【第14項】一種近紅外光發光二極體,其係包含:
一基板;
一電洞傳輸層,係設置於該基板之上;
一發光層,係設置於該電洞傳輸層之上,其係為具鈣鈦礦結構之Cs(Sny Pb1-y )X3-Z X’z ,X以及X’係為鹵素元素,0<y≦1,0≦z≦3;
一電子傳輸層,係設置於該發光層之上;以及
一電極層,係設置於該電子傳輸層之上。 - 【第15項】如申請專利範圍第14項所述之近紅外光發光二極體,其中X以及X’係為相同之鹵素元素。
- 【第16項】如申請專利範圍第14項所述之近紅外光發光二極體,其中X以及X’係為不相同之鹵素元素。
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TWI626768B (zh) * | 2016-08-01 | 2018-06-11 | 國立成功大學 | 發光二極體及其製造方法 |
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TWI593134B (zh) * | 2016-05-19 | 2017-07-21 | Method and structure for manufacturing graphene quantum dot on light-emitting diode | |
KR102586044B1 (ko) | 2016-08-10 | 2023-10-10 | 삼성디스플레이 주식회사 | 발광 소자 |
CN106229424B (zh) * | 2016-08-23 | 2019-05-03 | 陕西师范大学 | 一种基于钙钛矿薄片的发光器件及其制备方法 |
KR20180090116A (ko) * | 2017-02-02 | 2018-08-10 | 삼성전자주식회사 | 광 필터 및 이를 포함하는 광 분광기 |
CN107195710A (zh) * | 2017-05-31 | 2017-09-22 | 苏州大学 | 一种基于一步法制备高发光效率无机钙钛矿薄膜的方法 |
CN109216517B (zh) * | 2017-06-29 | 2020-11-27 | 苏州新纳晶光电有限公司 | 一种提高led波长命中率的处理方法 |
CN108417676B (zh) * | 2018-02-09 | 2019-05-17 | 郑州大学 | 基于等离子体增强效应的核壳结构钙钛矿led及其制备方法 |
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WO2007109734A2 (en) * | 2006-03-21 | 2007-09-27 | Ultradots, Inc. | Luminescent materials that emit light in the visible range or the near infrared range |
US20100072374A1 (en) * | 2008-03-31 | 2010-03-25 | Stc.Unm | Lead-iodide-based scintillator materials |
EP2510073B1 (en) * | 2009-12-08 | 2017-07-05 | Omnipv, Inc. | Luminescent materials that emit light in the visible range or the near infrared range and methods of forming thereof |
US8529797B2 (en) * | 2011-06-01 | 2013-09-10 | Kai Shum | Perovskite semiconductor thin film and method of making thereof |
US8840809B2 (en) * | 2011-06-01 | 2014-09-23 | Kai Shum | Solution-based synthesis of CsSnI3 thin films |
US9196482B2 (en) * | 2011-06-01 | 2015-11-24 | Kai Shum | Solution-based synthesis of CsSnI3 |
US9181475B2 (en) * | 2012-02-21 | 2015-11-10 | Northwestern University | Photoluminescent compounds |
US8901547B2 (en) * | 2012-08-25 | 2014-12-02 | Polyera Corporation | Stacked structure organic light-emitting transistors |
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TWI626768B (zh) * | 2016-08-01 | 2018-06-11 | 國立成功大學 | 發光二極體及其製造方法 |
US10497882B2 (en) | 2016-08-01 | 2019-12-03 | National Cheng Kung University | Light emitting diode and method of fabricating the same |
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