TWI470822B - 藉由粗糙化而改善光取出之發光二極體 - Google Patents
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Description
本發明係關於發光二極體,且特別地關於增強光取出之新LED結構。
發光二極體(LEDs)係一轉換電能為光波的重要固態裝置之類別。LEDS通常提供夾於兩對向摻雜層(doped layers)之間的半導體材料活性層。當施加偏壓通過摻雜層,電洞及電子即被射入該活性層,於此處其再結合以產生光波。由活性區域所產生的光波沿全部方向放射並且經由所有暴露表面而自半導體晶片逸出(escape)。
由於半導體材料已加以改良,故半導體裝置的效能亦已改善。新的LEDs正由InAlGaN這一類的材料來製成,其允許在紫外光至黃褐光光譜中之有效發光。相較於習知光源,許多新LEDs在將電能轉換成光波時更有效率且更加穩定可靠。因為LEDs的改善,故預期其於甚多應用中將取代習知光源,如交通號誌燈、室外與室內顯示器、汽車頭燈與尾燈、及傳統室內照明等等。
習知LEDS的效率受限於無法發射由其活性層所產生之所有光線。當供給LED能量時,自其活性層發射之光線(沿所有方向)將以許多不同角度到達發射表面。典型之半導體材料比周圍空氣(n=1.0)或封裝樹酯(n1.5)有較高之折射率(n2.2-3.8)。根據司乃耳定律(Snell's law),光線自具有高折射率的區域行進到在某一臨界角度內之具有低折射率的區域,將穿越較低折射率的區域;以超過臨界角度到達表面之光線將不會穿出表面,但是會經歷內部全反射(TIR)。於LED案例中,TIR光線可持續於LED內反射,直到被吸收為止。由於該反射現象,多數由習知LEDs所產生之光線並未發射出去,降低了本身之效率。
一種降低TIR光線比例之方法為於LED表面上以隨機蝕紋(random texturing)之形式建立光散射中心。該隨機蝕紋係藉由在反應性離子蝕刻期間以在LED表面上之次微米直徑聚苯乙烯球體作為遮罩而經圖案化於表面。已蝕紋表面具有光波長階次(order)之特徵部,該特徵部因隨機干涉效應(random interference effects)而以司乃耳定律無法預測之方式折射或反射光線。此方法已經證明可改善發光效率9至30%。
如同美國專利第6,821,804號中所討論者,表面蝕紋的一項缺點為其會阻礙在已蝕紋電極層之導電性不良之LEDs中的有效電流散佈,如p型GaN。在較小裝置或者具有良好導電性之裝置中,來自p型及n型層接點(面)之電流將散佈遍及各層。在較大裝置或者由具有不良導電性之材料所製成之裝置中,電流無法從接點(面)散佈遍及各層。因此,部份活性層將不會有電流流過且將不會發光。為了在整個二極體區域產生均勻電流注入,可將導電材料之散佈層(spreading layer)沉積於表面上。然而,此散佈層通常必須具有透光性,以使光可經傳送通過該層。當LED表面上引進一隨機表面結構時,實際上細薄且透光之電流散佈層即無法輕易地沉積於其上。
增加來自LED之光取出的另一方法係包含發光表面或者內部介面之週期性圖案化,其係將光線方向由內部捕獲角(internally trapped angle)再改變至藉由表面形狀與週期所決定之定義模式,請參考Krames等人之美國專利第5,779,924號。此技術為隨機蝕紋表面之特殊案例,其中干涉效應不再為隨機,且該表面將光線耦合成特別模式或方向。此方案之一項缺點為此一結構可能不易製造,因為該表面之形狀與圖案必須均勻且極微小,為LED光之單一波長之階次。將如上所述之光學透明電流散佈層沉積於此圖案上亦存在著困難。
增加光取出已藉由使LED的發光表面形成為在其中心處具有一發光層之半球體而實現。雖然此結構可增加發光量,但其製造卻不容易。Scifres及Burnham之美國專利第3,954,534號揭露了一種LED陣列的形成方法,其中在每一LED上方均具有各自之半球體。該半球體係形成於基板上,且二極體陣列係生長於該半球體上。該二極體與透鏡結構(lens structure)接著即自基板上蝕刻去除。此方法之一項缺點為:基板介面處形成該結構將受到限制,且自基板上剝離(lift off)該結構將導致製造成本增加。又,每一半球體正上方皆有一發光層,故需要精準之製造技術。
美國專利第5,431,766號揭露了矽在無水份及氧氣下之光電化學氧化與分解。於無水HF-乙腈(MeCN)溶液中之蝕刻速率與光電流係直接正比於至少高達600mW/cm2
的光強度,產生了大於4微米/min之空間選擇蝕刻速率。由於電子係自高能量反應中間體射入,故產生每一矽分子有4個電子轉移反應,具有大於3.3之量子產率(quantum yield)。
美國專利第5,793,062號揭露一種用以增強來自LED之光取出之結構,其係藉由包含光學非吸收層以將光線導離吸收區域(如接點(面)),且亦將光線導向LED表面。此結構之一項缺點為:非吸收層需要形成底切狹角層(undercut strait angle layers),其不易於許多材料系統中製造。
美國專利第6,744,071號揭露一種具有相對端子結構之氮化物半導體元件,其端子彼此相對。該氮化物半導體元件包含依序位於支撐基板上之一導電層、一第一端子、一具有發光層之氮化物半導體、以及第二端子。該第一端子及一第一絕緣保護層係介於該導電層與該氮化物半導體之第一導電型氮化物半導體層之間。
美國專利第6,821,804號揭露一種LED,該LED上或其內部具有光取出結構以增強其效能。該新型光取出結構提供用以將光線反射、折射或散射至有利於光線逃逸進入封裝內之方向之表面,該結構可為光取出元件或色散層之陣列。該光取出元件可具有許多不同形狀且可設置於許多位置中,以增強LED之效率而優於習知LED。該色散層提供光線之散射中心並且同樣地可設置於許多位置中。
如同在美國專利第6,821,804號中所更進一步討論者,另一種增強光取出之方法係於LED發光表面上之薄膜金屬層內將光子耦合成表面電漿子模式,其中光子係經發射返回成輻射模式。這些結構係依靠自半導體上發出之光子耦合成金屬層中之表面電漿子,該表面電漿子則再耦合成最後被取出之光子。此裝置之一項缺點為難以製造,因為該週期性結構係一具有淺凹槽深度(<0.1 μm)之一維刻線光柵(one-dimensional ruled grating);此外,整體量子效率低落(1.4~1.5%),極可能是因為光子至表面電漿子以及表面電漿子至周圍空氣之光子轉換機制效率不彰所致。該結構亦存在與上述電流散佈層相同之難處。光取出亦可藉由使LED晶粒之側表面傾斜以產生一倒轉截形金字塔而改善,該斜向表面為陷落於基板材料中之TIR光線提供一發光表面。利用此方法可使InGaAlP材料系統增加35%~50%之外部量子效率。此方法對於其中有大量光波陷落於基板之裝置而言是可行的,然就生長於藍寶石基板上之GaN元件而言,多數光波係陷落於GaN薄膜中,以致於使LED晶粒之側表面傾斜將無法提供所期望的增強作用。用以增強光取出之又另一方案為光子再循環,此方法係依靠LED具有高效率活性層,其可輕易地將電子與電洞轉換成光波,且反之亦然。TIR光線反射離開LED表面並撞擊活性層,其係於此處轉變回電子電洞對,因為該活性層之高效率,電子電洞對幾乎立即地再轉換成光波,再度沿任意方向發出。部份再循環光波將撞擊在臨界角度內之LED發光表面其中之一並逸出,而反射回活性層之光波再次經歷相同過程。
茲揭露一種半導體發光二極體(LED)裝置之製造系統與方法,其係藉由在LED裝置上形成n型氮化鎵(n-GaN)、並且將n-GaN層的表面粗糙化、以增強來自LED裝置內部之光取出而達成。
上述系統的實施可包含以下其中之一或更多:LED晶圓之n-GaN層藉由光電化學氧化以及/或蝕刻製程予以粗糙化。LED晶圓包含:一導電基板(如Cu,W,Mo或其合金);一或更多磊晶層;一或更多歐姆接點以及位於磊晶層與導電基板間之反射金屬層(例如Ni,Au,Pt,Cr,Ti,Pd,及Ag);一保護層,例如在獨立式LED之側壁上之SiO2
,Si3
N4
,或SiON;以及在頂部n-GaN層上之n型電極。該光電化學氧化及蝕刻處理可在含水溶液之系統、照明系統、以及/或電偏壓系統中實施。該水溶液可為氧化劑以及酸性或鹼性溶液之組合,其中氧化劑可為H2
O2
,K2
S2
O8
其中之一或其組合,酸性溶液可為H2
SO4
,HF,HCl,H3
PO4
,HNO3
,CH3
COOH其中之一或更多,鹼性溶液可為例如KOH,NaOH,NH4
OH其中之一或更多。如果使用照明系統,即可藉由具有波長範圍在可見光與紫外光光譜間之Hg或Xe弧光燈實施照明,而以小於200mW/cm2
之強度照射暴露的n-GaN表面;如果使用電偏壓系統,可將其施加於導電層且將電壓控制於-10V與+10V之間。氧化支配、蝕刻支配、或其組合反應可藉由改變水溶液之組成、電偏壓、浴溫以及/或照明強度加以控制,以將n-GaN表面之粗糙度最佳化,無次序(non-ordered)蝕紋型態亦於此粗糙化處理後顯露出來。
粗糙化處理可應用於晶圓級之n側在上(n-side-up)垂直LED之暴露n-GaN。在從載具移除GaN基底(GaN-based)LED磊晶薄膜後,即於n型GaN層上形成n型電極(如Cr/或Ni)。N型金屬焊墊不只是作為歐姆接點而已,亦是後續粗糙化處理所用的遮罩。粗糙化處理係於n型電極金屬化後藉由光電化學(PEC)氧化以及/或蝕刻方法實施,在光照下將晶圓浸沒入水溶液中以及使導電基板電偏壓;水溶液係氧化劑與酸性或鹼性溶液之組合。n型GaN之粗糙化表面將顯露出無次序蝕紋型態,不同於金字塔、圓錐體、或半圓形型態。藉由改變溶液組成、偏壓電壓、溶液溫度或照光強度,可將粗糙化機制控制成氧化支配或蝕刻支配反應。表面粗糙度之RMS值係控制在0.05 μ m至2 μ m。選擇粗糙化表面尺寸,以於約1/2 λ下使光最佳化地散射。在另一實施中,粗糙化表面之有效折射率大約是2.0~2.5。
粗糙化表面的優點可包含下列其中之一或更多。粗糙化表面在GaN上產生一有效粗糙表面以自內部取出更多光,與具有平滑表面之LED相較,具有無次序蝕紋表面之LED之照度可增強超過兩倍。就相同晶粒尺寸/功率消耗而言,LED可提供更多光線;或者,假設相同光輸出需求,LED可製作得更小型,且此種較小尺寸將消耗較少功率及資源,節省成本。LED可以標準處理技術加以製造,使其相較於標準LED相當地具有成本競爭力。
圖1係顯示一實施光電化學(PEC)氧化與蝕刻製程之示範性系統。電解質溶液之本質在確保高蝕刻速率及確保直接與光強度成正比之蝕刻速率時特別重要。PEC蝕刻製程係施行於圖1所示之系統中,在此系統中,光係藉由一光源而投射在位於支座10上方且由夾鉗12固定之LED晶圓表面上,該LED晶圓係與電解質溶液16相接觸。光強度可選擇性地加以變化,以藉此選擇性地改變蝕刻速率。該電池可具有許多幾何配置(configuration)以及可由任合適當材料組成,以支撐LED半導體晶圓並容納含離子之電解質溶液16。可將電池之特定配置最佳化,以用於大量產業應用。一參考電極14(如鉑電極14)經由電池本體而延伸至電解質溶液16中。參考電極14建立了參考電壓Vr e f
且其通常由金屬導線形成,如鉑或銀導線,為了便利起見,可由飽和甘汞電極(saturated calomel electrode,SCE)或由任何其他電極機構來形成。
發生於電池中之光電化學反應係由穩壓器(potentiostat)供給電能並加以監測,於此項技藝中其已為人所熟知。穩壓器包含:一電流偵測器,與用以跨越電極施加電位之源電壓相串聯;及一接線,將穩壓器連接至半導體晶圓。該接線可經由任何黏合機構而固定至半導體晶圓。
在實施於圖1之系統內之PEC蝕刻製程中,半導體晶圓為氧化還原反應之一部分,半導體晶圓成為陽極且對向電極成為陰極。對半導體晶圓施加電位,於製程中利用參考電極14測量與監測電位。在半導體晶圓與電解質溶液16間之介面處,因光生成電洞所誘發之分解反應而引起蝕刻反應。
圖2A係顯示在針對各種不同持續時間之氧化支配條件下,具有金屬遮罩之第一樣品之表面輪廓圖。該樣品晶圓包含一基板30,一GaN薄膜32,一具有粗糙化表面之金屬遮罩34。在氧化支配條件下持續200秒之具有金屬遮罩之第一樣品的表面輪廓圖係顯示於圖2B,持續400秒者顯示於圖2C,而持續600秒者顯示於圖2D。
圖3係顯示在針對各種不同持續時間之蝕刻支配條件下,具有金屬遮罩之第二樣品之表面輪廓圖。該樣品晶圓包含一基板30,一GaN薄膜32,一具有粗糙化表面之金屬遮罩34。在蝕刻支配條件下持續200秒之具有金屬遮罩之第二樣品的表面輪廓圖係顯示於圖3B,持續400秒者顯示於圖3C,而持續600秒者顯示於圖3D。
圖4係顯示一垂直LED晶圓之結構。一示範性n-GaN層在上LED之多層磊晶結構係顯示於一載具(carrier)上,在此實施例中其可為厚含銅層。在金屬承載基板上形成之多層磊晶結構包含一n-GaN基底層80、一MQW活性層78、一p-GaN層76、反射器/接觸層74、一黏附金屬層72、一金屬基板70、一n型接點82、以及一非導電性鈍化層84。舉例來說,n-GaN基底層80之厚度為4 μm。
MQW活性層78可為InGaN/GaN MQW活性層。一旦將電功率經由基板70而饋入於n-GaN基底層80與接觸層74之間,MQW活性層78便可受激發而因此產生光,所產生的光具有介於250nm與600nm間之波長。P型層76可為p+
-GaN基底層,如p+
-GaN,p+
-InGaN或p+
-AlInGaN層,且其厚度可介於0.05-0.5 μm之間,可大於0.5 μm。圖5係顯示在粗糙化製程後垂直LED晶圓之橫剖面圖。如圖5至圖6所示,無次序蝕紋型態(non-ordered textured morphology)係於n-GaN表面上形成。
圖5係顯示在圖4之LED之金屬層上的粗糙化表面之橫剖面圖,而圖6顯示該粗糙化表面之示範性SEM影像圖。於該表面上之變化可有效地使表面粗糙化,且使得對於空氣之折射率具有較佳匹配度。因此,該效果促使自LED內部更好之光取出。
雖然本發明已參照其某些較佳實施例甚為詳細地加以說明,但亦可有其他變化形式。在另一實施例中,GaN層之表面係利用球/球體或利用濕式/乾式蝕刻技術加以粗糙化,但其他具有錐形之粗糙化表面之LED結構亦為熟悉此項技藝者所能預見。該新LED可具有不同表面處理之組合,錐形可有不同形狀、大小、間距(space);同樣地,錐形可具有各種不同密度。因此,所附申請專利範圍之精神與範疇不應限制於上述之較佳實施例。
雖然本發明已藉由舉例及就較佳實施例加以敘述,惟應了解本發明並非限制於此。相反地,本發明應包含各種修改例及類似結構及步驟,且因此所附申請專利範圍之範疇應給予最廣義之解釋,以包含所有此類修改及類似結構及步驟。
10...基座
12...環形夾鉗
14...鉑極
16...水溶液
30...基板
32...GaN薄膜
34...金屬遮罩
70...基板
72...黏附金屬層
74...接觸層
76...p型層
78...MQW活性層
80...n-GaN基底層
82...n型接點
84...非導電性鈍化層
圖1係顯示一實施光電化學氧化及蝕刻製程的示範性系統。
圖2A-2D係顯示具有金屬遮罩之第一樣品之表面輪廓圖,其係在氧化支配條件下就各種不同持續時間實施者。
圖3A-3D係顯示具有金屬遮罩之第二樣品之表面輪廓圖,其係在蝕刻支配條件下就各種不同持續時間實施者。
圖4係顯示具有頂部n-GaN層之垂直LED晶圓之結構。
圖5係顯示將暴露n-GaN層粗糙化後之垂直LED晶圓之橫剖面圖。
圖6係顯示n-GaN表面之無次序蝕紋型態之示範性SEM圖。
70...基板
72...黏附金屬層
74...接觸層
76...p型層
78...MQW活性層
80...n-GaN基底層
82...n型接點
Claims (34)
- 一種半導體垂直發光二極體(VLED)裝置之製造方法,包含:形成該VLED裝置之多層磊晶結構,其包含一n型氮化鎵(n-GaN)層、一活性層、及一p型氮化鎵(p-GaN)層;以及藉由改變一水溶液之組成、電偏壓、以及照光強度使該VLED裝置之該n-GaN層之表面於該水溶液中粗糙化。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該n-GaN層係藉由濕式蝕刻製程加以粗糙化。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,更包含氧化及蝕刻該LED。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該氧化及蝕刻係於具有水溶液之系統中實施。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該水溶液可為氧化劑及酸性或鹼性溶液之組合。
- 如申請專利範圍第5項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該氧化劑包含H2 O2 、K2 S2 O8 其中之一或其組合。
- 如申請專利範圍第5項之半導體垂直發光二極體 (VLED)裝置之製造方法,其中該酸性溶液包含H2 SO4 、HF、HCl、H3 PO4 、HNO3 、及CH3 COOH其中之一或更多。
- 如申請專利範圍第5項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該鹼性溶液包含KOH、NaOH、及NH4 OH其中之一或其組合。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,更包含以波長範圍在可見光與紫外光光譜之間的Hg或Xe弧光燈系統來照亮該LED。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,其中該n-GaN層係以小於200mW/cm2 之光強度曝光。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,更包含對該導電基板施以電偏壓且將電壓控制於-5V與+5V之間。
- 如申請專利範圍第1項之半導體垂直發光二極體(VLED)裝置之製造方法,更包含控制氧化支配、蝕刻支配、或兩反應,以使該n-GaN層之該表面之粗糙度最佳化。
- 一種n側在上(n-side up)LED晶圓之曝露n-GaN層的粗糙化方法,其中該LED晶圓具有一金屬基板,該方法包含:在一承載基板上方沉積一n-GaN部分;在該n-GaN部分上方沉積活性層;在該等活性層上方沉積一p-GaN部分; 沉積一或更多金屬層;施加一遮罩層;蝕刻該金屬層、p-GaN層、活性層、及n-GaN層;移除該遮罩層;沉積一鈍化層;將位於該p-GaN層頂部上之該鈍化層之部分移除,以曝露該金屬層;沉積一或更多金屬層;沉積一金屬基板;移除該承載基板以暴露該n-GaN表面;將該n-GaN表面粗糙化。
- 如申請專利範圍第13項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該n側在上LED晶圓之該n-GaN層於該粗糙化製程之前係實質上光滑且平坦。
- 如申請專利範圍第14項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該n側在上LED晶圓之該n-GaN層於該n-GaN層經粗糙化之前具有小於5000Å之表面粗糙度。
- 如申請專利範圍第13項之之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該承載基板係藍寶石。
- 如申請專利範圍第13項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該金屬基板係利用以下其中之一來沉積:電化學電鍍、無電化學電鍍、濺鍍、化學氣相沉積、電子束蒸發、熱噴灑(thermal spray)。
- 如申請專利範圍第13項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該金屬基板係一金屬或包含銅、鎳、鋁、鈦、鉭、鉬、鎢其中之一的金屬合金。
- 如申請專利範圍第13項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該承載基板係利用以下其中之一來移除:雷射剝離(LLO)、濕式蝕刻、化學機械研磨。
- 如申請專利範圍第13項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中將該n-GaN層粗糙化包含在水溶液中之濕式蝕刻。
- 如申請專利範圍第20項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該水溶液可為稀釋劑及酸性或鹼性溶液之組合。
- 如申請專利範圍第21項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該稀釋劑包含水。
- 如申請專利範圍第21項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該酸性溶液包含H2 SO4 ,HF,HCl,H3 PO4 ,HNO3 ,及CH3 COOH其中之一或更多。
- 如申請專利範圍第21項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該鹼性溶液包含KOH,NaOH,及NH4 OH其中之一或其混合物。
- 如申請專利範圍第21項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該水溶液係加熱至較高於25℃之溫度。
- 一種n側在上LED晶圓之曝露n-GaN層的粗糙化方法,該LED晶圓具有一金屬基板,該方法包含:在一承載基板上方沉積一n-GaN部分;在該n-GaN部分上方沉積活性層;在該等活性層上方沉積一p-GaN部分;沉積一或更多金屬層;施加一遮罩層;蝕刻該金屬層、p-GaN層、活性層、n-GaN層;移除該遮罩層;沉積一鈍化層;將位於該p-GaN層頂部之該鈍化層之部分移除,以曝露該金屬層;沉積一或更多金屬層;沉積一金屬基板;移除該承載基板以暴露該n-GaN層之表面;在該n-GaN層之表面上形成一或更多金屬層;將該n-GaN層之該表面粗糙化。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該水溶液可為稀釋劑及酸性或鹼性溶液之組合。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該稀釋劑包含水。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該酸性溶液包含H2 SO4 ,HF,HCl,H3 PO4,HNO3 ,及CH3 COOH其中之一或更多。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該鹼性溶液包含KOH,NaOH,及NH4 OH其中之一或其混合物。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該金屬基板係利用以下其中之一來沉積:電化學電鍍、無電化學電鍍、濺鍍、化學氣相沉積、電子束蒸發、熱噴灑(thermal spray)。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該金屬基板係一金屬或包含銅、鎳、鋁、鈦、鉭、鉬、鎢其中之一的金屬合金。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中該承載基板係利用以下其中之一來移除:雷射剝離(LLO)、濕式蝕刻、化學機械研磨。
- 如申請專利範圍第26項之n側在上LED晶圓之曝露n-GaN層的粗糙化方法,其中在該n-GaN表面之一或更多金屬層包含鎳、鉻、金、鈦、鉭、銅、錫、鋅、鋁其中之一。
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CN (1) | CN100550287C (zh) |
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EP1856716A2 (en) | 2007-11-21 |
JP2008527717A (ja) | 2008-07-24 |
CN100550287C (zh) | 2009-10-14 |
WO2006076207A2 (en) | 2006-07-20 |
WO2006076207A3 (en) | 2006-11-02 |
US20060154391A1 (en) | 2006-07-13 |
TW200705710A (en) | 2007-02-01 |
KR20070115869A (ko) | 2007-12-06 |
US7186580B2 (en) | 2007-03-06 |
CN101103439A (zh) | 2008-01-09 |
KR101231091B1 (ko) | 2013-02-07 |
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