TW588016B - Process for obtaining bulk mono-crystalline gallium nitride - Google Patents
Process for obtaining bulk mono-crystalline gallium nitride Download PDFInfo
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- TW588016B TW588016B TW091112459A TW91112459A TW588016B TW 588016 B TW588016 B TW 588016B TW 091112459 A TW091112459 A TW 091112459A TW 91112459 A TW91112459 A TW 91112459A TW 588016 B TW588016 B TW 588016B
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- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- H01S5/00—Semiconductor lasers
- H01S5/02—Structural details or components not essential to laser action
- H01S5/028—Coatings ; Treatment of the laser facets, e.g. etching, passivation layers or reflecting layers
- H01S5/0281—Coatings made of semiconductor materials
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- H01S5/00—Semiconductor lasers
- H01S5/30—Structure or shape of the active region; Materials used for the active region
- H01S5/32—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures
- H01S5/323—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser
- H01S5/32308—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser emitting light at a wavelength less than 900 nm
- H01S5/32341—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser emitting light at a wavelength less than 900 nm blue laser based on GaN or GaP
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/102—Apparatus for forming a platelet shape or a small diameter, elongate, generally cylindrical shape [e.g., whisker, fiber, needle, filament]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
Description
588016
發明之技術領域 本發明係有關由超臨界溶液在晶種上結晶,生成氮化鎵 之塊狀單結晶的方法。尤其藉由利用超臨界氨之技術,使 炫化法所得之氮化鎵經再結晶後,可以得到氮化鎵之塊狀 單結晶。 先前技術 氮化鎵之塊狀單結晶的形成方法中,為了降低生成步驟 的溫度與壓力,有人提議利用超臨界氨。其中之一是,以 鎵當作供料’藉由合成含有鹼金屬胺(KNh2或LiNH2)之氨 來成長GaN結晶的方法,將反應溫度設在55〇。〇以下,壓力 在5 kbar以下,則成長之結晶有5 μΐΏ大「Α1τιηιοηο meth〇(i 〇f BN? AIN, and GaN synthesis and crystal growth" R. Dwilinski et al.5 Proc. EGW-3, Warsaw, June 22-24, 1998, MRS Internet Journal of Nitride Semiconductor Research ] 。其它的方法是,使用市售之GaN粉末,使氮化鎵再結晶 之方法[’Crystal Growth of gallium nitride in supercritical ammonia·' J. W. Kolis et al·,J. Cryst. Growth 222, 43 1-434 (2001)]。然而,在使用前者將鎵金屬當做供料之方法中, 很難控制反應。另外,在後者是將GaN當做供料之再結晶 方法中,得不到0.5 mm程度之GaN結晶,得不到塊狀结晶 。這是因為在超臨界溶液内之化學輸送也見不到在晶種上 成長。又,氮化鎵是與水晶不同,為天然中不存在之原料 ,供應上有困難。 -4- 本纸張尺度適用中國國家標準(CNS) Α4規格(210X 297公釐) α 2 五、發明説明( 發明所欲解決之課題 再結晶熔化法中所得 成氮化鎵塊狀單結晶 在此,本發明之第1個目的是提供, 到之氮化鎵結晶,使在晶種上可以形 的方法。 單-曰再-曰…: 法中所得到之氮化 元 早一再一成長為在品質上可以應用之能做 件基板的氮化鎵塊狀結晶。 課題之解決手段 為了達成上述目的❾本發明^構成是,著眼在利用μ 法得到氮化料結晶塊時,於含有付與氨基㈣Monobasic)之 1種或多 數驗化劑的超臨界氨溶劑中 產生化學輸送 ,可以得到再結晶氮化鎵之單結晶,是提供: 其特徵為得到氮化鎵塊狀單結晶之方法中,於高壓銷内 將炼化法所形成之氮化鎵單結晶塊,溶解到含有氨與驗 金屬離子之超臨界溶劑中,供給氮化鎵之溶解度為負溫度 係2之超臨界溶液,上述超臨界溶液利用氮化鎵之溶解度 負服度如數,只在高壓鍋内所配置之晶種面上選擇性的成 長氮化鎵結晶之方法, 以及其特彳政為得到氮化鎵塊狀單結晶之方法中,在高壓 鍋内將熔化法所形成之氮化鎵單結晶塊溶解到含有氨與鹼 至屬離子之超臨界溶劑中,供給氮化鎵之溶解度為正壓力 係數之超臨界溶液,上述超臨界溶液利用氮化鎵之溶解度 正壓力係數’只在高壓鍋内所配置之晶種面上選擇性的生 長氮化鎵結晶之方法。 五、發明説明( 在第1構成中,供仏、、交紐备 水晶之水敎合成法不°广化叙之超臨界溶液步驟,是與 ;、去:同,做為此原料之氮化鎵在天然中並 ’ Μ化法所形成之11化鎵單結晶塊做為供 屬=中1;?是彻化法為代㈣化_金 ,藉由在κ/*屬與11氣的反應)所得之氮化鎵單結晶 物超臨界溶液之對流’以未炫解狀態不用 物理的私動而成為所謂之可固定物體。 中中’所得超臨界溶財之溶解性氮化錄濃度 在一皿度中,以調整在不超 免在後面步驟中產生自發結晶。 ^疋為了避 種2^構’ $彳7帛2之結晶步驟,重點是選擇性在晶 單处曰之在此,本案發明之第3構成是氮化鎵塊狀 屬離子之超臨界溶劑中,將央u金 之μ只…六^τ⑯孔化叙之溶解度為負溫度係數 界浴液,至少配置在高壓銷内晶種領域中,上昇到 所定之溫度或下降到所定之壓力下,超臨界溶液之溶:产 於相當晶種過飽和領域中,調節自發結 二 鎵結晶之方法。 置之“重面上選擇性的成長氮化 :=中’在高壓鋼内同時形成所謂的溶解領域與結 :以之2個領域時,為了控制針對晶種超臨界溶液之過 飫和,U调整溶解溫度與結晶化溫 領域之溫度若設;ξ在400〜帽。D 因此’結晶化 : 。显度則能容易控制,在 冋谷解溫度與結晶化溫度之溫度差以在Η。。。以下 -6 - 4 五、發明説明(
為宜,較佳是保持在loot以下則能容易控制。X 種超臨界溶液之過飽和調整,在高壓鍋内是可以# ’ 、晶 多數個閥來區分低溫溶解領域與高溫結晶化領 或 藉由調整溶解領域與結晶化領域之對流量來進^。’可以 同㈠·,在上述第〗構成中,上述鹼金屬離子 或不含i素物質之鹼化劑形狀,做為鹼金屬離選 自由Li+、Na+、K+所組成族群中之!種或2種者。疋、 又’本發明方法是依靠在氨基驗性反應者,為㈣化法 所形成之氮化鎵單結晶塊做為料,對鈉、其它本來含驗 金屬之氨基驗性超臨界反應無害,驗金屬是有必要做為驗 化劑之元素。 使用上述鈉熔化法中所形成之氮化鎵做為原料時,能容 易控制結晶化之反應’纟此場合’做為晶種者以使用氮化 鎵單結晶為宜。 本發明是提供,上述第1溶解步驟與第2結晶化步驟是在 同時,且在高壓鍋内進行做為分離方法之下面構成,即, 提供其特徵為,得到氮化鎵之塊狀單結晶之方法,在高嬋 鍋中形成含有鹼金屬離子之超臨界氧溶劑,在該超臨界^ 溶劑中溶解以熔化法所形成之氮化鎵單結晶塊,對超臨界 溶劑在比熔化法所形成氮化鎵單結晶塊溶解時更高溫及/ 或更低壓之條件下,溶解上述熔化法所形成之氮化鎵單結 晶塊之超臨界溶液中,氮化鎵會在晶種面上結晶之方法。 在第1構成中,在熔化法所形成之氮化鎵單結晶塊的溶解 步驟之外,也可以具備比超臨界溶液更高溫及/或更低壓中 本紙張尺度t g S家標毕(CNS) A4規格(21GX297公爱) :動之步驟。X,在高a鍋令同時形成有溫度 2域,在低溫溶解領域中配置以炫化法所形成之氮㈣ =晶塊’在高溫結晶化領域中配置晶種來進行。溶解領 晶:::之溫度差,必須設定超臨界溶液内能禮保 :::之範圍内’超臨界溶液内之化學輸送主要是藉由 來進行’通常,溶解領域與結晶化領域之溫度差是在 以上,較佳是在5〜l5〇t,更好是在1〇〇。〔以下。 在本發明中,氮化鎵因應用途之需求,可以含有給予體 、接受體或磁性之處理劑,超臨界溶劑是如下定義,含有 NH3或其衍生物、做為鹼化劑之鹼金屬離子、至少為含有 鈉或鉀之離子。 f本發明中,晶種至少含有鎵或其它ΙΠ族元素之氮化物 結晶層,晶種為含有鎵之氮化物結晶層中,表面之缺陷 密度= 下者為佳’又’晶種是以炼化法所形成之 氮化鎵為且,(0002)面之χ線的鎖定曲線半值寬(fwhm)是 120 arcsec以下為宜。 在本發明中,氮化鎵之結晶化是可以在100〜800°C之範 圍進行,但較好是在3〇〇〜6〇〇。〇,更好是可以在4〇〇〜55〇〇c 之脈度進行’又,氮化鎵之結晶化是可以在100〜10000 bar 進行’但較佳是在1000〜5500 bar,更好是可以在1500〜 3000 bar之壓力進行。 超臨界溶劑内之鹼金屬離子濃度是,確保可以調整以熔 化法所形成之GaN單結晶塊及在晶種之含有鎵的氮化物的 特定溶解度’針對超臨界溶液内之其它成分,鹼金屬離子
之莫爾比以控制在1 : 200〜1 : 2,較佳者為1 : 100〜1 ·· 5 ’更好為1 · 20〜1 · 8之範圍以内為宜。 同時,本發明是有關在含有付與氨基鹼性丨種或多數鹼化 劑之超臨界氨溶劑中產生化學輸送,可得氮化鎵單結晶成 長,氨基鹼性結晶成長技術,為了認可原本的高技術,在 本發明中,所使用之下面用詞,是可以用以下之本案說明 書來定義其意義。 以熔化法所形成之氮化鎵者,是以Na熔化法所代表之以 金屬熔融液中的氮化反應,BN(氮化硼)製之坩堝中在氮氣 氣氛下,加入鎵金屬與鈉金屬,調成5〇氣壓、75〇t之狀態 ,此狀態於7天以上所形成之氮化鎵單結晶,做成丨〜1〇 之板狀塊。 氮化鎵之塊狀單結晶是,指藉*M〇CVD或是等之 表(epi)成長方法,可以形成如LED*LD之光及電子零件的 氣化紅早結晶基板。 日超臨界氨溶劑是被認為,至少含有氨,超臨界氨溶劑, 疋含有為了溶解GaN之1種或多數之鹼金屬離子。 驗化劑纟,是指在超臨界氨溶劑中,為了溶解氮化嫁供 給所謂的之1種或多數之鹼金屬離子者,在說明書中有具體 例示。 、超臨界氨溶液,是指上述超臨界氨溶劑與以熔化法所形 成之鼠化鎵單結晶塊由溶解所產生之溶解性氮化錄的意思 。依我們之實驗,發現於充分之高溫高壓下,在固體之氮 化鎵與超臨界溶液間存在著平衡關係,因此,溶解性氮化 588016 A7 B7 錄之溶解度是可以定義為在含有固態鎵之氮化物存在下, 上述溶解性氮化鎵之平衡濃度。相關步驟中,此平衡是依 溫度及/或壓力的變化而移動。 浴解度之負溫度係數者,是指保持其它全部之參數時, 溶解度是以溫度之減少係數(m〇n〇t〇nically Ια —叫 funcuon)來表示,同樣的,溶解度之正壓力係數者,是指 保持其它全部之參數時,溶解度是以壓力之增加係數來表 不,在我們之研究中發現,在超臨界氨溶劑中溶解性氮化 鎵的溶解度至少從300到55〇。〇之溫度領域,自u〗5 5汕以 之壓力範圍中,出現負溫度之係數及正壓力之係數。 針對氮化鎵超臨界氨溶液的過飽和者,是指在上述超臨 界氨溶液中可溶性GaN濃度為平衡狀態之濃度,即,指溶 解度更咼之意思。在閉鎖系統中氮化鎵之溶解情形,此過 飽和是依溶解度之負溫度係數或是正壓力係數,藉由增加 溫度或是減少壓力可以達成。 超臨界氨溶液中有關氮化鎵之化學輸送者,是經由^^熔 化法所形成之氮化鎵單結晶塊的溶解、可溶性GaN之超臨 界氨溶液之移動、包含過飽和超臨界氨溶液之氮化鎵的結 晶、等連續步驟,一般化學輸送步驟是藉由溫度梯度、壓 力梯度、濃度梯度、溶解之氮化鎵與結晶化生成物之化學 的或是物理的不同性質等之、驅動力來進行。依本案發明 方法雖可得到氮化鎵塊狀單結晶,但上述化學輸送是分別 在溶解步驟與結晶化步驟之領域中進行,結晶化領域以維 持在比溶解領域更高溫度來達成較佳。 -10 - 本紙張尺度適用巾S S家標準(CNS) A4規格(21GX297公爱)
裝 訂 8 五、發明説明( 但也提供進行含鎵氮化 成長品質,所以與所成 晶種雖在本案說明書中有例示, 物之結晶化領域,因其支配結晶之 長之結晶相同,能選擇品質良好者 自發之結晶化(Spontaneous crystaUizati〇n),是浐自尚飽 和超臨界氨溶液形成氮化料核及成長,纟高^内= -邊都可能產是不被期望之步驟,包含在晶種表面之 不同方向性成長(disoriented growth)。 曰對晶種之選擇性結晶纟,是指所謂之非自發的成長、結 晶化是在晶種上進行之步驟,為達成塊狀單結晶成長中所 不可欠缺之步驟,為本案發明方法之一。 結晶成長之閉鎖系 高>1鍋是不管形態、是進行氨基鹼性 反應室。 同日守,本案發明之實施例中高壓鍋内之溫度分布,因是 在沒有超臨界氨存在下,所測定之空高壓鍋者,並非實際 2臨2溫度。又,愿力是直接測定的,{由最初導入之 氨量、高壓鍋之溫度、容積等來計算決定者。 上述方法於實施時,以使用如下之裝置為佳,即,本發 明是提供特徵為備有產生超臨界溶劑之高壓鍋1之設備、在 上述高壓鍋中設置有對流控制管理裝置2、投入在備有加熱 裝置5或冷卻裝置6之爐體4中,之氮化鎵塊狀單結晶的生產 設備。 述爐體4,是相當於高壓鍋丨之結晶化領域14、備有加 …、衣置5之同溫領域及相當於高壓鍋丨之溶解領域1 3,備有 加熱裝置5或冷卻裝置6之低溫領域,或是上述爐體4,是相 588016 A7 B7 五、發明説明(9 ) - 當於高壓鍋1之結晶化領域14、備有加熱裝置5或冷卻裝置6 之南溫領域及相當於高壓鍋1之溶解領域1 3,備有加熱穿置 5或冷卻裝置6之低溫領域。對流控制管理裝置2,是區八成 結晶化領域14與溶解領域13,在中心或周圍由_張或$張 之有孔洞橫型閥12所構成。在高壓鍋丨内,溶解領域13中配 置有炫化法所形成之氮化鎵16,結晶化領域丨4中配置有晶 種17 , 13與14領域間之超臨界溶液的對流是依控制管理= 置2來設定組成,其特徵為溶解領域13是位在橫型閥丨2之1 方’結晶化領域1 4是位在橫型閥1 2之下方。 圖式說明(元件符號說明) 圖1表示在T= 400t與T=50(TC中,壓力與含有胺化鉀 (KNH2 : NH3= 0.07)之超臨界氨内的GaN溶解度關係圖。 圖2表示實施例丨中,p=常數,因時間之變化,高壓鍋内 之溫度變化圖。 圖3表示實施例2中,p=常數,因時間之變化,高壓鍋内 之壓力變化圖。 圖4表示實施例4中,因時間之變化,高壓鍋内之溫度變 化圖。 圖5表示實施例6中,因時間之變化,高壓鍋内之溫度變 化圖。 圖6表示實施例7中,因時間之變化,高壓鍋内之溫度變 化圖。 又 圖7表示實施例3、4、5中所述之高壓鍋與爐體之剖面 圖0 -12-
588016 A7
圖8表示生產含鎵之氮化物。 物塊狀早結晶之設備概要圖。 最良好之發明貫施形態 在本發明方法中,可以公A ^切 刀為浴解以熔化法所形成之氮化
鎵塊狀單結晶之步驟,盥在S插品L w /、在日日種面上進行氮化鎵成長的高 溫或低壓條件下移動超臨界溶 4 /合履之步驟。或是,高壓鍋中 至少分成2個有溫度差之々g祕 p 炙項域,熔化法所形成之氮化鎵塊狀 I結晶也可以配置在低溫之溶解領域中,晶種配置在高溫 之結晶化領域中,雖藉由溶解領域與結晶化領域間之溫度 差使對流,可以設定在超臨界溶液内可能進行化學輸送之 範圍,但土述之溶解領域與結晶化領域間之溫度差是^ °C以上。氮化鎵也可以含有給予體、接受體、磁性處理劑 等。超臨界溶劑中是使用含有鹼金屬(至少為鉀)離子之氨 或其衍生物。晶種至少含有鎵或其它族號13 (IUPAC、1989〕 儿素的氮化物結晶層,此結晶層之表面欠缺密度是在 106/cm2以下。 氮化紅之結晶化是在溫度為1 〇 〇〜8 〇 〇、壓力工⑽〜 10000 bar之條件下進行。超臨界溶劑中鹼金屬離子之濃度 ,是可以調整到確保氮化鎵之適當溶解度者,對於超臨界 溶劑内之其它成分,鹼金屬離子之莫爾比控制在丨:2〇〇〜^ :2之範圍内。 氮化鎵之單結晶生產設備是由,備有控制對流裝置之產 生超臨界溶劑的高壓鍋,及高壓鍋配置有1台或數台備有加 熱、冷卻措把之爐體所組成,在爐體中備有相當於高壓编 結晶化領域之加熱措施高溫領域、與備有相當於高壓鋼溶 -13-
裝 訂
本紙張尺度適用中國國家標準(CNS) A4規格(210X297公爱) 11 五、發明説明 解領域之加熱、冷卻裝置 加執、六"壯 {夏〈低酿領域。又,可以利用備有 …冷部I置之高溫領域、盥偌古 溫領域之爐體。上述對”制;;有加熱、冷卻裝置之低 與溶解領域,可以在中ΐ裝置,是區分成結晶化領域 壓M。或周圍製成1張或數張橫型間。高 s二:解領域中配置以鈉炫化法所形成之氮化鎵單結 m :曰曰化項域配置晶種。溶解領域與結晶化領域間之 位在橫型閥之上方,二化二:匕來控制。溶解領域是 、、,口日日化領域是位在橫型閥之下方。 依進行之研究結果,最佳之氮化料狀單 度約為10W,對於表面⑽叫之X線測定半值寬,因^ 60 arcsec以下,所以使用此之半導體元件可以確保適當之 品質與壽命特性。 一氮化鎵在含有鹼金屬或其化合物(KNH2等)2NH3中,顯 π出有良好之溶解度。圖i所示超臨界溶劑内氮化鎵的溶解 度在4001到5001之溫度與壓力的關係,但此溶解度是定 義為莫爾比·· S^GaN溶液··(KNH2+Nh3) 1〇〇%。在此情形 之溶劑,是莫爾比χΞΚΝΗ2 ·· 1^3為0 07之超臨界氨内之 ΚΝΗ2浴液。藉由上述之圖時,溶解度是與壓力之增加有關 ,與溫度之減少有關。利用此關係,在溶解度高的條件下 進行含鎵氮化物之溶解,藉由在溶解度低的條件下結晶, 可以成長氮化鎵之塊狀單結晶。此負溫度梯度的意思是指 在產生溫度差之場合,GaN之化學輸送為自低溫溶解領域 邁向高溫之結晶化領域。其次,適當變化加熱等之條件來 進行,造成氮化鎵過飽和溶液,在晶種面上成長結晶。本 588016
發明之方法是與下述有關聯,是在曰插;u π ^ ^ 疋任日日種面上可以成長氮化 鎵之塊狀單結晶,氮化鎵之單結晶變成晶種做成塊狀單結 晶層而得到GaN的化學理論成長。上述之單結晶,因是在 含有鹼金屬離子之超臨界溶液内成長,因此所得之單結晶 也含有(M PPm以上之鹼金屬。又,為了防止設備腐蝕需: 持超臨界溶液之鹼性,期望在溶劑中不要投入鹵素物質。 再者,氮化鎵之塊狀單結晶中,可以接受處理濃度1〇丨7〜 l〇21/cm3之給予體(Si、Ο等)、接受體(Mg、Zn等)、磁性物 質(Mn、Cr等),藉由接受處理可以改變含鎵氮化物之光學 、電性、磁性特性。在其它之物理特性中,成長之〇_塊 狀單結晶表面的欠缺密度是可以在1 〇6/cm2以下,較佳是在 l〇5/cm2以下,更佳是在loVcm2以下。又,對(〇〇〇2)面之χ 線半值寬是在600 arxsec以下,較佳是在3〇〇 arcsec以下, 更佳疋在60 arcsec以下成長。 實施例1 使用導入有2台掛鋼之容積為10.9 cmJ之高壓加壓鋼[η. Jacobs, D. Schmidt, Current Topics in Material Science, vol.8, ed. E. Kaldis (north — Holland, Amsterdam, 19810, 381設計)’ 一個是配置0.4克以熔化法形成之厚度為〇 i mm 的GaN薄板,另一個是配置重量為〇·ι克以HVPE法所得之厚 度為0.2 mm的晶種,在高壓鍋中投入〇·72克純度為4N之金 屬鉀。再投入4 · 8 1克氨後,緊閉高壓鍋。將高壓鍋投入爐 中,加熱到400°C,高壓鍋内之壓力為2 kbar,8天後,溫度 加熱到500°C,壓力保持在2 kbar*狀態,再放置8天(圖2), -15-
本紙張尺度適用中國國家標準(CNS) A4規格(210X 297公釐) 588016
操作結果,供料之鈉熔化法所形成之全量GaN會溶解,部 刀在’谷解之晶種上再結晶成G aN層。兩面之單結晶層纯厚 度約為0.4 m m。 實施例2 在容積10.9 cm3之高壓加壓鍋中,導入2台坩鍋,一個是 加入0_4克以鈉熔化法形成之厚度為〇·ι mm的GaN薄板,另 一個是配置重量為0.1克以HVPE法所得厚度為2倍的晶種 ’在高壓鍋中投入0.82克純度為4N之金屬鉀。再投入5.43 克氨後,緊閉高壓锅。將高壓鋼投入爐中,加熱到5 〇 〇。〇, 高壓鍋内之壓力為3.5 kbar,2天後,壓力降到2 kbar,溫度 保持在500°C之狀態,再放置4天(圖3),操作結果,以鈉熔 化法所形成之全量GaN會溶解,部分在溶解之晶種上再結 晶成GaN層。兩面之單結晶層總厚度約為〇·25 mm。 實施例3 在容積35.6 cm3之高壓加壓鍋1(圖7)中,將3.0克以鈉溶 化法形成之GaN同量分開配置在溶解領域丨3與結晶化領域 14中,投入2.4克純度為4N之金屬鉀,其次投入15.9克之氨 水(5 N)’緊閉高壓鋼1後,投入爐體4中,加熱到4 5 〇 ,高 壓鍋1内之壓力為2 kbar,1天後,結晶化領域14之溫度增加 到500°C,將溶解領域13之溫度降到400°C ,在此狀態之高 壓鍋1再放置6天(圖4)。操作結果,溶解領域13之GaN—部 分溶解,在結晶化領域14之GaN晶種上成長氮化鎵。 實施例4 在容積36 cm3之高壓加壓鍋1(圖7)之溶解領域13中,將 • 16- 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公爱) 588016
1·6克以鈉熔化法形成之GaN做為供料,在結晶化領域“中 配置〇·8克以HVPE法所得之GaN晶種,再投入3·56克純度為 4Ν之金屬鉀,其次投入14·5克之氨水(5Ν),緊閉高麼鍋卫。 將高壓鍋1投入爐體4中,加熱到425 V,高壓鍋内之壓力為 1·5 kbar , 1天後,溶解領域13之溫度降到4〇〇t,將結晶化 領域14之溫度增加到450t:,在此狀態之高壓鍋再放置8天 (圖5)。操作結果,溶解領域132GaN一部分溶解,在結晶 化領域14之HVPE· GaN晶種上成長氮化鎵。兩面之單結晶 層總厚度約為0.15 mm。 實施例5 在容積36 cm3之高壓加壓鍋丨(圖7)之溶解領域13中,配置 2克以鈉熔化法所形成之GaN做為供料,加入〇.47克純度為 4N之金屬鉀,在結晶化領域丨4中配置〇·7克以hvpe法所得 之GaN晶種,其次投入16·5克之氨水(5Ν),緊閉高壓鍋1。 將南壓鋼1投入爐體4中,加熱到500 °C ,高壓鋼内之壓力為 3 kbar , 1天後,溶解領域13之溫度降到45(rc ,將結晶化領 域1 4之溫度增加到5 5 0 °C,在此狀態之高壓鍋再放置8天 (圖6)。操作結果’溶解領域1 3之〇aN 一部分會溶解,在結 晶化領域14之晶種上成長氮化鎵。兩面之單結晶層總厚度 約為0.4 mm。 有關本發明之方法,是利用在超臨界溶劑内生產含鎵氮 化物之塊狀單結晶設備來進行,此設備之主要部分是由生 成超S品界溶劑之高壓銷1,與高壓銷1中可能有之超臨界溶 液内控制化學輸送的管理裝置2所組成,將上述之高壓鍋1 -17- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
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588016 A7
投入備有加熱措施5或冷卻措施6之爐(2台)體4室内3中,為 了對爐體4保有一定之位置,以帶子之固定裝置7來固定: 爐體4設置在爐床8上,在爐體4與爐床8之周圍以鋼帶9固定 ,爐床8與爐體4在回轉台10上設置,藉由特定之角度栓固 定裝置1 1固定,可以處理高壓鍋丨内之對流種類與對流速度 。在爐體4所投入之高壓鍋1内的超臨界溶液對流,可以區 分成結晶化領域14與溶解領域13,在中心或周圍設定一張 或數張有孔洞之橫型閥12所組成的對流管理裝置2。將高壓 銷1内之兩領域溫度,藉由設置在爐體4上之控制裝置丨5, 設在100〜800°C之範圍内,相當爐體4低溫領域的高壓鍋! 内之溶解領域13,是位於橫型閥12之上方,在此領域13内 配置GaN 16,相當爐體4之高溫領域的高壓鍋1内之結晶化 領域14 ’是位於橫型閥12之下方,在此領域丨4雖配置有晶 種1 7 ’但將此配置之位置設定在對流之上流與下流為交差 場所之下方。 發明之效果 如此所得之含鎵的氮化物塊狀單結晶,因結晶性良好, 可以應用在如利用氮化物半導體之雷射二極體等光學元件 基板上。 -18- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公爱)
Claims (1)
- %09|m2459號申請案 中文f請專利範圍替生土(刃年1 j£C8 專利範圍 ^—種氮化鎵塊狀單結晶之製造方法,其係在高壓銷中形 成ί有驗金屬離子之超臨界氨溶劑、在該超臨界氨溶劑 中洛解以炼化法所形成之氮化鎵單結晶塊、 二溶劑溶解前述以溶化法所形成之氛化嫁單結晶:更 南溫及/或更低壓條件下,由溶解上述炼化法所形成之氮 =單結晶塊的超臨界氨溶液,在晶種面上結晶出氮化 2·如申請專利範圍第1項 ……丄“方法’其具備與上述以溶 更 ΐ*=所$成之51化鎵單結晶塊的溶解步驟分開且在 1¾溫及/或更低壓移動超臨界溶液之步驟。 同 中 在 時::二::二第1項之製造方法,其中在高邀銷中 2= 至少2個領域’在低溫之溶解領域 配置上述熔化法所形成之氮 高溫結晶化領域中。 錄早一塊,晶種配置 結 學 4.如申請專利範圍第3項之製造方法,其中 晶化領域之溫度差,是設定在臨 " 能輸送範圍内。 確保㈣界溶液内之化 其中超臨界溶液内 其中溶解領域與結 5·如申請專利範圍第4項之製造方法, 之化學輸送主要是藉由對流來進行。 6·如申請專利範圍第4項之製造方法, 晶化領域之溫度差在1艺以上。⑽016 ⑽016 A8 B8 C8 D8 申請專利範圍 8·如申請專利範圍第1項 _ 貝< I &万法,其中超臨界溶劑是 含有氨或其衍生物者。 9·如申請專利範圍第“員之製造方法,其中超臨界溶劑至 少含有鈉或鉀之離子。 1〇.^申請專利範圍第1項之製造方法,其中晶種至少含有 鎵或其它之III族元素的氮化物結晶層。 11·如申睛專利範圍第1項 甘+ >人 万去,其中在含有晶種之 鎵氮化物之結晶層之表面欠缺密度為106/(;1112以下。 12·如申請專利範圍第i項之製造方法,其中晶種為以溶化 法所形成之氮化鎵單結晶塊。 13. 如申請專利範圍第i項之製造方法,其中在晶種表面中 之(〇〇〇2)面之X線閉銷曲線半值寬(fwhmm 12〇而“ 以下。 14. 如申請專利範圍第!項之製造方法,其中氮化鎵之結晶 化步驟是在100〜8〇〇〇C之溫度下進行。 K如申請專利範圍第i項之製造方法,其中氣化鎵之結晶 化步驟是在300〜600。(:之溫度下進行。 16.如申請專利範圍第i項之製造方法,其中氮化鎵之結晶 化步驟是在400〜550°C之溫度下進行。 17·如申請、專利範圍第1項之製造方法, 其中氮化鎵之結晶 化步驟是在100〜10000 ba之壓力下進行。 18·如申請專利範圍第1項之製造方法, 其中氮化鎵之結晶 化步驟是在1000〜5 500 bar之壓力下進行 19如申請專利範圍第1項之製造方法, 其中氮化鎵之結晶 -2 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 裝 訂 588016 A8 B8化步驟是在1500〜3000 bar之壓力下進行。 2°:Π專利範圍第1項之製造方法’其丁中超臨界溶劑内 =屬離子之漢度是調整到可以確保氮化鎵之特定溶 解度。 21.如申請專利範圍第〗項之製造方法,其中相當於超臨界 ,谷液内之其它成分的驗金屬離子莫爾比控制在工:2〇〇〜 1 · 2之範圍以内。 △=申請專利範圍第丨項之製造方法,其中相當於超臨界 溶液内之其它成分的鹼金屬離子莫爾比控制在1 : 100〜 1 · 5之範圍以内。 ’其中相當於超臨界 爾比控制在1 : 20〜1 23.如申請專利範圍第1項之製造方法 溶液内之其它成分的鹼金屬離子莫 :8之範圍以内。 24· —種製造氮化鎵塊狀單結晶之方法,其係在高壓鍋内將 溶化法所形成之氮化鎵單結晶塊溶解在含有氨與驗金 屬離子之超臨界溶劑中、供給氮化鎵之溶解度為負溫度 係數之超臨界溶液,上述超臨界溶液利用氮化鎵之溶解 度負溫度係數,只在高壓鍋内所配置之晶種面上,選擇 性成長氮化鎵結晶。 25· —種製造氮化鎵塊狀單結晶之方法,其係在高壓鍋内將 熔化法所形成之氮化鎵單結晶塊溶解到含有氨與鹼金 屬離子之超臨界溶劑中、供給氮化鎵之溶解度為正壓力 係數之超臨界溶液,上述超臨界溶液利用氮化鎵之溶解 度的正壓力係數後’只在高壓銷内所配置之晶種面上, -3 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公爱) 588016 六、申請專利範圍 選擇性成長氮化鎵結晶。 26·如申請專利範圍第24或25項之方法,其中上述鹼金屬離 子是以鹼金屬或不含鹵素物質之鹼化劑形態來投與。 27·如申請專利範圍第26項之方法,其中鹼金屬離子為含有 選自Li+、Na+、K+中1種或2種以上者。 28. 如申請專利範圍第24或25項之方法,其中上述晶種係為 以熔化法所形成之氮化鎵單結晶塊。 29. —種結晶氮化鎵之塊狀單結晶之方法,其係溶解到含有 氨與驗金屬離子之超臨界溶劑中、將氮化錄之溶解度有 負溫度係數之超臨界溶液至少放在高壓鍋内之晶種所 配置領域中,上昇到所定溫度或下降到所定壓力,將超 臨界溶液的溶解度調至相對於晶種為過飽和領域,調節 到不會產生自發性結晶漢度以下後,只在高壓銷内所配 置之晶種面上,選擇性成長GaN結晶。 30·如申請專利範圍第29項之方法,在高壓鋼内同時形成所 謂的溶解領域與結晶化領域2個領域,才目當於晶種,依 調整溶解溫度與結晶化溫度,將超臨界溶液進行過飽和 控制。 31. 如申請專利範圍第30項之方法,其中結晶化領域之溫度 設定在400〜600°C之溫度。 32. 如申請專利範圍第29項之方法,其中在高麼銷内同時形 成所謂之溶解領域與結晶化領域2個領域,領域間之溫 差在1 5 0 °c以下。 处如申請專利範圍第29項之方法,其中在高⑽内同時形 6 80 8 5 A B c D 々、申請專利範圍 成所謂之溶解領域與結晶化領域2個領域,領域間之溫 差在100°C以下。 34·如申請專利範圍第29項之方法,其中相對於晶種超臨界 溶液之過飽和調整,設有1個或數個為區分成低溫溶解 領域與高溫結晶化領域之閥,藉由調整溶解領域與結晶 化領域之對流量來進行。 35.如申請專利範圍第29項之方法,其中在高壓鍋中形成所 謂之有特定溫度差之溶解領域與結晶化領域2個領域, 相對於晶種之超臨界溶液的過飽和調整是,利用投入做 為有提高晶種總面積之總面積氮化鎵結晶且以炼化法 所形成之氮化鎵單結晶塊來進行。 -5- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
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