TW546272B - Process for obtaining bulk mono-crystalline aluminum nitride - Google Patents
Process for obtaining bulk mono-crystalline aluminum nitride Download PDFInfo
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- TW546272B TW546272B TW091112458A TW91112458A TW546272B TW 546272 B TW546272 B TW 546272B TW 091112458 A TW091112458 A TW 091112458A TW 91112458 A TW91112458 A TW 91112458A TW 546272 B TW546272 B TW 546272B
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- C30B29/10—Inorganic compounds or compositions
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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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- 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
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Description
546272 A7 B7
五、發明説明(i 超臨界溶液在晶種上 以及氮化鋁塊狀單結 氨之技術,可以成長 發明之技術領域 本發明係有關由 塊狀單結晶之方法 其藉由利用超臨界 晶者。 先前技術 結晶來成長氮化鋁 晶之製造設備,尤 氮化鋁之塊狀單結 應用氮化物之電子光學機器,雖然一般是在與堆積之氣 化物層不同之藍寶石基板上或是碳化矽之基板上來造^ (不定向附晶生長法),但在異質基板上之定向成長,品質 上自然而然地受到限制。 在此期望不僅提供GaN也期望提供AiN之塊狀單結晶的 製造方法。做為製造GaN塊狀單結晶的方法有下面幾個建 議,利用氣相鹵素定向附晶生長法(HVPE) [,,〇pticai patterning of GaN films" Μ. K. Kelly, 〇. Ambacher, Appl. Phys. Lett. 69 (12) (1996) and "Fabrication of thin-film InGaN light-emitting diode membranes’丨 W. S. Wrong, T· Sands,Appl. Phys. Lett. 75 (10) (1999)]、用高壓氮氣之 HNP法[’’Prospects for high-pressure crystal growth of III-V nitrides*丨 S,Poro'vski et al·,Inst. Phys· Conf. Series,137, 3 69 ( 199 8)],為了降低成長步驟中之溫度與壓力,利用超 臨界氨之氨基法["Ammono method of BN,AIN,and GaN synthesis and crystal growth'丨 R. Dwilinski et al·,Proc. EGW-3, Warsaw, June 22-24, 1998, MRS Internet Journal of Nitride Semiconductor Research]及[’’Crystal Growth of _____-4- 本紙張尺度適用中國國家標準(CNS) A4規格(21〇x 297公釐) 546272 A7 B7 五、發明説明(2 ) gallium nitride in supercritical ammonian J. W. Kolis et al·, J. Cryst. Growth 222, 43 1-434 (2001)] 〇 然而,關於AIN塊狀單結晶,D· PETERS雖提議利用超臨 界氨自紹金屬形成氮化鋁結晶之方法(J〇urnal 〇f Crystal
Growth 104 (1990) 41 1-418),但只不過得到包裝用之微小 結晶,在此,近年,在定向附晶生長之用途中,Y、shi等 成功達成在SiC基板上通過A1N緩衝層,以昇華法成長Ain 單結晶之方法(MI J-NSR Vol. 6, Art· 5)。然而,因氣相成 長法畢竟是非平衡化學,要提高結晶之品質自然而然受到 限制。另外,使用半導體之光學元件的壽命特性,主要是 與含轉位密度之活性層結晶性有關,應用A1N基板之雷射 一極官的情形,GaN層之轉位密度以降低到1〇6/(:1112以下為 佳’但應用以往之方法就非常困難達到此目的。 發明所欲解決之課題 在此,本發明之第丨個目的是提供,在晶種上可以形成氮 化鋁塊狀單結晶的方法及裝置。 又,本發明之第2個目的是,成長品質上可以應用之做為 光學元件基板的氮化鋁物塊狀結晶。 此目的之特徵是藉由,在存有含鹼金屬離子之超臨界溶 — 劑的高壓鍋中溶解供料,作成超臨界溶液後,在比溶解溫 ”· 度更高溫度或比溶解壓力更低之壓力下,來自溶液中之氮 一 化鋁在晶種面上結晶,成長氮化鋁塊狀單結晶之方法,來 達成。 為了達成上述目的之本發明第丨構成,係有關在付與氨基 ^紙張尺度適财A4規格(2iqχ 297t) 546272 A7
五 、發明説明( 4 數之超臨界溶液,至少一 配置在南壓鍋内晶種領域中,上昇 声:…度或下降到所定之壓力下,超臨界溶液之、容解 ===領域中’調節到不產生自發結度: 鋼内所配置之晶種面上選擇性的成長氮化 第2構成中’在高壓鋼内同時形成所謂的溶解領域與結晶 /域之2個領域情形,是以針對晶種超臨界溶液藉由調敫 溶解溫度與結晶化溫度來控 日°正 領Μ夕、、w疮π — + ^ J、見不馮且,因此,結晶化 m皿度故疋在400〜 600t之溫度 壓鍋内溶解溫度與結晶化、.θ $夕、0 ¥ 勿4制在同 佔Β仅杜士 日日化/皿度之溫度差以在丨50t以下,較 在峨以下較容易控制。又,針對晶種超臨界溶 a 6和调整是在高壓鍋内設置1個或多數個可以巴八 ΐ低溫溶解領域與高溫結晶化領域”,也^藉由= 洛解領域與結晶化領域之對 9 。 厂堅鋼中形成有特定溫度差之所=2°再者’在特定高 2個領域之情形,針對晶種超:::解領域與心 心m人 裡欠L界各液之過飽和調整,也可 以利用含鋁供料,其是由做為 的謂結晶所投與而成。 &心日種總面積之總面積 同時,在上述第1構成中,μ、+、认入 述鹼金屬離子為投與鹼金屬 或不含齒素物質之鹼化劑形狀, 抖狀做為鹼金屬離子者,是選 自二;:、K+所組成族群中之1種或2種者。又,在超 ”;劑:所溶解之含有紹之供料,雖是以氮化紹為宜, 但也可以使用在超臨界溶液中 ㈣胃。 <tT-谷解生成紹化合物之銘 546272
時,因是平衡反應之故,所 此情形,是使用氮化鋁單結 成長,也可以使用優良品質 又’本舍明方法是依靠在氨基驗性(annTL〇n〇basic)反應者 ’含链之供料是以HVPE法所形成之氮化鋁,或是以化學反 應所形成之Α1Ν ’例如,即使本來在含有氯素之氨基鹼性 超臨界反應,也沒有阻害之問題存在。 利用上述第2構成之情形,做為供料在相對於超臨界氨溶 劑之平衡反應中,雖是使用溶解之氮化鋁或其前驅體,但 針對超臨界氨溶劑也可以使用不可逆反應之,與鋁金屬組 合,在對結晶化之平衡反應無害下,也可以避開過大量之 溶解。 使用上述做為供料之氮化|呂 以可以谷易控制結晶化反應。 晶做為晶種,為了進行選擇性 之晶種。 本發明是提供,同時進行上述第i溶解步驟與第2結晶化 步驟,且在高壓鍋内進行做為第3構成之分離方法。即,提 供其特徵為,得到氮化鋁塊狀單結晶之方法,在高壓鋼中 形成含有鹼金屬離子之超臨界氨溶劑,該超臨界氨溶劑中 溶解含有鋁之供料,對超臨界溶劑在比含有鋁供料溶^時 更π溫及/或更低壓之條件下,氮化鋁自上述溶 溶液中,在晶種面上結晶之方法。 知界 在第3構成中,在含有鋁供料溶解步驟之外,也可以具 在比超臨界溶液更高溫及/或更低壓中之移動步驟。又, 高壓鍋中同時形成有溫度差之至少2個領域,是藉由在低 溶解領域中配置含鋁供料,在高溫結晶化領域^配置晶
裝 訂
546272 A7
來進行。溶解領域I处B ,.^ , /、,、、〇日日化7員域之溫度差,必須設定確保 在起&(¾界溶液内,介風处认、、, 予此輸迗之範圍内,超臨界溶液内之 化學輸送主要是*机、ώ十^ 、 3由對机來進行,通常,溶解領域與結晶 化?頁域之溫度差是名:彳〇 疋在C以上,較佳是在5〜150°c,更好是 在10 0 °C以下。 在本I月中’氮化紹因應用途之需求,可以含有給予體 、、接受體或磁氣處理劑,超臨界溶劑是定義如了,含有氨 或其何生物、做為鹼化劑之鹼金屬離子、至少含有鈉或鉀 之離子另外,含有紹之供料者主要是由氣化銘或其前驅 體所構成,前驅體是選自含有鋁之疊氮基、亞胺基、胺基 亞胺基胺基、氫化物等。 一在本I明中,晶種也可以為氮化鋁,但也可以為不含氧 氣之秸子疋數接近六方晶或是兩面體構造。例如,可以使 用:1C 2 GaN等之單結晶,晶種之表面欠缺密度是使用在 10 /cm以下者為宜,做為其它之晶種者,因可以使用異質 基板’例如’在導電性基板上結晶AiN者,所以使用用途 廣。做為此之候補者,因應用途需求a 〇軸之格子定數為2.8 3.6之L自立方結晶系之铜、鶴,六方最密充填結晶 糸之α — Hf、α 一 Zr ,正方晶系金剛石,Wc構造結晶系 WC、W2C ’ ZnO構造結晶系 a -Sic、TaN、NbN、A1N,六 方晶(P6/mmm)系 AgB2、AuB2、HfB2,六方晶(P63/mmc)系 γ — MoC、ε — MbN等。體心立方結晶系之鉬、鎢是以使 用自[1,1,1 ]方向切出之晶種為宜。 在本發明中,氮化鋁之結晶是可以在100〜8〇〇。〇之範圍 ____ -9- 本紙張尺度適用中國國家標準(CNS) Α4規格(210 X 297公爱) 546272 A7
進行,但較佳也可以在400〜6〇〇。〇之溫度進行,又,氮化 鋁之結晶化是可以在100〜1〇〇〇〇 bar進行,但較佳是在1〇⑽ 〜5 500 bar,最好是以在1 500〜3〇〇〇 bar之壓力進行較佳。 超臨界溶劑内鹼金屬離子之濃度,是調整確保可以供料 及氮化鋁的特定溶解度,針對超臨界溶液内之其它成=, 驗金屬離子之莫爾比控制在丨:2〇〇〜n 2,較佳者為1 ·· i 〇〇 〜1 · 5,更好為在1 ·· 2〇〜1 ·· 8之範圍以内者為宜。 同時’本發明是有關在含有付與氨基鹼性1種或多數鹼化 劑之超臨界氨溶劑中產生化學輸送,可得氮化鋁單結晶成 長,氨基鹼性結晶生成技術,為了認可原本的高技術,在 本發明中,所使用之以下用詞,是可以用以下之本案說明 書來定義其意思。 μ 氮化鋁,並不限上述氨基鹼性結晶成長技術,可以含有 雜質者。 氮化紹之塊狀單結晶,是指藉由M〇CVd或是HVPE等之 定向附晶(epi)成長方法,可以形成如led或LD般光及電子 令件的氮化鋁單結晶基板。在藍寶石基板上成長之情形是 必須有緩衝層,但使用A1N基板時,無緩衝層也可以成長 良質之氣相成長膜。在本發明方法所得之a1n基板的半值 寬是在2分鐘(120 arcsec)以下,較佳是在!分以下。在藍寶 石基板上成長之A1N因半值莧為4分鐘之故,所以品質之提 向極為優異。 又,A1N基板到200 nm為止不會光吸收,因GaN基板是在 短波長區之365 nm吸收,所以A1N基板做為(JV—LED之基
546272 A7 ------ B7 五、發明説明(8) " " " 板可望提问光輸出,又,因a in基板是放熱性,所以可適 於做電力零件基板。再者,使用A1N基板的話,可能成長 问此日日之AlGaN ’若有雷射元件的話,縱方向之關閉變得 很好。 氮化紹之可驅物質,是指用來代替氮化鋁之供料物,至 少要有結’要的話含有鹼金屬、XIII族元素、含氮氣及/或 疋氫氣或其混合物,金屬鋁、其合金或金屬間化合物、其 氫化物、胺基類、亞胺基類、胺基一亞胺基類、疊氮類等 ,以下定義是所謂的在超臨界氨溶劑中形成可溶解之鋁化 合物。 含链之供料,是指所謂之氮化鋁或其前驅物質。 超e品界氨溶劑者是認為,至少含有氨之超臨界氨溶劑, 疋含有為了溶解氮化鋁之丨種或多數之鹼金屬離子。 鹼化劑者,是所謂的在超臨界氨溶劑中,供給為了溶解 氮化鋁之1種或多數之鹼金屬離子者,在說明書中有具體例 示。 含鋁之供料的溶解,是指上述供料在超臨界溶劑之相對 溶解性鋁化合物,例如稱取得可逆性或非可逆性鋁錯體化 合物形態之過程。鋁錯體化合物者,是與N ^^ 生物顧2',般之配位,以紹為配位中心所== 了 化合物。 a肢 超臨界氨溶液,是指溶解上述超臨界氨溶劑與含有鋁供 料,產生溶解性鋁化合物之意。依吾等之經驗,可以預測 在充分高溫高壓下存在著固體氮化鋁與超臨界溶液間之平 -11 -
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在比溶解領域更高溫度來達成較佳。 曰晶種在本案說明書中雖有例示,但也提供進行氮化_ 日日化之領域,因其支配結晶之生長〇拼 、、、口 結晶相同,能選擇品質良好者。 Μ與所成長之 自發之結日日日(Spontaneous erystallizatiGn)者,是指 和㈣氣溶液形成氣化紹的核及成長,纟高壓銷: -邊都會產生,這是不被期望之步驟,包含在晶種表面之 ,同方向性之成長(disoriented gr㈣帅若其它纟數_ 話,隨溫度之上昇,溶解界限及自發結晶界限是 般,有減少之傾向。 所不 的成長、結 成長中不可 對晶種之選擇性結晶,是指所謂之非自發性 晶是在晶種上進行之步驟,為達成塊狀單結晶 欠缺之步驟,為本案發明方法之一。 /高壓鍋,是不管形態、為了進行氨鹼性結晶成長之閉鎖 系反應室。又,在本發明中使用之氮化鋁顆粒為成形粉末 狀者,稱為燒成物,為極高密度者,例如可以取得99.8% 者0 同時’本案發明實施例中之高壓鍋内的溫度分布,因是 在沒有超臨界氨存在下,測定空高壓鍋者,並非實際之超 臨界溫度。又,壓力是直接測定的,是由最初導入之氨量 、南壓鋼之溫度及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 明是提供其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、投入備有加
546272 A7 B7
五、發明説明(11 熱裝置5或冷卻震置6之爐體4中,之氮化紹塊狀單結晶的生 產設備。
裝 上述爐體4,是具有相當於高壓鍋丨之結晶化領域14、備 有加熱裝置5之高溫領域,及相當於高壓鍋丨之溶解領域u ,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 ,是相當於高壓鍋丨之結晶化領域14、備有加熱裝置$ 或冷卻裝置6之高溫領域及相當於高壓鍋丨之溶解領域u , 備有加熱裝S 5或冷卻裝置6之溫領域。冑流控制管理裝 置2,是區分成結晶化領域14與溶解領域丨3,在中心或周圍 由一張或多張之有孔洞橫型閥12所構成。在高壓鍋丨内,是 將供料16配置在溶解領域13中,晶種Π配置在結晶化領域 14中’ 與14領域間之超臨界溶液的對流是依控制管” 置2來設定所構成,其特徵為溶解領域13是位在橫型閥J 之上方,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表示實施例”中’ p=常數中,因時間之變化,高尿 鍋内之溫度變化圖。 &
圖2表不貫施例2)中,j:丁 一受奴A J 在1 一 $數中,因時間之變化,高 壓鍋内之壓力變化圖。 圖3表示實施例3)中,固定容量中,因時間之變 取 鍋内之溫度變化圖。 圖4表示實施例4)中,因時間之變化,高墨鍋内之 化圖。 又 圖5表示實施例5)中,因時間之變化’高壓鍋内之溫度變 -14 - 546272 A7
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546272 五 Λ發明説明( 14 裝 度之減少係數(負的溫度係數)。利用此關係,在溶解度高 乂條件下,進行氮化鋁之溶解,在溶解度低之條件下,進 行結晶,可以成長氮化紹之塊狀單結晶。此負溫度係數, 是指在產生溫度差之情形,氮化紹之化學輸送為自低溫容 2領域邁向高溫之結晶化領域。其次,藉由適當變化加熱 寺條件來進行,藉由造成氮化紹之過飽和溶液,在晶種面 上成長結晶。本發明之方法是,在晶種面上可以成長氮化 鋁之塊狀單結晶,在由氮化紹或碳化砂等結晶所成之晶種 上,可得到塊狀單結晶層是得到氮化紹的化學理論成長。 士述之單結晶’因是在含有驗金屬離子之超臨界溶液:成 因此所得之單結晶也含有01 ppm以上之驗金屬。又, 為了防止設備腐钱需保持超臨界溶液之驗性,期望 中不要投入函素物質。再者’氮化紹之塊狀單結晶中; 以接受處理濃度10】7〜102丨/cm3之給 m 丁 (Sl、0等)、接受體 (Mg、Zri寺)、磁性物質(Mn、Cr等),葬士 /上 ㈣卜 稽由接受處理可以改 •交氮化鋁之光學、電性、磁性特性。在 ^ ^ 共匕之物理特性中 ’成長之氮化銘塊狀單結晶表面之欠缺宓 ^ e . 5 , 人尺在度是在l〇6/cm2以 下,較佳疋在10 /cm-以下,更佳是在1〇4 ,mi以下。又,斜 (0002)面之X線半值寬是在6〇〇 arc Λ下’較佳是在300 arcsec以下,更佳是在60 arcsec以下成具 ^ .„ a θ ^ _ /戍長。最佳之塊狀Α1Ν 早結晶疋,可以在欠缺密度為l〇4/cm2 , 卜’對表面(0002) 之X線測定半值寬為60 arcsec以下成長。 貫施例 使用導入有2台掛鋼,容積為10.9 - <向壓加壓鍋[Η· -17 本紙張尺度適用中國國家標準(CNS) Α4規格(210 X 297公釐) 546272
Jacobs, D. Schmidt, Current Topics in Material Science, v〇l.8,ed. E. Kaldis (north—Holland, Amsterdam,19810, 381設計)。可以使用之供料為以HvpE法生成之氮化鋁薄板 ,氮化鋁粉體燒結品(德山蘇打製)。做為晶種者是可以使 用以HVPE法所得之AIN、GaN、及SiC。 做為超臨界狀態之氨溶液之形成及結晶方法,以下面之 例子來表示。同時,除了 T丨,丁2〜丁5可以設定在4〇〇〜6〇〇 °c之範圍。 ① 在高壓鍋中投入〇·72克純度為4N之金屬鉀。再投入4.81 克氨後,緊閉高壓鍋,藉由下面之溫度控制(圖2)形成超臨 界氨溶液,即加熱到丁2,高壓鍋内之壓力為2 kbar。數曰後 ’溫度加熱到丁4 ’壓力保持在2 kbar之狀態,再放置數曰, 使結晶(圖1)。 ② 在高壓鍋中投入0.82克純度為4N之金屬鉀。再投入5.43 克氣後’緊閉向壓銷。將高壓鋼投入爐中,加熱到5 〇 〇 , 高壓鍋内之壓力為3.5 kbar,形成超臨界氨溶液,數日後, 壓力降到2 kbar·,溫度保持在500°C之狀態,再放置數曰, 使結晶(圖2)。 ③ 在高壓鍋中投入0.6克純度為4N之金屬鉀,再投入4克 氨後,緊閉高壓鍋。將高壓鍋投入爐後,加熱到Τι,形成 超臨界氨溶液,2天後,溫度加到500°C,加壓到2 kbar,此 狀態再放置4天使結晶(圖3)。 ④ 在容積35.6 cm3之高壓加壓鍋1(圖6)中,以HVPE法所 得之A1N同量分開配置在溶領域1 3與結晶化領域1 4中,其 -18-
本纸張尺度適用中國國家標準(CNS) A4規格(210X 297公釐) 546272 A7 ___B7 五、發明説明(16 ) 次投入2 · 4克純度為4 N之金屬卸,其次投入1 5 · 9克之氨水 (5N),緊閉高壓鍋1,投入爐體4内,加熱到T3,高壓鍋内 之壓力約為2 kbar,1天後,結晶化領域丨4之溫度增加到丁4 ,將溶解領域1 3之溫度降到T 2,在此狀態之高壓鍋1再放置 6天(圖4)。 ⑤ 在容積36 cm3之高壓加壓鍋1(圖6)之溶解領域13中,配 置以HVPE法所得之A1N所做成之供料,投入〇·47克純度為 4Ν之金屬鉀,在結晶化領域14中同樣配置以HVPE法所得之 Α1Ν晶種,其次投入16.5克之氨水(5Ν),緊閉高壓鍋1。將 高壓鍋1投入爐體4中,加熱到Τ4,高壓鍋内之壓力為3 kbar ,:I天後,溶解領域13之溫度降到T3,將結晶化領域14之溫 度增加到A,此狀態之高壓鍋再放置8天(圖5)。 ⑥ 在容積3 5.6 cm*5之高壓加壓鋼1之溶解領域1 3中,配置 以HVPE法所得之A1N板所成之供料,在結晶化領域14中配 置以HVPE法所得之GaN晶種,再投入〇·4 1克純度為3N之金 屬鉀,其次投入14.4克之氨水(5Ν),緊閉高壓鍋1。將高壓 锅1技入爐體4中,結晶化領域之溫度加熱到,溶解領域 之溫度加熱到Ts,所得壓力為2.6 kbar,將此狀態之高壓鍋 放置8天(圖7)。 有關本發明之方法,是利用在超臨界溶劑内生產含氮化 紹之塊狀單結晶設備來進行,此設備之主要部分是由生成 超臨界溶劑之高壓鍋丨,與高壓鍋丨中可以在超臨界溶液内 控制化學輸送的控制裝置2所組成,將上述之高壓鋼1投入 備有加熱措施5或冷卻措施6之爐(2台)體4的室内3中,為了 _— _19_ 本紙張尺度通用中國國家標準(CNS) A4規格(21GX 297公爱) ' - 546272
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中,在爐體4與爐床8之周圍以圍繞鋼帶9 來固定,爐床8與爐體4在回轉台1〇上設置,藉由特定之角 度栓住固定裝置1 1加以固定,可以控制高壓鍋丨内之對流種 類與對流速度。將投入爐體4之高壓鍋丨内超臨界溶液之對 流’區分成結晶化領域丨4與溶解領域丨3,在中心或周圍設 定一個或數個有孔洞之橫型閥12所組成的對流控制裝置2 。將高壓鍋1内之兩領域溫度,藉由設置在爐體4上之控制 扃置1 5,ό又疋在1〇〇〜8〇〇。〇之範圍内,相當爐體4低溫領域 的高壓銷1内之溶解領域13,是位於橫型閥12之上方,在此 領域1 3内配置供料丨6。相當爐體4高溫領域的高壓鍋内之結 晶化領域14是,位於橫型閥12之下方,在此領域14中雖配 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
如此所得之含氮化鋁塊狀單結晶,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。例如形成做為 A1N基板/under dope AlGaN/Si—AlGaN/ under dope AlGaN/Mg — GaN之定向附晶成長構造,自AIN 基板側邊取得光的話,AlGaN之A1混晶若高的話,短波長 之光感度提高,不僅在360 nm程度之短波長,若是 Al0.5Ga〇.5N的話,到28〇 ηιτ^ι度都有光感度。此基板因是 Α1Ν之故’有可能高混晶在GaN基板則是困難值。 _ -20- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
Claims (1)
- 本口 624 5 A BCD 申請專利範圍 1· 一種氮化鋁塊狀單結晶之製造方法,其係在高壓鍋中形 成含有驗金屬離子之超臨界氨溶劑、在該超臨界氨溶劑 中溶解έ鋁ί、料、以比超臨界溶劑溶解含紹供料時更高 溫及/或更低壓條件下,自溶解上述供料之超臨界溶液在 晶種面上結晶氮化鋁出來。 2. 如申請專利範圍第丨項之製造方法,其具備與上述供料 溶解步驟分開且在更高溫及/或更低壓移動超臨界溶液 之步驟。 3. 如申請專利範圍第}項之製造方法,其中在高壓鋼中同 時形成至少有2個有溫度差之領域,在低溫之溶解領域 中配置含紹供料’並在高溫之結晶化領域中配置晶種。 4. 如申請專利範圍第3項之製造方法,其中溶解領域與結 晶化領域之溫度差’是設定在能確保於超臨界溶液内之 化學輸送之範圍内。 其中超臨界溶液内 其中溶解領域與結 5·如申凊專利範圍第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11以上。 其中氮化鋁是可以 7·如申請專利範圍第1項之製造方法 έ有給予體、接受體或磁性之處理劑 8. 如申請專利範圍第1項之製造方法,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i項之製造方法,其中超臨界溶劑至 少含有鈉或_之離子。 -21 - 本紙張尺度適财X 297公釐)546272 申請專利範圍 •如申凊專利範圍第1項之势生 . e ^ ^ 乐貝之衣坆方法,其中含鋁供料主要 疋由氮化鋁或是其前驅體所構成。 11·如申請專利範圍第10項製 人 ^戶、心衣k方法,其中前驅體是選自 :有鋁之疊氮物、亞胺基、醯胺基亞胺基、醯胺 物0 12·:πί利範圍第1項之製造方法,其中晶種至少含有 s鋁或其它之111族元素的氮化物結晶層。 如申請專利範圍第1 萝 # Λ 吊貝之衣4方法,其中在含晶種之氮 、,呂之結晶層中之表面欠缺密度為106/em2以下。 14·如申請專利範圍第1項之掣 图珩1貝之衣k方法,其中氮化鋁之結晶 匕是在400〜6〇〇。〇之溫度進行。 15.如:請專利範圍第!項之製造方法,其中氮化鋁之結晶 匕疋在1000〜55〇〇 bar,較佳在15〇〇〜3〇⑽bar之壓力下 進行。 A如申請專利範圍第1項之製造方法,其中超臨界溶劑内 之驗金屬離子濃度是調整到可以確保供料與氮化紹之 特定溶解度。 /合液内之其它成分的鹼金屬離子莫爾比,控制在1 : 200 1 · 2,較佳在丨·· 100〜丨·· 5,更佳在1 ·· 2〇〜 々々 m Α · Ο 乾圍以内。 18·:種氮化鋁塊狀單結晶之生產設備,其備有生成超臨界 溶劑之高壓銷i、纟上述高壓㉟中設置有^空制對流之裝 置 彳又入備有加熱裝置5或冷卻裝置6之爐體4中。 22- 本紙張尺度適财_家解(CNS) M規格τ^Χ297公董)546272 A8 B8 C8 - ----—- D8 六、申請專利範圍 19·如申請專利範圍第18項之生產設備,其中爐體*含有高 /凰領域其具備適合高壓鍋1之結晶化領域14之加熱裝置 5 ’以及低溫領域其具備適合高壓鍋1之溶解領域13之加 熱裝置5或冷卻裝置6。 2〇·如申請專利範圍第18項之生產設備,其中爐體4含有高 溫領域其具備適合高壓鍋1之結晶化領域14之加熱裝置 5或冷卻裝置6,以及低溫領域其具備適合高壓鍋丨之溶 解領域1 3之加熱裝置5或冷卻裝置6。 21.如申請專利範圍第丨8項之生產設備,其中對流控制裝置 2 ’是區分成結晶化領域14與溶解領域13,在中心或周 圍由1張或多張有孔洞之橫型閥丨2所構成。 2· 士申明專利範圍苐1 8項之生產設備,其中高壓鋼1内, 在供料16溶解領域13中,將晶種17配置在結晶化領域14 上,藉由控制裝置2設定13與14領域間之超臨界溶液的 對流。 · 23. 如申明專利範圍弟2 1項之生產設備,其中溶解領域1 3是 位於;^型闊1 2之上方’結晶化領域1 4是位於橫型閥1 2之 下方。 24. 種以造氦^化铭塊狀單結晶之方法,其係在高壓鋼内含 有溶解銘供料於含有氨與鹼金屬離子之超臨界溶劑中 、供給氮化鋁之溶解度有負溫度係數的超臨界溶液,上 述超臨界溶液利用氱化鋁之溶解度負溫度係數,只有在 高壓鍋内所配置之晶種面上,選擇性成長氮化鋁結晶。 25·種製造氮化铭塊狀單結晶之方法,其係在高壓鋼内溶 -23- 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公釐) 546272 六、申請專利範圍 解鋁供料於含有氨與鹼金屬離子之超臨界溶劑中、供給 鼠化鋁之溶解度有正壓力係數的超臨界溶液,上述超臨 界溶液利用氮化鋁之溶解度正壓力係數,只有在高壓= 内所配置之晶種面上,選擇性成長氮化鋁結晶。 26·如: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盥。 27·二申請專利範圍第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,其中超臨界溶劑所 溶解之含鋁供料是由在氮化鋁或在超臨界溶液中生成 可溶解之鋁化合物之鋁前驅體所組成。 29. 如申請專利範圍第24或25項之方法,其中含铭供料為以 HVPE所形成之氮化链或是以其它化學反應所形成之氮 化鋁且含有對氨基鹼性超臨界反應無害之元素。 3〇·如申請專利範圍第24或25項之方法,^中超臨界氨溶液 之形成,為含鋁供料在超臨界氨溶劑之平衡反應中所溶 解的氮化鋁,與在超臨界氨溶劑為不可逆反應之鋁金屬 所組成。 31.如申請專利範圍第24或25項之方法,其中上述供料為氮 化鋁燒結體。 32·如申請專利範圍第24或25項之方法,其中上述晶種是氮 化鋁單結晶。 33.種氮化|g塊狀單結晶之結晶方法,其係溶解在含有氨 與鹼金屬離子之超臨界溶劑中、將氮化鋁之溶解度有負 -24- 本紙張尺度適财_家料(CNS) A4規格?210X297公釐) 546272 申清專利祀園 溫度係數之超臨尺、、六 置之領域中 '合液,至少放在高壓鍋内之晶種所配 綠上昇到所定溫度〇降到所定壓力,將超 =生=解度調至對晶種為過飽和領域,調節到不 曰曰=發性結晶之濃度下後,只在高㈣内所配置之 :,上’選擇性成長氮化紹結晶。 .二範圍第33項之結晶方法,其編鋼内同時 7、域與結晶化領域等2個領域’針對晶種之超 π:::和控—度與結晶化溫 35·1°Π:Ι?圍第34項之結晶方法,其中結晶化領域之 /皿度故疋為400〜60(rc。 36·:;Γ=範圍第34項之結晶方法,其中在高壓銷内同 /成冷解領域與結晶化領域等2個領域, 度差是在Hot以下,較佳是保持在·c以下Μ之恤 37· ^申請專利範圍第34項之結晶方法,其中針對晶種 甌界溶液過飽和調整’是設計有1個或多數個用來區分 成低溫溶解領域與高溫結晶化領域之閥,以刀 域與結晶化領域之對流量。 …貝 38.如申請專利範圍第34項之結晶方法,其中在高壓鋼中形 成有特定溫度差之溶解領域與結晶化領域2個領域,在 對日日種之超8品界溶液過飽和調整是,利用投與有提古曰 種總面積之總面積氮化鋁結晶之含鋁供料來進行。 -25-
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TWI402217B (zh) * | 2005-07-08 | 2013-07-21 | Univ California | 使用高壓釜於超臨界氨中成長第三族氮化物晶體之方法 |
US8709371B2 (en) | 2005-07-08 | 2014-04-29 | The Regents Of The University Of California | Method for growing group III-nitride crystals in supercritical ammonia using an autoclave |
US9551088B2 (en) | 2005-07-08 | 2017-01-24 | The Regents Of The University Of California | Method for growing group III-nitride crystals in supercritical ammonia using an autoclave |
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