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TW420725B - Improved process for purification of organometallic compounds - Google Patents

Improved process for purification of organometallic compounds Download PDF

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Publication number
TW420725B
TW420725B TW87121035A TW87121035A TW420725B TW 420725 B TW420725 B TW 420725B TW 87121035 A TW87121035 A TW 87121035A TW 87121035 A TW87121035 A TW 87121035A TW 420725 B TW420725 B TW 420725B
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item
precursor
purification
compound
organic
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TW87121035A
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English (en)
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Barry Albert Leese
Megan S Ravetz
Lesley M Smith
Simon A Rushworth
Ravi Kanjolia
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Epichem Ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4402—Reduction of impurities in the source gas
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Description

420725 Α7 Β7 經濟部中央標隼局員工消費合作社印製 五、發明説明（丨） 本發明乃有關於化學氣相蒸著法技術中所使用有機金 屬化合物之純化方法，尤其是三甲基絪的純化。 有機金鼷化合物，如三甲基絪，在Μ化學氣相蒸著法 技術，如金鼷有機氣相嘉晶（MOVPE )—被用當前驅物以 便附著一金臑薄膜於固體被覆物上，此金靨薄膜對於使用 於電子及光電產業中的半導體之製造是很重要的。 近來，高飽含量的合金組成*如AlGalnP，特別被發 展用來製造高亮度的發光二極體*它比傳統發光二極體較 省電，又可製成數種不同顔色，及衛星所使用的絪糸太陽 電池，然而，此種薄膜對於在蒸著過程可能引入的微量含 氧物種是特別敏感，存在於前驅物的典型不純物包括二乙 / .V . /V 基醚，三甲基絪-二乙基醚互屬錯合物，二甲基-甲氧基絪 I ，甲基-二甲氧基絪，及三甲氧基絪。 可能被引人前驅物的含氧物種之來源有，如用以製造 前驅物的原料或其製程中所使用之溶劑，如醚類，亦可能 自空氣中進入這些來源的容器或鼓泡器與有機金屬化合物 反應產生烧氧化物，而協助傳送已氣化前驅物至被覆物的 載送氣體也可能含有氧，與有機金鼷合物反應產生焼氧 化物。 存在於有機金屬前驅物之含氧物會随著載送氣釋之輸 送進入反應器，此反應器在裂解金靥化合物使成一金屬薄 膜之同時亦很容易將氧帶入，用此遭污染的薄膜製成的半 導體，其晶級是非常的低劣。 本發明的目標即是要克服這種有機金屬前I區物受到氧 (請先閱讀背面之注意事項再'填寫本頁) 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐）il 42^725 A7 B7 五、發明説明（1 化物污染之問題，進而改善金屬薄膜之品質，特別是高亮 度的發光二極體及太陽電池之甩途。 因此•本發明提供一種純化有機金屬前驅物的方法， 藉由化學氣相蒸著法技術製造金麋薄膜，其中之步驟乃令 前驅物置於一容器内，導入一鎮基物，令前驅物氣化之前 驅物減少氧化物的污染。 本發明即是含有更進一步的步驟將前驅物的金屬蒸著 於被覆物上。 一般來說，前驅物是在鼓泡器中氣化，然後Μ載送氣 體，如氦氣，傳送至被塗物上。氣基溶劑較常被放入鼓泡 器，它較易與含氧物反應而自蒸氣中脫雛，因此可使前驅 物減少氧化物的污染，而此含氧物蒸氣壓的降低，可防止 其在載有前驅物的載送氣體中之傳輸，進而防止導入蒸著 薄膜内。 使用低揮發性的氨基溶劑較不易自鼓泡器被載送氣體 送出*同時，較未氣化前驅物的密度為低的鎮基溶劑亦較 易為所用，此氣基溶劑亦常置於輸送載送氣體及氣化前軀 物之管子底部上方，期使前驅物能與摄基溶劑混合接觸之 經濟部中央標準爲貝工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 較受本發明垂愛的氨類是三烧基氨，尤其是Ν-Ν二甲 基十二基氣。 本發明特別適合Μ三甲基銦當前驅物製造姻薄膜的方 法，但其他絪化合物，例如1至4個碳的R In，亦可使用於 類似的方法；本方法也Μ用來蒸著其他金屬薄膜或混合金 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） 420725 經濟部中央標隼局負工消費合作社印製 A7 B7__五、發明説明（θ ) 屬薄膜，特gfj是鼷Μ及屬v金廳薄膜，女口AlInAs與AlGalnP Ο 讁來自鼓泡器含微量氧污染物的前驅物通過鎮溶液， 這種在鎮基物裡的有機金屬前驅物溶液可用來當做捉拿者 K驅除氧不純物。 本發明提供化學氣相蒸著法技術製造低氧污染物金屬 , 薄膜，這種高品質薄膜特別適合做為太陽電池及高密度發 光二極體之裝置，瑄種薄膜可由各種化學氣相蒸善技術製 得，特sa是金屬有機氣相晶晶（MOVPE)。 本發明將以下面諸例更進一步敘述。 r }. 例一 [ΙΪ 取50克三甲基銦樣品，先MFTNMR分析其酸不純度，， 置於一玻璃鼓泡器内，再加入10克N-N二甲基十二基氧， 徐徐攬拌後，靜置12小時，再用高純度氮氣以每分鐘1公 升的速率通過下傾腳，將帶出的三甲基銦集於一玻璃接收 器，並冷卻至-2〇r： ; MFTNMR分析所收集的三甲基絪，並 與先前的比較，分析發琨先前的樣本含56PPM二甲基醚， 經處理的樣品在此儀器的精確度下無法測出醚的含量，其 精確度為7PPM。 例二 取200克三甲基銦樣品，先MFTNMR分析其含氧物種， 然後分成二份：第一份100克置於一含有17克N-H二甲基 十二基氣且經完全標準清洗過之S/S鼓泡器*第二份1〇〇克 則置於一相同完全標準清洗過之回流鼓泡器；然後，將此 (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）厶 42Q725 A7 B7 五、發明説明（斗） 二樣品置於一*CVT MOCVD反應器’各自做為生長A1 InAs露 晶薄_的姻來源原料，所有其他前驅物及蒸著條件均保持 一定。所得二種薄膜分析其載送氣體濃度*接著msims( Secondary Ion Mass Spectrometry )測誠嵌於薄膜的氧 Ο 初始固體三甲基因，从FTNMR分析含酸量為40PPM。 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央櫺準局員工消費合作社印製 此結果很清楚表示，用Μ氣化三甲基絪的鼓泡器，若 有:基物導入，可以使氣化的前驅物降低其含氧物，進而 夜蒸著中製得較純的金靥薄膜，此乃因氨基物易與含氧物 作用，降低其蒸氣麼，進而胆礙載送氣體將其送至反應器 Ο 氧量分析 載送氣體濃度 (cm ) SIMS (cm ) 第一樣品 7X el5 <1x1077 (detection limit) 第二樣品 4 X el6 4x 1017 本紙浪尺度適用中國國家標準（CNS ) Α4規格（210X 297公釐）y

Claims (1)

  1. AS 公告本ρπ25 I__ P申請專利範園 1. 一種有機金靨化合物之純化改菩方法•藉由化學氣 相蒸著法技術製造金屬薄膜*其中之步驟乃令前驅物置於 一容器内，導入一截基物，令前驅物氣化並輸送雛開此容 器·此截基物可以鑲氣化之前驅物減少氧污染〇 2. 如申請専利範圍第1項所述有機金臛化合物之純化 改菩方法*包含蒸著此前驅物金靨薄膜於被播物上之步驟 〇 3. 如申誚専利範画第1項或第2項所述有機金靥化合 之純化改菩方法•歧氣基物具低揮發性。 4. 如申謫專利範圍第3項所述有機金靨化合物之純化 改巷方法，此氛基物比未氣化之前驅物密度低。 5. 如申辅專利範園第4項所述有機金靨化合物之純化 改菩方法•此截基物是三综基® 〇 6. 如申請專利範圍第5項所述有機金鼷化合物之純化 改善方法，肋截基物是N-N二甲基十二基氣。 7. 如申請専利範圍第2項或第4項或第5項或第6項 所述有機金匾化合物之純化改菩方法，此氣化之前驅物是 藉一戟送氣艘被送至被授物上。 8. 如申請專利範園第7項所述有機金围化合物之純化 改善方法· 氛基物是以溶液狀態置於容器内•使琴與含 氣物反應•逍而自蒸氣中將其驅除。 9. 如申辅専利範圃第8項所述有機金膈化合物之純化 改普方法，此氣基物是置於輸送載进氣雅及氣化前驅物之 管子底部上方。 本紙張U4用中家#準（CNS ) Λ4規格（210X297公釐）f • *~ • .·>^ (請先E讀背面之注意事項再填寫本頁) 經濟部中央慄準曷員工消费合作.ti印装 ^20725 Α% Β8 C8 D8 經濟部中央標隼局貝工消费合作社印製 六、申請專利範園 10. 如申請専利範圍第1項所述有機金屬化合物之純化 改畚方法*此前驅物是絪的有機金觴化合物。 11. 如申請専利範醣第10項所述有機金靨化合物之純化 改善方法，此前驅物是RIn，R為1至4個碳。 12·如申請專利範画第1〇項所述有機金靨化合物之純化 改畚方法，此前驅物是三甲基姻。 13♦如申誧専利範圃第1項所述有機金觸化合物之純化 改菩方法，製造屬m及雇V的金靨薄膜。 14·如申請專利範圍第1項所述有機金屬化合物之純化 改普方法•此化學氣相蒸著法技術乃金屬有機氣相磊晶（ M0VPE ) 〇 15. 如申誚專利範園第1項所述有機金匾化合物之純化 改窖方法•鑲來自鼓泡器含微量氣污染物的前驅物通過氨 溶液，埴種在截基物裡的有機金觸前驅物溶液可用來當做 捉韋者，Μ驅除氧不純物〇 16. 如申請専利範晒第1項所述有機金鼷化合物之純化 改普方法，蒸著之金臁薄膜所製得的高密度發光二極雅〇 17. 如申請專利範圃第1項所述有機金圈化合物之純化 改善方法•蒸著之金雇薄膜所製得的太陽霣池。 (請先閲讀背面之注意事項再填寫本頁) 訂 ^. 本紙張尺度逋用中國國家榣率{ CNS ) Α4规格（210X 297公釐）f
TW87121035A 1998-11-13 1998-12-17 Improved process for purification of organometallic compounds TW420725B (en)

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US8215292B2 (en) 1996-07-17 2012-07-10 Bryant Clyde C Internal combustion engine and working cycle
US6956127B2 (en) 2002-01-17 2005-10-18 Shipley Company, L.L.C. Alkyl group VA metal compounds
US7178492B2 (en) 2002-05-14 2007-02-20 Caterpillar Inc Air and fuel supply system for combustion engine
US6688280B2 (en) 2002-05-14 2004-02-10 Caterpillar Inc Air and fuel supply system for combustion engine
US7201121B2 (en) 2002-02-04 2007-04-10 Caterpillar Inc Combustion engine including fluidically-driven engine valve actuator
US7191743B2 (en) 2002-05-14 2007-03-20 Caterpillar Inc Air and fuel supply system for a combustion engine
US7252054B2 (en) 2002-05-14 2007-08-07 Caterpillar Inc Combustion engine including cam phase-shifting
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