TW200920490A - A vessel for providing organometallic compound - Google Patents

A vessel for providing organometallic compound Download PDF

Info

Publication number
TW200920490A
TW200920490A TW097132869A TW97132869A TW200920490A TW 200920490 A TW200920490 A TW 200920490A TW 097132869 A TW097132869 A TW 097132869A TW 97132869 A TW97132869 A TW 97132869A TW 200920490 A TW200920490 A TW 200920490A
Authority
TW
Taiwan
Prior art keywords
container
carrier gas
organometallic compound
carrier
compound
Prior art date
Application number
TW097132869A
Other languages
Chinese (zh)
Inventor
Toshimitsu Abe
Kenichi Sawara
Original Assignee
Sumitomo Chemical Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Chemical Co filed Critical Sumitomo Chemical Co
Publication of TW200920490A publication Critical patent/TW200920490A/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06Chemical 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 metallic material
    • C23C16/18Chemical 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 metallic material from metallo-organic compounds
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/455Chemical 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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563Gas nozzles
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
    • H01L21/28556Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD

Abstract

Provided is a vessel for providing organometallic compound, wherein a front end of a carrier gas introducing pipe is disposed in an upper portion of the vessel, and a front end of a carrier gas leading-out pipe is disposed in a lower portion of the vessel, wherein the vessel is filled with carrier-carried organometallic compound formed by covering an organometallic compound which is in solid state at room temperature on a carrier which is inert against the organometallic compound, the vessel for providing organometallic compound being characterized in that, in a case that the vessel is provided vertically, the front end of the carrier gas introducing pipe is such configured that the carrier gas supplied from the front end of the carrier gas introducing pipe is ejected in a direction roughly perpendicular to a central axis of the vessel.

Description

200920490 九、發明說明: 【發明所屬之技術領域】 . 本發明係有關有機金屬化合物供給容器。更詳細言 •之三本發明係有關一種有機金屬化合物供給容器,其中充 =者經擔體承载之有機金屬化合物,該經擔體承载之有機 屬。物為由常溫下為固體之有機金屬化 有機金屬化合物呈情性之擔體而成者。 覆於對 【先前技術】 i在電子工業中,有機金屬化合物係作為例如化合物半 導體之原料而使用。名雷; 3 用在電子工業中使用有機金屬化合物 :通氫氣等載體氣體(carriergas 機金屬化合物接觸,並作為 一有 w m 作騎機金屬化合物之飽和蒸氣而 予以v引使用於氣相成長裝置等。 #用:吊’皿(至溫)下為固體之有機金屬化合物時,盘 體金屬化合物之情形不同,即使流通载體氣 通路卜财機金屬化合物+形絲體氣體流 X:二在::⑽而變成小粒徑的固體有機金屬化合物 :ί積在μ底部’結果固體有機金屬化合物盘載體氣體 無法充分接觸,而具有不能以,、曲Λ U體乳體 ,,^ 女疋/辰度供給有機金屬介人 物至氣相成長襞置之缺點。 錢孟屬化口 關於此等常溫下為固體狀 得且古— 篮狀之有機金脣化合物,就可獲 侍具有.一定之再現性之有機 U獲 -,Ρ . 口物之裔發量的容器而 5,已知有一種氣相成長 谷-向 中,扁交哭》· Μ Α 另戰金屬化合物供給容器,其 ψ在谷盜上部垂直地配設载體氣體墓入* _ 虱媸蛉入官之前端部,在 320554 5 200920490 谷器底部配設載體氣體導出營 填著由有機金屬化合物被以在f器内充 擔體而成的經擔體承n之有機壬惰性之 .平卜細1公報(專利文獻^:屬化合物(參照日本特開 ’一::’專利文獻1所記载之供給容器雖然可獲得具有 ^ ia , . ^ ^ ^ 物之瘵發1,但若為了提高 乳相成長之效率而增加載體畜挪〇 物夕w Θ 戰體虱體流量並增加有機金屬化合 物之虱化1,則所充填之右嫌 、 機金屬化合物之使用率會降 低’亦即在變得無法獲得含 6曲 ^ ,,^ ^ ^ ± 有疋浪度之有機金屬化合物 仏嫩夕 仏、,、σ谷态内所殘留之有機金屬化合 物艾夕的問題。又,供仏完哭# & $ 〜、,〇 内所殘留之有機金屬化合物 專係被取出,將容㈣部洗淨,而再利用容器。 【發明内容】 (發明欲解決之課題) 士發明之目的係提供一種有機金屬化合物供給容器, =合器可獲♦具有—^之再現性之有機金屬化合物之蒸發 里呈並且田〜加載體氣體流量並增加有機金屬化合物之氣 里夺可減夕充填之有機金屬化合物之使用率降低的情 (解決課題之方法) 本毛明人為了解決該課題而精心研究,結果發現若使 用。種谷态(其t ’當垂直設置容器時,以{吏經由配設於容 士广之載體氣體導入管之前端部而供給之載體氣體朝著 略垂直之方向噴出的方式來構成載體氣體 320554 6 200920490 導入管之前端部,並在容器底部配設載體氣體導出管之前 端部),在如此所構成之容器内充填著由常溫下為固體之有 機金屬化合物被覆於對有機金屬化合物呈惰性之擔體而成 的經擔體承載之有機金屬化合物,並從載體氣體導入管之 前端部導入載體氣體,從载體氣體導出管將已氣化之含有 有機金屬化合物之載體氣體排出,藉此即可獲得具有:定 =再現性之有機金屬化合物之蒸發量,當增加載體氣體= 量並增加有機金屬化合物之氣化量時,可減少充填之有機 金屬化合物之使用率降低的情形,因而完成本發明。 亦即,本發明係一種有機金屬化合物供給容器,豆中, 在容器上部配㈣體氣體導人管之前端部,在容器底部配 設載體氣體導出管之前端部,並且在該容_充填著 :下為固體之有機金屬化合物被覆於對有機金屬化合物呈 = 生之擔體而成的經擔體承載之有機金屬化合物;該有機 ,屬化合物供給容器之特徵為:當垂直設置容器時,以使 =载體氣體導人管之前端部而供給之载體氣體朝著對容 f垂直之方向噴出的方式,來構成載體氣體導 入官之前端部。 (發明之效果) 為固^ 屬化合物供給容器中充填著由常溫_ 之有機金屬化合物被覆於姆有機金屬化合物呈惰,丨 之擔體而成的經擔體承載之有機金人 ^ 發明之有機金屬化合物供給容器,即可;得且】 現性之有機金屬化合物之蒸發量,當增域體氣體^量: 320554 200920490 可減少充填之有機金屬 增加有機金屬化合物之氣化量時 化合物之使用率降低的情形。 【實施方式】 於有機金屬化合物係在室溫下為㈣,且使用 化!列舉如:三甲基銦、二甲基氯 =I紅縣銦、三甲基銦/三甲基胂加成物、三甲基 二其二转甲絲加成㈣域合物;乙基料鋅、乙基環戊二 乂二.、%<戊:烯基鋅等鋅化合物;甲基二氯化鋁等鋁化 作人4甲基一氯化鉀、1曱基氣化鉀、二甲基溴化鉀等鉀 化5物;雙環戊二烯基鎂等。 另外,承載此等有機金屬化合物且對有機金屬化合物 呈惰性之擔體’可使用例如:氧化紹⑷咖_)、二氧化石夕 (s山ca)、富!g紅柱石(mulHte)、玻璃碳(細巧 =rbon)石墨、欽酸卸、石..英、氮化石夕、氮化蝴、碳化石夕 專陶竟類;不鏽鋼、銘、鎳、鶴等金屬類;氟系樹脂、玻 、擔體之形狀並無特別限定,可使用不定形狀、球狀、 纖維狀、網狀、線圈狀、圓管狀等各種形狀。 擔體係以比表面積較A者為佳,又,比起擔體表面丰 滑者,以具有約100至2〇〇〇 Am左右之微細凹凸者、或擔 體本身具有多數氣孔(空隙)者為更佳。此等擔體可列舉如 氧化鋁球、拉西環(Raschig ring)、海利填料 (_Heli Pack)、迪克松填料(Dix〇n packing)、不鏽鋼燒結 元件、破璃織(glass wool)等。 320554 8 200920490 冑此等有機金屬化合物承載於擔體之方法, 般所實施之方法。可列舉例如4依據重量比而將擔 I有機金屬化合物投人容器中,其次將其 機 .=合:?解,然後-邊迴娜-邊使其緩二 、、,3是在將有機金屬化合物加熱熔解後於其中 擔體,其次將過多之炫融有機金屬化合物、^ 冷卻的方法等。 使冉予以 #進行承载時,重要的是要切擔體原本所含有 =氣、、其轉發性雜質^錢。若錢體表面中存在 乳或濕氣等,則會使有機金屬化合物變質或受污染,故 在使用作為氣相成長用時,不僅會損及所得之膜之^ 亦會無法達成本發明之目的「原料 、游 較宜為該擔體要先一邊以其材料所容許之 乾圍之溫度加熱,一邊進行真空 氣等惰性氣體將空隙部予以朱代/ 4再以氮氣或氬 J體上所承載之有機金屬化合物通常㈣ =重讀為約!〇至⑽重量份之範圍,又以約2〇至7〇 ==圍為佳。當其為約1〇重量份以下時,由於有機 =Γ在容器容積中所佔之量為少,故必須將容器增 重旦二Γί以上,而為不經濟。另外,當承载超過約100 里知時,與未承載此份量之情形相比,每 金屬:合r表面積並不會變大為如期待值的程 …'法充分獲付本發明之目的效果。 第1圖係本發明之有機金屬化合物供給容器之一種實 320554 9 200920490 施態樣之刮面示意圖(容器工)。 容益1通常係使用具有彎曲狀底部之圓筒狀者。在容 盗1之上部裝設有載體氣體導入管2,並在導入管之前端 :3 f设有阻隔板3’,當垂直設置容器時,經由載體氣體 V入官2之岫端部3而供給之載體氣體係配設成因阻隔板 3而朝著對谷器中心軸呈略垂直(具體而言為9〇。±5。,較 佳為90 士3 )之方向喷出。載體氣體導出管4之前端部5 係配δ又於谷态底部。容器内部填充著經擔體承載之有機金 屬化合物6。 第4圖係以往之有機金屬化合物供給容器之剖面示意 =:本發明之供給容器、與以往之將載體氣體導入管2之 3垂直配設之供給容器係在「在載體氣體導入管2 之Μι端配4有阻隔板3’等’而將載體氣體朝著水平方 向喷出」之特點上不同。又,在容器i,設置有有機金屬 化。物及擔體、或經擔體承載之有機金屬化合物的投入口 (未圖示)。 味雖、、、在第1圖中,載體氣體導入管2及載體氣體導出 :4係裝叹在谷器之上部’但只要載體氣體導入管2之前 係裂設在容器之上部、且載體氣體導出管4之前端 容11之底部’職體氣體導人管2及載體氣 、s4之裝設位置亦可在容器之側部。 第2=係'顯示載體氣體導人管2之前端^之構造例 圖α)之構成態樣中,容器之天花板7之部分 錢成為垂直方向,並以附著於天花板7之内壁的 320554 10 200920490 方式裝設有阻隔板3’ 花板7朝著垂直方向延伸之導入管2 阻隔板3 ’而構成為從天花板7之内 著水平方向導入導體氣體。 。在第2圖⑻之構成態樣中 ,從天 之前端部3係裝設有 壁偏向容器内部如朝 第3圖係顯示載體氣體導入管2之前端部之構造之另 -例的圖,當垂直設置容器時,將配管以朝㈣容器中心 軸呈略垂直之方向(具體而言為朝著斜下方約〇至5。,較 佳為0至3°)傾斜的方式配設,而構成前端部。 經擔體承載之有機金屬化合物對於容器的殖充量,通 常是設為比載體氣體導人管2之前端部更為下方之處,但 當在容器内使有機金屬化合物承載於擔體時,則為容器之 30至70容積%左右。 ^ 一在第1圖中,就本發明之有機金屬化合物供給容器而 言’雖然是例示如底部為彎曲狀之纟器,但並非特別限定 於此’亦可使用圓錐狀等之容器。從製作簡易程度及可安 定且高效率地供給一定濃度之氣體的觀點來看,以具有彎 曲狀底部之容器為較適用。 容器底部與载體氣體導出管之前端部5的間隔較佳為 約2至15_’更佳為約2至1〇随,特佳為2至5丽。若大 於約15mm,則有機金屬化合物之使用率會下降,而不佳。 將以上述方法填充有被承載於擔體之有機金屬化合物 的供給容器1 ^以搬運到使用場所,並將其載體氣體導出 & 4連接至氣相成長裝置等(未圖示),並且,將其載體氣 肢‘入f 2連接至虱氣等載體氣體之供給源。使供給容界 320554 11 200920490 保持一定溫度而供給载體氣體,一邊填補經擔體承載之有 機金屬化合物之間隙,一邊使載體氣體從容器上部移行至 .下部,藉此而將含有該溫度下之濃度之有機金屬化合 .物的載體氣體經由載體氣體導出管4而供給至氣相成長裝 置等。因此,即可獲得具有一定之再現性之有機金屬^ 物之蒸發量,即使當增加載體氣體流量而增加有機金屬化 合物之氣化量時,亦可減少充填之有機金屬化合物之使用 率降低的情形。 (貫施例) 以下籍由實施例而詳細說明本發明,但本發明並非限 定於此等實施例。 使用下述容器作為有機金屬化合物供給容器。 (容器A) ° 使㈣容積8_1之不鏽鋼製容器(f曲狀之底部), j與第i圖概略顯示者同樣地在天花板裝設載體氣體導 吕2:載體軋體導出管4、擔體及有機金屬化合物之投入 :者。載體氣體導人管之前端部之構成態樣係如第2圖(A) 所不,在容器天花板7之邱八 般处_ 之〇卩刀之開口部,將直徑18mm之圓 盤狀阻隔板3 ’以令:M:盘子y 4 一 ^ ’、’、 化板之間隔為約3丽之方式襄 叹’並使其對於天花板 e ^ „ 壬尺千方向。另外,容器底部與载 體虱體導出管之前端部5的間隔為3_。 (容器B) 使用如下述之容器:載體 如證 興體轧體導入官2之前端部3係 第4圖所示相對於容霁 各态天化板王垂直之方向,並配設成 320554 12 200920490 使載體氣體導入管2之前端部3位於容器天花板内壁面之 面位置,除此以外與容器A相同者。 使用如此之容器A與容器B,在將容器内及導管進行 氮氣取代後,在各個容器内,於氮氣氛圍中,將以經真空 脫氣且經氮氣取代空隙部之約4匪φ之氧化鋁球435g所構 成之擔體、以及三甲基銦300g經由投入口填充至容器内。 將經填充之容器加熱至三曱基銦之熔點以上而使三甲 基銦熔解,其次,一邊迴轉容器,一邊使其緩緩地冷卻, 而令三曱基銦固化、承載於擔體之氧化鋁球之表面。 (有機金屬化合物之供給) 依序連接氫氣瓶、流量調控裝置、填充有上述經擔體 承載之有機金屬化合物的有機金屬化合物供給容器、氣體 濃度計、三曱基銦收集用课冷阱、壓力調控裝置及真空泵 (未圖示)。 將該供給容器放入恆溫槽中,保持於25°C。氣體濃度 計係使用亞比森濃度計(Thomas Swan Scientific Equipment公司製品) 貫驗1 對於填充有經擔體承載之有機金屬化合物的容器A, 從載體氣體導入管以900ml/分鐘(換算大氣壓)供給氫 氣,使三曱基銦氣化,並以氣體濃度計測定三甲基銦濃度。 實驗2 對於填充有經擔體承載之有機金屬化合物的容器B, 從載體氣體導入管以900ml/分鐘(換算大氣壓)供給氳 13 320554 200920490 ; 氣,並與實驗1同樣地測定三甲基銦濃度。 實驗3 對於填充有經擔體承載之有機金屬化合物的容器B, 從載體氣體導入管以600ml/分鐘(換算大氣壓)供給氳 ’氣,並與實驗1同樣地測定三甲基銦濃度。 由各實驗之測定結果,求出使用率(在可獲得一定濃度 之三曱基銦氣體之期間中所氣化之三甲基銦之總重量相對 於填充至容器内之三甲基銦之填充量的比率)之比(以實驗 1作為基準)。其結果係示於表1。 表1 貫驗編號 使用容器 載體氣體之流量 (ml/分鐘) 使用率之比 1 A 900 1.0 2 B 900 0. 91 3 B 600 1.2 如上所述,當使用以往之容器(B)時,若增加氫氣流量 則會使令使用率降低,但藉由使用本發明之容器(A),即使 增加氫氣流量,亦可令使用率比使用以往之容器時更加提 南。 【圖式簡單說明】 第1圖係本發明之有機金屬化合物供給容器之一種實 施態樣之剖面示意圖。 第2圖(A)及(B)係顯示載體氣體導入管之前端部之構 造例的圖。 14 320554 200920490 第3圖係顯示載體氣體導入管之前端部之構造例的 圖。 第4圖係以往之有機金屬化合物供給容器之剖面示意 圖 【主要元件符號說明】 1 容器 2 載體氣體導入管 3 載體氣體導入管之前端部 3’ 阻隔板 4 載體氣體導出管 5 載體氣體導出管之前端部 6 經擔體承載之有機金屬化合物 7 容器之天花板 15 320554200920490 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to an organometallic compound supply container. More specifically, the third aspect of the invention relates to an organometallic compound supply container in which an organometallic compound carried by a carrier is supported by the carrier. The material is composed of an organometallic compound which is solid at normal temperature and which is an emotional carrier. [Prior Art] In the electronics industry, an organometallic compound is used as a raw material of, for example, a compound semiconductor. 3; used in the electronics industry, the use of organometallic compounds: through a carrier gas such as hydrogen (carrier gas metal compound contact, and as a wm as a rider metal compound saturated vapor, v cited for use in gas phase growth devices, etc. #用: When the solid metal compound is solid under the dish (to the temperature), the metal compound of the disk is different, even if the flow of the carrier gas channel metal compound + filament gas flow X: two: : (10) and become a small particle size solid organometallic compound: ί accumulation at the bottom of μ 'Results solid organometallic compound disk carrier gas can not be fully contacted, but has no,, Qufu U body milk, ^ ^ 疋 / 辰Degrees of supply of organic metal to the shortcomings of the gas phase growth. The Qianmeng sputum is a solid and ancient-like organic lip compound at room temperature, which can be obtained with a certain degree of reproducibility. The organic U gets -, Ρ. The container of the genital volume of the mouth and 5, is known to have a vapor-growth valley - to the middle, the flat to cry" · Μ Α Another metal compound supply container, which is in the valley thief Upper vertical The carrier gas tomb is placed * _ into the front end of the official, at 320554 5 200920490, the bottom of the trough is equipped with a carrier gas derivation camp filled with an organometallic compound to be filled in the f 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 ^ ^ ^ 瘵 瘵 1 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , The use rate of organic metal compounds will decrease, that is, it will become impossible to obtain organic metals remaining in the organic metal compound containing 6 , , , ^ ^ ^ ± 疋 疋 , The problem of the compound Ai Xi. In addition, the 有机 哭 哭 # & & & & & & & & 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机 有机The subject of the invention is to provide a kind of The metal compound supply container, = combiner can obtain the reproducibility of the organometallic compound evaporation, and the field-loading gas flow rate and increase the organometallic compound gas can be reduced in the organic compound The situation in which the usage rate is reduced (method of solving the problem) The author has carefully studied the problem in order to solve the problem, and found that if it is used, the seed state (when t' is set vertically, the container is set to The carrier gas supplied from the front end of the wide carrier gas introduction tube is sprayed in a direction perpendicular to the vertical direction to form a carrier gas 320554 6 200920490 at the front end of the introduction tube, and the end portion of the carrier gas outlet tube is disposed at the bottom of the container) The container thus constituted is filled with a carrier-supported organometallic compound in which an organometallic compound which is solid at a normal temperature is coated on a carrier which is inert to the organometallic compound, and is introduced from the front end of the carrier gas into the tube. Introducing a carrier gas, and discharging the vaporized carrier gas containing the organometallic compound from the carrier gas outlet tube Thereby, the evaporation amount of the organometallic compound having the constant=reproducibility can be obtained, and when the carrier gas amount is increased and the gasification amount of the organometallic compound is increased, the use rate of the filled organometallic compound can be reduced. Thus the present invention has been completed. That is, the present invention is an organometallic compound supply container in which the end portion of the upper portion of the container is provided with a front end portion of the gas guide tube, and the end portion of the carrier gas outlet tube is disposed at the bottom of the container, and is filled in the container. The solid metal compound is coated with a carrier-supporting organometallic compound which is a carrier of the organometallic compound; the organic compound supply container is characterized by: when the container is vertically disposed, The carrier gas supplied to the front end of the carrier gas guiding tube is ejected toward the direction perpendicular to the volume f to constitute the front end portion of the carrier gas introduction member. (Effect of the Invention) The organic compound supply container is filled with an organic metal compound which is coated with an organic metal compound at a normal temperature, and is supported by a carrier of an organic metal compound. The metal compound can be supplied to the container, and the evaporation amount of the present organometallic compound can be reduced. When the amount of the organic gas is increased, the compound can be used to reduce the gasification of the organometallic compound. Reduced situation. [Embodiment] The organometallic compound is (IV) at room temperature and is used! For example: trimethyl indium, dimethyl chloride = I red county indium, trimethyl indium / trimethyl hydrazine adduct, trimethyl bis-methyl ketone addition (tetra) domain compound; ethyl material Zinc, ethylcyclopentadienyl diamide, % < pentane: alkenyl zinc and other zinc compounds; methyl aluminum dichloride and other aluminization as human 4 methyl potassium chloride, 1 fluorenated potassium, two Potassium 5 such as potassium methyl bromide; biscyclopentadienyl magnesium. Further, a support which carries these organometallic compounds and is inert to the organometallic compound can be used, for example, Oxidation (4) Coffee _), Sebium Oxide (ssan ca), rich! g montmorillonite (mulHte), glassy carbon (fine = rbon) graphite, acid acid unloading, stone.. Ying, nitrite, nitriding butterfly, carbonized stone ceremonial ceramics; stainless steel, Ming, nickel, crane and other metals The shape of the fluorine-based resin, the glass, and the support is not particularly limited, and various shapes such as an indefinite shape, a spherical shape, a fibrous shape, a mesh shape, a coil shape, and a circular tube shape can be used. It is preferable that the support system has a specific surface area of A, and that the surface of the support is smooth, and the fine unevenness of about 100 to 2 Å Am or the carrier itself has a large number of pores (voids). Better. Examples of such a support include alumina balls, Raschig rings, _Heli Pack, Dix〇n packing, stainless steel sintered elements, glass wool, and the like. 320554 8 200920490 A method of carrying out the method of carrying such an organometallic compound on a support. For example, 4, the organometallic compound is placed in a container according to the weight ratio, and secondly, the machine is combined with the solution, and then the mixture is neutralized, and then the organic metal is removed. The compound is heated and melted and then supported therein, followed by excessive amount of the organometallic compound, cooling method, and the like. When it is carried out, it is important to cut the carrier to contain the gas, and the transmissive impurities. If milk or moisture is present on the surface of the body, the organometallic compound may be deteriorated or contaminated. Therefore, when used as a vapor phase growth, not only the obtained film may be damaged, but also the object of the present invention may not be achieved. "Materials and swims should be carried out on the support of the carrier at the temperature allowed by the material. The inert gas such as vacuum gas is used to carry the voids on the nitrogen or argon J body. The organometallic compound is usually (iv) = re-read to a range of from about 〇 to (10) parts by weight, preferably from about 2 〇 to 7 〇 ==. When it is less than about 1 part by weight, since the organic = Γ in the container The amount occupied by the volume is small, so it is necessary to increase the weight of the container by more than two centimeters, and it is uneconomical. In addition, when the load exceeds about 100, the metal is combined with the case where the amount is not carried. The r surface area does not become as large as the expected value... The method fully satisfies the effect of the present invention. Fig. 1 is a schematic diagram of the scrap metal surface of the organometallic compound supply container of the present invention 320554 9 200920490 (container). Usually, a cylindrical shape having a curved bottom is used. A carrier gas introduction pipe 2 is installed on the upper portion of the mouthpiece 1 and a barrier plate 3' is provided at the front end of the introduction pipe: 3f, when the container is vertically disposed, The carrier gas system supplied via the carrier gas V into the end portion 3 of the member 2 is disposed so as to be slightly perpendicular to the central axis of the valley due to the barrier plate 3 (specifically, 9 〇 ± 5 Ω. It is sprayed in the direction of 90 士 3 ). The front end portion 5 of the carrier gas outlet pipe 4 is δ and is at the bottom of the valley state. The inside of the container is filled with the organometallic compound 6 carried by the carrier. Fig. 4 is a conventional organic metal Cross section of the compound supply container =: The supply container of the present invention and the supply container vertically disposed adjacent to the carrier gas introduction pipe 2 are "in the end of the carrier gas introduction pipe 2, 4 is provided with a barrier plate 3" The characteristics of 'and the carrier gas is ejected in the horizontal direction' are different. Further, in the container i, organic metallization is provided. The input port of the material and the support or the organometallic compound supported by the support (not shown). In the first figure, the carrier gas introduction pipe 2 and the carrier gas are led out: 4 is attached to the upper portion of the barn, but the carrier gas is introduced into the upper portion of the container before the carrier gas introduction pipe 2, and the carrier gas Before the outlet tube 4, the bottom of the end portion 11 of the 'body gas guide tube 2 and the carrier gas, s4 can be installed at the side of the container. In the second aspect, in the configuration of the structural example of the front end of the carrier gas guiding tube 2, the part of the ceiling of the container 7 is vertically oriented, and is attached to the inner wall of the ceiling 7 320554 10 200920490 In a manner, the introduction tube 2 and the barrier plate 3' extending from the partition plate 3' in the vertical direction are provided, and the conductor gas is introduced from the ceiling 7 in the horizontal direction. . In the configuration of Fig. 2 (8), the front end portion 3 is provided with a view in which the wall is biased toward the inside of the container, and the structure of the front end portion of the carrier gas introduction pipe 2 is shown in Fig. 3, When the container is vertically disposed, the pipe is disposed in a direction slightly perpendicular to the central axis of the (four) container (specifically, about 〇 to 5, preferably 0 to 3° obliquely downward), and constitutes the front end. unit. The organic metal compound supported by the carrier is generally set to be lower than the front end of the carrier gas guiding tube 2, but when the organometallic compound is carried on the carrier in the container, It is about 30 to 70% by volume of the container. In the first embodiment, the organometallic compound supply container of the present invention is exemplified as a crucible having a bottom portion, but is not particularly limited thereto. A container such as a conical shape may be used. It is preferable to use a container having a curved bottom portion from the viewpoint of ease of manufacture and supply of a certain concentration of gas in a stable and efficient manner. The distance between the bottom of the container and the front end portion 5 of the carrier gas discharge tube is preferably from about 2 to 15 Å, more preferably from about 2 to 1 Torr, and particularly preferably from 2 to 5 Å. If it is larger than about 15 mm, the use rate of the organometallic compound may be lowered, which is not preferable. The supply container 1 that is filled with the organometallic compound carried on the carrier is transported to the place of use by the above method, and the carrier gas is led out and connected to a vapor phase growth device or the like (not shown), and The carrier gas limb 'into f 2 is connected to a supply source of a carrier gas such as helium. The supply volume 320554 11 200920490 is supplied to the carrier gas while maintaining a certain temperature, and the carrier gas is moved from the upper portion of the container to the lower portion while filling the gap between the organic metal compound carried by the carrier, thereby containing the temperature. The carrier gas of the organic metal compound of the concentration is supplied to the vapor phase growth device or the like via the carrier gas discharge pipe 4. Therefore, the evaporation amount of the organometallic compound having a certain reproducibility can be obtained, and even when the carrier gas flow rate is increased to increase the gasification amount of the organometallic compound, the use rate of the filled organometallic compound can be reduced. . (Comparative Example) Hereinafter, the present invention will be described in detail by way of examples, but the invention is not limited thereto. The following container was used as the organometallic compound supply container. (Container A) ° (4) A stainless steel container (f-shaped bottom) having a volume of 8_1, j is mounted on the ceiling in the same manner as the one shown in Fig. i: the carrier gas guide tube 4, the carrier And the input of organometallic compounds: The configuration of the front end of the carrier gas guiding tube is as shown in Fig. 2(A). In the opening of the container ceiling 7, the disc-shaped blocking plate with a diameter of 18 mm is used. 3' to order: M: plate y 4 a ^ ', ', the spacing of the plates is about 3 丽 ' 并 ' and make it to the ceiling e ^ „ 壬 feet thousands direction. In addition, the bottom of the container and the carrier 虱The distance between the ends 5 of the body outlet tube is 3_. (Container B) The container is as follows: the carrier, such as the front end of the body 2, is introduced into the official 2, and the end 3 is shown in Fig. 4 as shown in Fig. 4 The direction of the plate king is vertical, and is arranged to be 320554 12 200920490. The front end portion 3 of the carrier gas introduction pipe 2 is located at the surface of the inner wall surface of the container ceiling, and otherwise the same as the container A. Using such a container A and the container B, After the inside of the vessel and the conduit were replaced with nitrogen, a carrier composed of 435 g of alumina balls of about 4 匪φ which was vacuum-degassed and replaced with nitrogen in the void portion in a nitrogen atmosphere was used in each container, and 300 g of trimethyl indium is filled into the container through the inlet port. The container is heated to a melting point or higher of tridecyl indium to melt the trimethyl indium, and secondly, the container is rotated while being slowly cooled, and the trimethyl indium is solidified and supported on the surface of the alumina ball of the support. (Supply of organometallic compound) The hydrogen bottle, the flow rate control device, the organometallic compound supply container filled with the organic metal compound supported by the above-mentioned carrier, the gas concentration meter, and the trap for the trisyl indium collection are sequentially connected. Pressure regulating device and vacuum pump (not shown). The supply container was placed in a constant temperature bath and kept at 25 ° C. The gas concentration meter was measured using an Abyssin concentration meter (manufactured by Thomas Swan Scientific Equipment Co., Ltd.). The container A having the organometallic compound supported by the carrier was supplied with hydrogen gas at 900 ml/min (atmospheric pressure) from the carrier gas introduction tube to vaporize the trimethyl indium, and the trimethylindium concentration was measured by a gas concentration meter. 2 For the container B filled with the organometallic compound supported by the carrier, the crucible is supplied from the carrier gas introduction tube at 900 ml/min (converted to atmospheric pressure). 320554 200920490 ; Gas, and the concentration of trimethyl indium was measured in the same manner as in Experiment 1. Experiment 3 The container B filled with the organic metal compound supported by the carrier was supplied from the carrier gas introduction tube at 600 ml/min (converted to atmospheric pressure). 'Gas, and the concentration of trimethyl indium was measured in the same manner as in Experiment 1. From the measurement results of the respective experiments, the usage rate (trimethyl indium vaporized during the period in which a certain concentration of trimethyl indium gas was obtained was obtained) was determined. The ratio of the total weight to the ratio of the filling amount of trimethylindium filled in the container (based on Experiment 1). The results are shown in Table 1. Table 1 The flow number of the carrier carrier gas used in the inspection number ( Ml/min) Ratio of use 1 A 900 1.0 2 B 900 0. 91 3 B 600 1.2 As mentioned above, when the conventional container (B) is used, increasing the hydrogen flow rate will reduce the use rate, but borrow By using the container (A) of the present invention, even if the flow rate of hydrogen gas is increased, the usage rate can be made more advanced than when using a conventional container. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic cross-sectional view showing an embodiment of an organometallic compound supply container of the present invention. Fig. 2 (A) and (B) are views showing a configuration example of the end portion of the carrier gas introduction pipe. 14 320554 200920490 Fig. 3 is a view showing a configuration example of the end portion of the carrier gas introduction pipe. Fig. 4 is a schematic cross-sectional view of a conventional organometallic compound supply container. [Main element symbol description] 1 container 2 carrier gas introduction pipe 3 carrier gas introduction pipe front end portion 3' barrier plate 4 carrier gas outlet pipe 5 carrier gas outlet pipe The front end portion 6 is supported by the carrier of the organometallic compound 7 container ceiling 15 320554

Claims (1)

200920490 十、申請專利範圍: 1.=錢金屬化合物供給容器,其中,在容器上部配設 =s之月…在奋為底部配設載體氣體導 出吕之心部’並且在容器内充填著經擔體承载之有機 金屬化合物,該經擔體承載之有機金屬化合物係由常溫 下為固體之有機金屬化合物被覆於對有機金屬化合物 ,情性之擔體而成者;該有機金屬化合物供給容器之特 认為’ *垂直&置容II時’以使經由載體氣體導入管之 前端部而供給之載體氣體朝著相對於容器中心軸呈略 f直之方向噴出的方式,來構成载體氣體導入管之前端 2.如申請專利範圍帛1項之有機金屬化合物供給容器,A :’從載體氣體導人管之前端部噴出之角度係相對於容 器.中心轴呈9_〇。±5。。 3·如申請專利範圍第1項或第2項之有機金屬化合物_ 谷益’其中’該有機金屬化合物係三甲基銦。 ° 4· 一财機金屬化合物之供給方法,其特徵為··搬運申产 專利範圍第1項之有機金屬化合物供給容器 ;導出管,相成長裝置,並將載體氣體導!= 至载體乳體之供給源,使該有機金屬化合物供給容器 =於疋"皿度,供給裁體氣體,使載體氣體從該有機 給容器之上部移行至下部,將含有該$ 疋/辰又之有機金屬化合物的載體氣體經由载體 氣體導出管而供給至氣相成長裝置。 戟體 320554 16200920490 X. Patent application scope: 1.=The money metal compound supply container, in which the month of the container is equipped with =s... The carrier gas is provided at the bottom of the container to derive the core of the heart and the container is filled with the carrier. The organometallic compound supported by the support is composed of an organometallic compound which is solid at normal temperature and coated with an organic metal compound, and the organic metal compound is supplied to the container. '*Vertical &amplitude II' constitutes the carrier gas introduction tube at the front end of the carrier gas introduction tube so that the carrier gas supplied through the front end portion of the carrier gas introduction tube is ejected in a direction slightly perpendicular to the container center axis 2. For the organometallic compound supply container of the patent application 帛1, A: 'The angle ejected from the front end of the carrier gas guiding tube is 9 〇 with respect to the central axis of the container. ±5. . 3. The organometallic compound of the first or second aspect of the patent application _ 谷益' wherein the organometallic compound is trimethylindium. ° 4· A method for supplying a metal compound of a financial machine, which is characterized in that it transports an organometallic compound supply container of the first patent scope of the patent application; a discharge tube, a phase growing device, and a carrier gas guide! = to the carrier milk The supply source of the body is such that the organometallic compound is supplied to the container=the container is supplied with the cut-off gas, and the carrier gas is transferred from the upper portion of the organic feed container to the lower portion, and the organic metal containing the 疋/chen is contained. The carrier gas of the compound is supplied to the vapor phase growth apparatus via the carrier gas outlet pipe. Carcass 320554 16
TW097132869A 2007-08-31 2008-08-28 A vessel for providing organometallic compound TW200920490A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2007225595A JP5050739B2 (en) 2007-08-31 2007-08-31 Organometallic compound supply container

Publications (1)

Publication Number Publication Date
TW200920490A true TW200920490A (en) 2009-05-16

Family

ID=40420702

Family Applications (1)

Application Number Title Priority Date Filing Date
TW097132869A TW200920490A (en) 2007-08-31 2008-08-28 A vessel for providing organometallic compound

Country Status (4)

Country Link
JP (1) JP5050739B2 (en)
KR (1) KR20090023166A (en)
CN (1) CN101376967A (en)
TW (1) TW200920490A (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103518165B (en) 2011-05-10 2016-06-08 株式会社富士金 Pressure flow-rate controller with flow monitor
JP5755958B2 (en) 2011-07-08 2015-07-29 株式会社フジキン Raw material gas supply equipment for semiconductor manufacturing equipment
JP5652960B2 (en) * 2011-08-01 2015-01-14 株式会社フジキン Raw material vaporizer
JP5647083B2 (en) 2011-09-06 2014-12-24 株式会社フジキン Raw material vaporization supply device with raw material concentration detection mechanism
KR101389011B1 (en) 2012-03-28 2014-04-24 주식회사 유니텍스 Source container and reactor for vapor phase deposition

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090159003A1 (en) * 2006-05-30 2009-06-25 Ube Industries Ltd Device for supplying organic metal compound

Also Published As

Publication number Publication date
JP5050739B2 (en) 2012-10-17
CN101376967A (en) 2009-03-04
KR20090023166A (en) 2009-03-04
JP2009059871A (en) 2009-03-19

Similar Documents

Publication Publication Date Title
JP5438142B2 (en) Supply device
TW200920490A (en) A vessel for providing organometallic compound
TWI352745B (en) Delivery device
JP5645985B2 (en) Bubbler for constant supply of solid compound vapor
JP5257197B2 (en) Organometallic compound feeder
JP2651530B2 (en) Organometallic compound supply equipment for vapor phase growth
JP2020114941A (en) Low temperature sintering of solid precursor
US8758515B2 (en) Delivery device and method of use thereof
WO2007139159A1 (en) Device for supplying organic metal compound
JP2013028854A (en) Device and method for supplying solid material gas
TWI379018B (en)
JP5521680B2 (en) Organometallic compound feeder
US8021441B2 (en) Method of vaporizing solid organometallic compound
JP5262083B2 (en) Solid organometallic compound feeder
WO2015145907A1 (en) Organic metal compound-containing gas supply device
CN116497438B (en) Silicon carbide single crystal growth device and growth method
JPH0620951A (en) Vessel for vaporizing organic metal
CN114515561A (en) Low-cost preparation device and preparation method of high-purity silicon carbide powder capable of realizing mass production
KR20070015955A (en) Bubbler for constant vapor delivery of a solid chemical