1379018 %日修正替換頁 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。更詳細者係 有關塡充已被覆常溫下爲固體之有機金屬化合物於對有機 金屬化合物爲惰性的載體上之載體擔載有機金屬化合物所 成之有機金屬化合物供給容器。 〇 【先前技術】 有機金屬化合物係於電子工業用中做爲化合物半導體 原料使用。有機金屬化合物用於電子工業時，通常使氫氣 等載氣進行流動吹入與有機金屬化合物接觸，做成有機金 • 屬化合物之飽和蒸氣載入氣相成長裝置等中，使用之。 常溫（室溫）下爲固體之有機金屬化合物的情況下， 與液體不同，即使吹入載氣，所層合之固體有機金屬化合 物中仍形成載體通過之流路，或經由氣化呈小粒徑之固體 〇 有機金屬化合物會於容器底部堆積，結果其固體有機金屬 化合物與載氣無法充份接觸，導致對於氣相成長裝置無法 供給穩定濃度之有機金屬化合物之缺點出現。 針對此常溫下爲固體狀有機金屬化合物，做爲可取得 具一定的再現性之有機金屬化合物之蒸發量之容器，公知 者有於容器上部使載氣導入管之前端部呈垂直配設，於底 部配置載氣導出管之前端部，且於容器內塡充已被覆有機 金屬化合物於對有機金屬化合物爲惰性之載體上之載體擔 載有機金屬化合物所成之氣相成長用有機金屬化合物供給 -5- 1379018 替換' 容器（特開平1 -2655 1 1公報）。 惟，特開平1 -2655 1 1公報所記載之供給容器雖可得 具一定再現性之有機金屬化合物之蒸發量，爲提高氣相成 長之效率，若使載氣流量變大，使有機金屬化合物之氣化 量變大，會導致塡充有機金屬化合物之使用率降低，亦即 ，當無法獲得一定濃度之含有機金屬化合物氣體時，會有 供給容器內所殘留之有機金屬化合物變多之問題產生。另 外，供給容器內所殘留之有機金屬化合物取出後，洗淨容 〇 器內，容器再行利用。 【發明內容】 本發明目的係爲提供一種可得具一定再現性之有機金 . 屬化合物之蒸發量，使載氣流量變多，有機金屬化合物之 氣化量變多時，可減少所塡充有機金屬化合物使用率下降 之有機金屬化合物供給容器。 本發明者爲解決該課題，進行精密硏討結果發現，使 〇 用於容器上部設置對於水平方向往斜下方傾斜20〜50°之 載氣導入管之前端部，配設載氣導出管之前端部於底部之 容器，於容器內塡充已被覆於常溫下爲固體之有機金屬化 合物於對有機金屬化合物爲惰性的載體上之載體擔載有機 金屬化合物，藉由自載氣導入管之前端部導入載體，自載 氣導出管取出含有已氣化之有機金屬化合物之載氣，可得 具有一定再現性之有機金屬化合物之蒸發量，而使載氣流 量變多，有機金屬化合物之氣化量變大時，可減少塡充有 -6- 1379018 機金屬化合物使用率下降，進而完成本發明。 亦即，本發明係於容器上部配設載氣導入管之前端部 ，於底部配設載氣導出管之前端部，且於該容器內塡充已 被覆於常溫下爲固體之有機金屬化合物於對有機金屬化合 物爲惰性的載體上之載體擔載有機金屬化合物所成之有機 金屬化合物供給容器中，其載氣導入管之前端部對於水平 方向往斜下方傾斜20〜50°進行配設者爲其特徵之有機金 屬化合物供給容器》 藉由使用本發明之塡充已被覆於常溫下爲固體之有機 金屬化合物於對有機金屬化合物爲惰性的載體上之載體擔 載有機金屬化合物所成之有機金屬化合物供給容器，係可 得具一定再現性之有機金屬化合物之蒸發量，使載氣流量 變多，有機金屬化合物之氣化量變多時，可減少所塡充有 機金屬化合物使用率之下降。 【實施方式】 [發明實施之最佳形態] 本發明之有機金屬化合物於室溫下爲固體，係用於氣 相成長用等，具體例如：三甲基銦、二甲基氯銦、環戊二 烯銦、三甲銦•三甲砷加成化合物、三甲銦•三甲膦加成 化合物等銦化合物、乙基碘化鋅、乙基環戊二烯鋅、環戊 二烯鋅等鋅化合物、甲基二氯鋁等之鋁化合物、甲基二氯 鎵、二甲基氯鎵、二甲基溴鎵等鎵化合物、雙環戊二烯鎂 等例。 1379018 又，做爲可擔載此等有機金屬化合物之對有機金屬化 合物爲惰性的載體，係可使用氧化鋁 '二氧化矽、莫來石 (mullite)、碎碳、石墨、鈦酸鉀、石英、氮化矽、氮化 硼、碳化矽等陶瓷類'不銹鋼、鋁、鎳、鎢等金屬類、氟 樹脂、玻璃等。 載體形狀並未特別限定，一般可使用不定形狀、球狀 、纖維狀、網狀、螺旋狀、圓管狀等各種形狀者。 載體係以比表面積較大者爲宜，與平滑者相較，載體 表面係以具有約100〜2000 /zm程度之微細凹凸者爲宜， 或以於載體本身具有多數氣孔（空隙）者爲佳。做爲此載 體例者如：氧化鋁球、塡充圈、赫利塡充、迪克森襯墊、 不銹鋼燒結元件、玻璃綿等例。 於載體上擔載之有機金屬化合物之方法可採用過去一 般實施之方法。如：於容器中投入預先使載體及有機金屬 化合物既定的重量比，再將此加熱後熔解有機金屬化合物 ，之後，持續旋轉攪拌緩慢冷卻之方法、於有機金屬化合 物加熱熔融中投入載體，接著抽出過剩之熔融有機金屬化 合物後，進行冷卻之方法等例。 進行擔載時，以預先將含於載體之氧、濕份、其他揮 發性雜質去除爲其重點。若載體表面存在氧、濕份等，則 .因其有機金屬化合物將變質、受污染，因此，做爲氣相成 長用之使用時，不僅損及所得膜之品質，作爲本發明目的 之原料亦無法穩定供應。爲避免此些狀況，載體係以預先 於其材料之可谷許fe圍之溫度下持續進彳了加熱同時進行真 -8- 1379018 空脫氣’再以氮、氬等惰性氣體取代空隙部位者爲宜。 擔載於載體之有機金屬化合物通常，對於100重量份 之載體時，約爲10〜100重量份，較佳者約20〜70重量 份。若約10重量份以下時，因容器容積所佔有機金屬化 合物之量少，所以容器務必加大，在經濟面不理想。反之 ’超出約1 00重量份進行擔載時，相較於未擔載時，其單 位塡充容積之有機金屬化合物的表面積愈無法如所期待之 大’因此無法有效獲得本發明之目的。 圖1係本發明有機金屬化合物供給容器之—實施形態 的截面模式圖。容器1通常使用具有彎曲狀底部之圓筒狀 者。容器1之上部裝置有載氣導入管2及載氣導出管4, 載氣導入管之前端部3對於水平方向往斜下方傾斜20〜50 ° ’較佳者爲25〜45°被配設之。載氣導出管之前端部5 配設於容器之底部。容器內部塡充有擔載於載體之有機金 屬化合物6。圖4係代表先行技術有機金屬化合物供給容 器之截面模式圖’本發明供給容器，與其先行技術之載氣 導入管前端部3呈垂直配設之供給容器相較下，係因載氣 導入管之前端部3約傾斜20〜50°所配設之點而相異。另 外’容器1中設置有機金屬化合物及載體、或擔載載體之 有機金屬化合物之投入口（未圖示）。 載氣導入管2及載氣導出管4雖如圖1中裝置於容器 之上部’惟，只要載氣導入管之前端部3配設於容器上部 ，載氣導出管之前端部5配設於容器之底部，載氣導入管 2及載氣導出管4亦可裝置於容器之側部。 -9 - 1379018 載氣導入管之前端部3係以對於水平方向往斜下方傾 斜約20〜50°之同時，由遠離容器中心軸之位置往容器側 壁進行傾斜配置爲宜。 圖2係代表載氣導入管之前端部平面方向配置之截面 模式圖。載氣導入管2係配置於遠離圓筒容器之中心軸的 位置，其前端部3係往容器側壁進行傾斜配設之。藉由此 配置，由前端部之載氣形成旋回流而流動（圖中以箭頭示 之）’偏流消失。 圖3代表載氣導入管前端部構造例之圖。（Α)中， 其容器之上板7的部份開口部對於水平方向往斜下方傾斜 約20〜50°構成前端部。（Β)中於上板7配設對於水平 方向往斜下方傾斜約20〜50°之配管，構成前端部。 擔載載體之有機金屬化合物往容器之塡充量通常，以 較載氣導入管前端部稍爲下部爲準，而，於容器內使有機 金屬化合物擔載於載體時約爲容器之30〜70容積％。 一般顯示底部爲彎曲狀之容器，然而並未限定爲此， 亦可使用圓錐狀等容器。由製造之簡易度及以可穩定且高 效率地供給一定濃度氣體之觀點，係以使用具有彎曲狀底 部之容器爲佳。 容器底部與載氣導出管之前端部5之間隔約爲2〜 15mm，較佳者爲2〜10mm，更佳者爲 2〜5mm。當大於 15 mm則有機金屬化合物之使用率將下降而不理想。 上述方法中，塡充有擔載於載體之有機金屬化合物之 供給容器1係搬運至使用場所後，載氣導出管4係連接於 1379018 氣相成長裝置等（未圖示），又，載氣導入管2係連接於 氫氣等載氣之供給源。使供給容器保持在一定溫度，供給 載氣後，藉由移除擔載載體之有機金屬化合物間隙之同時 ’邊將載氣自容器上部移行至下部處，使該溫度下含有一 定濃度之有機金屬化合物之載氣經由載氣導出管4供給於 氣相成長裝置等。藉由此’可得具一定再現性之有機金屬 化合物之蒸發量，即使載氣流量變多、有機金屬化合物之 氣化量變多時，仍可減少所塡充有機金屬化合物之使用率 [實施例] 以下，依實施例進行本發明之詳細說明，惟，本發明 並未受限於此等實施例。 使用下述容器做爲有機金屬化合物供給容器。 (容器A) 內容積800ml之不銹鋼製容器（彎曲狀底部），與圖 1、圖2、及圖3(A)之代表模式爲相同者，於容器的上 板配設有載氣導入管2、載氣導出管4、載體及有機金屬 化合物之投入口。載氣導入管之前端部如圖3(A)所示 ，使容器上板7之部份開口部對於水平方向往斜下方傾斜 30°所構成。又，如圖2所示’載氣導入管2係配置於由 遠離圓筒容器之中心軸24mm之位置’其前端部3對於容 器之側壁進行傾斜配設之。更且’容器底部與載氣導出管 -11 - 1379018 之則端部5之間隔爲3 m m。 (容器B ) 除了載氣導入管之前端部如圖4所示對於容器上板呈 垂直方向之外’其餘係與容器A爲相同容器。 將容器內及導管進行氮取代後，載體方面，係以真空 脫氣’使經氮取代空隙部之約4mm φ之氧化鋁球43 5g及 三甲銦300g於氮雰圍中，由投入口塡充至容器內。將已 塡充之容器加熱至三甲銦之熔點以上，使三甲銦熔解，再 邊使容器旋轉邊緩慢冷卻，使三甲銦於載體之氧化鋁球表 面進行固化、擔載之。 (有機金屬化合物之供給） 依序連接氫高壓氣體容器、流量控制裝置、塡充上述 »載載體之有機金屬化合物之有機金屬化合物供給容器、 氣體濃度計、三甲銦收集用深冷凝氣閥、壓力控制裝置及 真空泵。 供給容器係置入恆溫槽，保持於25 °C。使用耶皮森濃 度計（Thomas Zswan Scientific Ichypment 公司製）做爲 氣體濃度計。 實驗1:針對塡充擔載載體之有機金屬化合物之容器 A ’由載氣導入管以9 00ml/分鐘（大氣壓換算）供給氫氣 ’使三甲銦氣化，以氣體濃度計測定三甲銦濃度。 -12- 1379018 實驗2:又，針對塡充擔載載體之有機金屬化合物之 容器B，由載氣導入管以900ml/分鐘（大氣壓換算）供給 氫氣，同法測定三甲銦濃度。 實驗3:針對塡充擔載載體之有機金屬化合物之容器 B，由載氣導入管以600ml/分鐘（大氣壓換算）供給氫氣 ，同法測定三甲銦濃度。 求出此等使用率（取得一定濃度之三甲銦氣體期間對 氣化之二甲銦總重量容器之三甲銦塡充量之比率）之比（ 以實驗1爲基準）。結果如表1所示。 [表1] 實驗No. 使用容器 載氣之流量 (ml/分、 使用率之比 1 A \ j 9〇〇 1.0 2 B 900 0.82 3 B 6〇〇 1.11379018 % Daily Correction Replacement Page IX. Description of the Invention [Technical Field of the Invention] The present invention relates to an organometallic compound supply container. More specifically, it relates to an organometallic compound supply container in which an organometallic compound which is coated with a carrier which is solid at a normal temperature and which is a carrier which is inert to an organometallic compound is supported. 〇 [Prior Art] Organometallic compounds are used as raw materials for compound semiconductors in the electronics industry. When the organometallic compound is used in the electronics industry, a carrier gas such as hydrogen is usually blown into contact with an organometallic compound to form a saturated vapor of an organic gold compound, which is loaded into a vapor phase growth apparatus or the like. In the case of an organometallic compound which is solid at room temperature (room temperature), unlike a liquid, even if a carrier gas is blown, a solid-state organometallic compound which is laminated forms a flow path through which the carrier passes, or is vaporized into small particles. The solid ruthenium organometallic compound of the diameter will accumulate at the bottom of the vessel, and as a result, the solid organometallic compound will not be in sufficient contact with the carrier gas, resulting in the disadvantage that the vapor phase growth apparatus cannot supply a stable concentration of the organometallic compound. The solid organometallic compound at normal temperature is used as a container for obtaining an evaporation amount of an organometallic compound having a certain reproducibility, and it is known that the end portion of the upper portion of the container is vertically disposed before the carrier gas is introduced into the tube. The bottom portion of the carrier gas outlet pipe is disposed at the bottom portion, and the organic metal compound for gas phase growth formed by the carrier-supporting organometallic compound on the carrier which is coated with the organometallic compound on the carrier which is inert to the organometallic compound is supplied in the container - 5- 1379018 Replacement 'container (Japanese Unexamined Patent Publication No. 1 - 2655 1 1). In the supply container described in Japanese Laid-Open Patent Publication No. Hei. No. Hei. No. 1 - 2655 1 1 , the amount of evaporation of the organometallic compound having a certain reproducibility is obtained, and in order to increase the efficiency of vapor phase growth, the organic metal compound is made to increase the carrier gas flow rate. When the amount of gasification becomes large, the use rate of the organometallic compound is lowered, that is, when a certain concentration of the organic metal-containing compound gas cannot be obtained, there is a problem that the amount of the organometallic compound remaining in the supply container increases. . Further, after the organic metal compound remaining in the supply container is taken out, the inside of the container is washed, and the container is reused. SUMMARY OF THE INVENTION The object of the present invention is to provide an evaporation amount of an organic gold compound having a certain reproducibility, which increases the carrier gas flow rate, and when the amount of vaporization of the organometallic compound increases, the organic content can be reduced. The organometallic compound whose metal compound usage is lowered is supplied to the container. In order to solve this problem, the inventors of the present invention have found that the crucible is used for the front end of the carrier gas introduction pipe which is inclined 20 to 50° in the horizontal direction in the upper portion of the container, and the front end of the carrier gas discharge pipe is disposed. a container at the bottom, which is filled with an organometallic compound which has been coated with an organometallic compound which is solid at normal temperature on a carrier which is inert to the organometallic compound, and which is supported by the carrier gas before the end of the tube. When the carrier is introduced, the carrier gas containing the vaporized organometallic compound is taken out from the carrier gas outlet tube, and the evaporation amount of the organometallic compound having a certain reproducibility is obtained, so that the carrier gas flow rate is increased, and the gasification amount of the organometallic compound is changed. When it is large, the use rate of the metal compound of -6- 1379018 can be reduced, and the present invention can be completed. That is, the present invention is disposed at the front end of the upper portion of the container where the carrier gas introduction pipe is disposed, and the front end portion of the carrier gas outlet pipe is disposed at the bottom portion, and the organic metal compound which has been covered with solid at room temperature is filled in the container. In the organometallic compound supply container in which the organic metal compound is supported on the carrier which is inert to the organometallic compound, the end portion of the carrier gas introduction pipe is inclined obliquely downward by 20 to 50° in the horizontal direction. The organometallic compound supply container characterized by the organic metal compound supported by the carrier which has been coated with the organometallic compound which is solid at normal temperature on a carrier which is inert to the organometallic compound by using the present invention. In the compound supply container, the evaporation amount of the organometallic compound having a certain reproducibility is obtained, and the flow rate of the carrier gas is increased. When the amount of vaporization of the organometallic compound is increased, the decrease in the use rate of the organometallic compound to be charged can be reduced. [Embodiment] [Best Mode for Carrying Out the Invention] The organometallic compound of the present invention is a solid at room temperature and is used for vapor phase growth, etc., specifically, for example, trimethylindium, dimethylchloroindium, cyclopentane Indium compound such as diene indium, trimethyl indium • trimethyl arsenic addition compound, trimethyl indium • trimethylphosphine addition compound, zinc compound such as ethyl zinc iodide, zinc cyclopentadienide or zinc cyclopentadienyl, methyl An aluminum compound such as dichloroaluminum, a gallium compound such as methyldichlorogallium, dimethylchlorogallium or dimethylbromide, or a dicyclopentadienyl magnesium. 1379018 Further, as a carrier which is inert to the organometallic compound capable of supporting these organometallic compounds, alumina 'cerium oxide, mullite, carbon scrap, graphite, potassium titanate, quartz can be used. Ceramics such as tantalum nitride, boron nitride, and tantalum carbide are metals such as stainless steel, aluminum, nickel, and tungsten, fluororesins, and glass. The shape of the carrier is not particularly limited, and generally, various shapes such as an indefinite shape, a spherical shape, a fibrous shape, a mesh shape, a spiral shape, and a circular tube shape can be used. Preferably, the carrier has a larger specific surface area, and the surface of the carrier preferably has a fine unevenness of about 100 to 2000 /zm, or the carrier itself has a plurality of pores (voids). . Examples of such carriers are: alumina balls, iridium rings, Hurricane filling, Dickson pads, stainless steel sintered components, glass wool, and the like. The method of supporting the organometallic compound on the carrier can be carried out by a method generally carried out in the past. For example, a predetermined weight ratio of the carrier and the organometallic compound is added to the vessel, and the organometallic compound is melted by heating, and then the mixture is continuously cooled by rotary stirring, and the carrier is heated and melted in the organometallic compound, followed by extraction. An example of a method of cooling after the molten organometallic compound is excessive. When carrying the load, it is important to remove oxygen, moisture, and other volatile impurities contained in the carrier in advance. When oxygen, moisture, and the like are present on the surface of the carrier, the organometallic compound is deteriorated and contaminated. Therefore, when used for vapor phase growth, not only the quality of the obtained film is impaired, but also the raw material of the object of the present invention. Unable to supply. In order to avoid such conditions, the carrier is continuously heated at a temperature pre-existing at the temperature of its material while performing the normal degassing of '-8-879018' and replacing the void portion with an inert gas such as nitrogen or argon. It is appropriate. The organometallic compound supported on the carrier is usually from about 10 to 100 parts by weight, preferably from about 20 to 70 parts by weight, per 100 parts by weight of the carrier. When the amount is less than 10 parts by weight, since the amount of the organometallic compound in the container volume is small, the container must be enlarged, which is not preferable in an economical manner. On the other hand, when the load is carried out in excess of about 100 parts by weight, the surface area of the organometallic compound in the unit charge volume is not as large as expected when it is not supported. Therefore, the object of the present invention cannot be effectively obtained. 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. The container 1 usually uses a cylindrical shape having a curved bottom. The upper part of the container 1 is provided with a carrier gas introduction pipe 2 and a carrier gas outlet pipe 4, and the end portion 3 of the carrier gas introduction pipe is inclined obliquely downward by 20 to 50 ° in the horizontal direction, preferably 25 to 45°. . The front end portion 5 of the carrier gas outlet pipe is disposed at the bottom of the container. The inside of the container is filled with an organic metal compound 6 supported on a carrier. 4 is a cross-sectional schematic view showing a prior art organometallic compound supply container. The supply container of the present invention is lower than the supply container vertically disposed at the front end portion 3 of the carrier gas introduction tube of the prior art, and is a carrier gas introduction tube. The front end portion 3 is different in that it is inclined by about 20 to 50 degrees. Further, the container 1 is provided with an organic metal compound and a carrier, or an input port (not shown) for supporting the organic metal compound of the carrier. The carrier gas introduction pipe 2 and the carrier gas outlet pipe 4 are disposed on the upper portion of the container as shown in Fig. 1. As long as the carrier gas introduction pipe is disposed at the upper end portion 3 of the container, the front end portion 5 of the carrier gas outlet pipe is disposed. At the bottom of the container, the carrier gas introduction tube 2 and the carrier gas outlet tube 4 may also be disposed at the side of the container. -9 - 1379018 Before the carrier gas introduction pipe, the end portion 3 is inclined at an angle of about 20 to 50° obliquely downward in the horizontal direction, and is inclined from the position away from the central axis of the container toward the side wall of the container. Fig. 2 is a schematic cross-sectional view showing the arrangement of the end portions in the plane direction before the carrier gas introduction pipe. The carrier gas introduction pipe 2 is disposed at a position away from the central axis of the cylindrical container, and the front end portion 3 is disposed obliquely to the side wall of the container. With this arrangement, the carrier gas from the front end portion forms a swirling flow and flows (indicated by an arrow in the figure). Fig. 3 is a view showing a configuration example of the front end portion of the carrier gas introduction pipe. In (Α), a part of the opening of the upper plate 7 of the container is inclined obliquely downward in the horizontal direction by about 20 to 50° to constitute a front end portion. In the upper plate 7, a pipe which is inclined obliquely downward in the horizontal direction by about 20 to 50° is disposed on the upper plate 7 to constitute a front end portion. The amount of the organometallic compound carrying the carrier to the container is usually slightly lower than the lower portion of the front end portion of the carrier gas introduction tube, and about 30 to 70 of the container when the organometallic compound is carried on the carrier in the container. Volume %. Generally, the container having a curved bottom is generally used, but it is not limited thereto, and a container such as a cone may be used. From the viewpoint of the ease of manufacture and the supply of a certain concentration of gas stably and efficiently, it is preferred to use a container having a curved bottom. The distance between the bottom of the container and the front end portion 5 of the carrier gas outlet tube is about 2 to 15 mm, preferably 2 to 10 mm, and more preferably 2 to 5 mm. When it is larger than 15 mm, the use rate of the organometallic compound will fall, which is not desirable. In the above method, after the supply container 1 filled with the organometallic compound supported on the carrier is transported to the place of use, the carrier gas outlet pipe 4 is connected to a 1379018 vapor phase growth device or the like (not shown), and the carrier gas The introduction pipe 2 is connected to a supply source of a carrier gas such as hydrogen. After the supply container is kept at a certain temperature and the carrier gas is supplied, the carrier gas is removed from the upper portion of the container to the lower portion by removing the gap of the organometallic compound supporting the carrier, so that the organic metal having a certain concentration at the temperature is obtained. The carrier gas of the compound is supplied to a vapor phase growth apparatus or the like via the carrier gas outlet pipe 4. By using the evaporation amount of the organometallic compound having a certain reproducibility, the use rate of the organometallic compound to be charged can be reduced even when the carrier gas flow rate is increased and the amount of vaporization of the organometallic compound is increased. Hereinafter, the detailed description of the present invention will be made by way of examples, but the present invention is not limited to the embodiments. The following container was used as an organic metal compound supply container. (Container A) A stainless steel container (curved bottom) having an internal volume of 800 ml is the same as the representative mode of Figs. 1, 2, and 3 (A), and a carrier gas introduction pipe 2 is disposed on the upper plate of the container. The carrier gas outlet pipe 4, the carrier and the input port of the organometallic compound. As shown in Fig. 3(A), the end portion of the carrier gas introduction pipe is formed such that a part of the opening portion of the container upper plate 7 is inclined obliquely downward by 30° in the horizontal direction. Further, as shown in Fig. 2, the carrier gas introduction pipe 2 is disposed at a position away from the central axis of the cylindrical container by 'the front end portion 3 is inclined to the side wall of the container. Further, the distance between the bottom of the container and the end portion 5 of the carrier gas outlet pipe -11 - 1379018 is 3 m. (Container B) The end portion is the same as the container A except that the end portion of the container is vertically oriented as shown in Fig. 4 except for the carrier gas introduction tube. After replacing the inside of the vessel and the tube with nitrogen, the carrier is vacuum degassed to make the alumina ball 43 5 g and the trimethyl indium 300 g of about 4 mm φ in the void portion replaced by nitrogen in a nitrogen atmosphere, and then charged into the inlet port. Inside the container. The container which has been filled is heated to a temperature higher than the melting point of trimethyl indium, and the indium triamide is melted, and then the container is rotated while being slowly cooled, and the indium triamide is solidified and supported on the surface of the alumina sphere of the carrier. (Supply of organometallic compound) The hydrogen high-pressure gas container, the flow rate control device, the organometallic compound supply container for charging the above-mentioned carrier-containing organometallic compound, the gas concentration meter, the deep condensing gas valve for trimethyl indium collection, and the pressure are sequentially connected. Control device and vacuum pump. The supply container was placed in a thermostatic bath and maintained at 25 °C. A skin density meter (manufactured by Thomas Zswan Scientific Ichypment Co., Ltd.) was used as a gas concentration meter. Experiment 1: A container A for charging an organometallic compound carrying a carrier A' was supplied with hydrogen gas by a carrier gas introduction tube at 900 ml/min (at atmospheric pressure) to vaporize trimethyl indium, and the concentration of trimethyl indium was measured by a gas concentration meter. -12- 1379018 Experiment 2: Further, the container B for the organometallic compound supporting the carrier was supplied with hydrogen gas at a rate of 900 ml/min (at atmospheric pressure) from a carrier gas introduction tube, and the concentration of trimethyl indium was measured by the same method. Experiment 3: For the container B of the organometallic compound supported on the carrier, hydrogen was supplied from a carrier gas introduction tube at 600 ml/min (at atmospheric pressure), and the concentration of trimethyl indium was measured by the same method. The ratio of the ratio (based on Experiment 1) to the usage rate (the ratio of the amount of trimethyl indium ruthenium to the vaporized xylene indium total weight container during a certain concentration of trimethyl indium gas) was determined. The results are shown in Table 1. [Table 1] Experiment No. Use container Flow rate of carrier gas (ml/min, usage ratio 1 A \ j 9〇〇 1.0 2 B 900 0.82 3 B 6〇〇 1.1
如上述，使用先行技術之容器（B)時，氫氣流量變 多時將降低使用率，而使用本發明容器（A)即使氫氣流 里變多，相較於使用先行技術之容器，較可提高使用率。 1379018 【圖式簡單說明】 [@ 1]本發明之有機金屬化合物供給容器之—實施形 態的截面模式圖。 [圖2]代表載氣導入管之前端部之平面方向配置之截 面模式圖。 [圖3]代表載氣導入管前端部構造例之圖。 [圖4]先行技術之有機金屬化合物供給容器之截面模 式圖。 $ 【主要元件之符號說明】 1 :容器 、 2 :載氣導入管 ：_· 3:載氣導入管前端部 4 :載氣導出管 5:載氣導出管前端部 6:擔載載體之有機金屬化合物 暴 7 :容器之上板 -14-As described above, when the container (B) of the prior art is used, the use rate of the hydrogen gas is reduced, and the use rate of the container (A) of the present invention is increased as compared with the container using the prior art. Usage rate. 1379018 [Simplified description of the drawings] [@ 1] A cross-sectional schematic view of an embodiment of the organometallic compound supply container of the present invention. Fig. 2 is a cross-sectional schematic view showing the arrangement of the end portions of the carrier gas introduction pipe in the plane direction. Fig. 3 is a view showing a structural example of a front end portion of a carrier gas introduction pipe. [Fig. 4] A cross-sectional mode view of a prior art organometallic compound supply container. $ [Description of Symbols of Main Components] 1 : Container, 2: Carrier gas introduction pipe: _· 3: Carrier gas introduction pipe front end portion 4: Carrier gas outlet pipe 5: Carrier gas outlet pipe front end portion 6: Organic carrier carrier Metal Compound Storm 7: Container Upper Plate-14-