200945479 六、發明說明： 【發明所屬之技術領域】 本發明，是有關於供給有機金屬化合物的裝置。詳細 的話，朝包含常溫較佳是常溫、常壓爲固體的有機金屬化 合物的裝置供給載體氣體，由更穩定的濃度調製包含有機 金屬化合物的載體氣體，朝使用有機金屬化合物的裝置供 給已調製的載體氣體，且，將在裝置所包含的有機金屬化 ❹ 合物由更高的比率使用來調製載體氣體，即’有關於可以 由更高的使用率調製的有機金屬化合物供給裝置。 【先前技術】 有機金屬化合物，是在化合物半導體的磊晶成長中作 爲原料使用。特別是，多使用量産性、控制性優異的有機 金屬氣相成長法（MOCVD法）。 例如常溫爲液體的有機金屬化合物也就是三甲基鎵和 〇 三甲基鋁、常溫爲固體的有機金屬化合物也就是三甲基銦 等，是在高移動度電子裝置、高輝度光裝置、大容量光通 訊用雷射、高密度記錄用雷射等所使用的元件中，作爲原 料被使用。且，其他的常溫爲固體的有機金屬化合物的使 用例，可舉例在製作藍色發光元件時作爲氮化鎵的p型掺 雜物使用的雙環戊二烯鎂的情況等。 有機金屬化合物，是被充塡在充塡容器，藉由朝其將 載體氣體流入，使與載體氣體接觸的有機金屬化合物在載 體氣體中作爲蒸氣被引入，與載體氣體一起朝充塡容器外 -5- 200945479 被取出，並被供給至氣相成長裝置等。 如此的充塡容器，是通常是使用不鏽鋼製的圓筒狀， 爲了提高熱效率、有機金屬化合物的載體氣體中的濃度的 控制性、使用率等，已知在容器的底部的構造、載體氣體 的導入管等具有各種特徵的充塡容器。且，從生産性提高 的觀點，漸使用更大型的充塡裝置。 在三甲基鎵和三甲基鋁等的常溫爲液體也就是有機金 屬化合物中，藉由在有機金屬化合物中將載體氣體蒸發， 容易引起載體氣體及有機金屬化合物的接觸，使有機金屬 化合物與載體氣體一起，被取出充塡容器外。常溫爲液體 的有機金屬化合物，是因爲在充塡容器中容易流動移動於 充塡容器底部，所以即使充塡容器中的有機金屬化合物的 殘量減少，也可由蒸發確實地進行所以可有效率地被消耗 (第1圖參照）。 另一方面，將如三甲基銦的常溫爲固體的有機金屬化 合物直接充塡的情況時，與載體氣體直接接觸的部分的有 機金屬化合物，是比其他的部分的有機金屬化合物更優先 被消耗，即，被引入載體氣體中。固體有機金屬化合物的 流動性因爲差，所以一旦部分的消耗是開始的話，持續地 其部分的消耗被促進而形成載體氣體流動容易的流路。如 此的流路形成的話，載體氣體及有機金屬化合物的接觸面 積下降，從充塡容器被導出的載體氣體中的有機金屬化合 物濃度會漸漸地下降。其結果，無法將有機金屬化合物朝 MOCVD裝置等的反應爐穩定地供給。 -6- 200945479 通常，載體氣體中的有機金屬化合物濃度開始下降時 點，有機金屬化合物的使用因爲被停止，所以未被消耗的 固體有機金屬化合物，是如第2圖所示殘留在充塡容器中 。因此，將常溫爲固體的有機金屬化合物直接充塡的情況 時，無法長期的獲得包含穩定濃度的有機金屬化合物的載 體氣體，使有機金屬化合物無法有效率地被使用。 在充塡容器內殘存的固體的有機金屬化合物的使用率 ❿ 低的話，生産性會下降而不佳。因此，爲了可以供給包含 穩定濃度的已充塡於容器中的固體的有機金屬化合的物載 體氣體，且，將有機金屬化合物效率良好地使用，已採取 各種的對策使載體氣體均一地流動至已充塡於容器將的固 體有機金屬化合物。 例如，將載體氣體在容器導入初期分散的方法、使用 擴散器的方法（專利文獻1參照）、在固體有機金屬化合 物上配置充塡材的方法（專利文獻2參照）、將載體氣體 e 對於容器中心軸略垂直地導入的方法（專利文獻3參照） 等。 且，將載體氣體均一地流動至固體有機金屬化合物中 ’使與載體氣體的接觸有效率地的方法，已被提案：將載 持在不活性載體的固體有機金屬化合物充塡至充塡容器， 從充塡部的上方朝下方將載體氣體流動的方法（第3圖參 照）（專利文獻4參照）：將固體有機金屬化合物與充塡 材一起充塡的方法（專利文獻5參照）等。藉由上述的樣 的方法，在載體氣體的導入初期部中使固體有機金屬化合 200945479 物均一地被消耗。 另一方面，將載體氣體導出的方法，已被提案：將載 體氣體導出管的先端部配置於固體有機金屬化合物中的容 器（專利文獻4參照）、在載體氣體導出口使用多孔質體 的方法（專利文獻2，專利文獻6參照）等。 但是，將載體氣體導出的方法具有各種的問題。固體 有機金屬化合物的消耗是從載體氣體的導入口附近依序進 入，隨著消耗的進行，在將載體氣體導出的部分附近會有 因流速的分布而使消耗不均一的問題。 例如，在使用載體氣體導出管等的方法中，在位於充 塡容器的底部的導出管的先端部分中載體氣體會集中，在 充塡容器的底部的壁面附近及載體氣體導出口附近中載體 氣體流速的差會變大。因此，在載體氣體導出管先端的周 邊部中的固體有機金屬化合物，是比充塡容器的底部的壁 面附近更優先被消耗，在載體氣體導出管的先端部分的周 邊部若充分量的固體有機金屬化合物無法存的話，被導出 的載體氣體中的固體有機金屬化合物的濃度會下降。其結 果’在容器內固體有機金屬化合物雖殘留，也無法朝 MOCVD裝置等的反應爐穩定供給包含所期濃度的有機金 屬化合物的氣體。 隨著由MOCVD裝置等的反應爐的大型化所産生的有 機金屬化合物的消耗量的增大，爲了將充塡固體有機金屬 化合物的容器大型化，進一步使單位時間接觸的供給量增 大的目的’而增加導入充塡容器的載體氣體量的情況時， -8 - 200945479 這種問題點會更顯著。即，由穩定的濃度將包含有機金屬 化合物的載體氣體長期導出，並且將殘存在充塡容器中的 固體有機金屬化合物有效率地消耗是更困難。 解決將載體氣體導出時的問題的方法，已被提案使用 燒結金屬過濾器和多孔板的充塡容器（專利文獻7參照） 。但是，燒結金屬和多孔板的開孔小的情況時，由固體有 機金屬化合物所産生的孔堵塞會產生，流動於固體有機金 〇 屬化合物中的載體氣體會產生偏流，成爲固體有機金屬化 合物不均一地被消耗的原因。 [專利文獻1]日本特開平02- 124796號公報 [專利文獻2]日本特開2007-314878號公報 [專利文獻3]日本特願2007-225595號公報 [專利文獻4]日本特開平1-265511號公報 [專利文獻5]日本特公平5-39915號公報 [專利文獻6]日本特開2002-83777號公報 Φ [專利文獻7]日本特開2006-161162號公報 【發明內容】 (本發明所欲解決的課題） 本發明的目的是提供一種有機金屬化合物供給裝置， 可以調製包含更穩定濃度的有機金屬化合物特別是在常溫 爲固體的有機金屬化合物的載體氣體並供給至其他的裝置 (例如有機金屬氣相成長裝置），將已充塡的固體有機金 屬化合物的使用率更提高。 -9- 200945479 (用以解決課題的手段） 本發明人等，是對於常溫特別是常溫、常壓爲固體的 有機金屬化合物的供給裝置銳意檢討的結果，發現藉由使 用以下的有機金屬化合物供給裝置可有效利用固體的有機 金屬化合物。即一種有機金屬化合物供給裝置，具有：將 載持在不活性載體被有機金屬化合物收容的充塡容器、及 將該有機金屬化合物保持在充塡容器內特別是其下部且使 載體氣體可以通過的支撐板、及位於該充塡容器的上部的 載體氣體導入口、及位於該充塡容器的底部並朝該支撐板 的下方開口的載體氣體導出口、及被安裝在該支撐板及該 載體氣體導出口之間並比該載體氣體導出口的口徑更大的 阻擋板，且載體氣體，是從載體氣體導入口被導入充塡容 器，並從上方朝下方通過被保持在支撐板上的有機金屬化 合物，且從載體氣體導出口被排出。 因此，本發明，是一種有機金屬化合物供給裝置，是 具有充塡容器，將常溫爲固體的有機金屬化合物充塡，供 給載體氣體將該有機金屬化合物昇華，其特徵爲，進一步 具有：在該充塡容器（1)內將載持在不活性載體的該有 機金屬化合物（8)保持並使載體氣體可以通過的支撐板 (9)、及位於該充塡容器的上部的載體氣體導入口（4) 、及位於該充塡容器的底部並朝該支撐板的下方開口的載 體氣體導出口（5)、及被安裝在該支撐板（9)及該載體 氣體導出口（5)之間並比該載體氣體導出口（5)的口徑 -10- 200945479 更大的阻擋板（ίο)，將載體氣體從上方朝下方通過被載 持在已充塡在支撐板上的不活性載體的該有機金屬化合物 [發明的效果] 藉由使用本發明的供給裝置，可以將常溫爲固體的有 機金屬化合物由更穩定的濃度與載體氣體一起供給，可以 φ 提高已充塡至充塡容器的有機金屬化合物的使用率。 【實施方式】 充塡至本發明的供給裝置的固體的有機金屬化合物， 是例如作爲由氣相成長法所產生的化合物半導體的原料等 有用的在常溫特別是常溫、常壓爲固體者，具體而言，可 以例示如下：三甲基銦、二甲基氯銦、環戊二烯銦、三甲 基銦•三甲基胂加成物、三甲基銦·三甲基膦加成物等的 Φ 銦化合物；乙基碘化鋅、乙基環戊二烯鋅、環戊二烯鋅等 的鋅化合物；甲基二氯鋁等的鋁化合物；甲基二氯鎵、二 甲基氯鎵、二甲溴鎵等的鎵化合物；雙環環戊二烯鎂等。 且，將如此的有機金屬化合物載持的載體，是對於固 體有機金屬化合物不活性的話無特別限定。可以使用如以 下：氧化鋁、二氧化矽、模來石、玻璃碳、石墨、鈦酸鉀 、石英、氮化矽、氮化硼、碳化矽等的陶瓷類；不鏽鋼、 鋁、鎳、鎢等的金屬類；氟化樹脂、玻璃等。載體的形狀 無特別限定’如不定形狀、球狀、纖維狀、網狀、線圈狀 -11 - 200945479 、圓管狀等的各種形狀皆可以。載體，是其表面平滑且具 有100〜2 000 // m程度的尺寸的微細的凹凸者，或是在載 體本身具有多數的氣孔（空隙）者較佳。這種載體可舉例 :氧化鋁球、拉希環、亥里派克（Heli Pack)密封墊、狄 克松（Dixon )密封墊、不鏽鋼燒結體、玻璃纖維、金屬 棉等。 支撐板，可舉例第6圖所示的金網狀、孔盤狀者。且 ，支撐板，是在其中心部具有導出管用的開口部。支撐板 的開孔的大小，是載體不落下程度的大小即可，通常，約 1〜5mm，較佳使用約1.5〜3mm。開孔的形狀無特別限定 ，可舉例例如多角形狀、圓形狀、橢圓形狀等。支撐板的 材質，是對於固體有機金屬化合物不活性的話無特別限定 ，使用例如玻璃、金屬、陶瓷等雖也可以，但是從熱傳導 性的觀點金屬製者較佳，特別是不鏽鋼製者最佳。 另一方面，雖可以將燒結金屬過瀘器作爲支撐板使用 ，但是燒結金屬的開孔太細的情況，又會壓力損失大，又 會孔堵塞，而有使載體氣體偏流的可能性。 在本發明的有機金屬化合物供給裝置，載體氣體導入 口及載體氣體導出口，是各別爲朝充塡容器內的載體氣體 的入口及從充塡容器內的載體氣體的出口的意思。在1個 較佳態樣中，載體氣體導入口及載體氣體導出口，是各別 爲在將載體氣體供給至充塡容器的作爲的導入管的配管的 端部中的開口部及從充塡容器將載體氣體排出的作爲導出 管的配管的端部中的開口部。通常，如此的氣體的配管， -12- 200945479 是剖面圓形的管，此情況，導入口及導出口的形狀也爲圓 形。當然，導入口及導出口是別的形狀也可以，對應其， 載體氣體流動的配管也具有別的剖面也可以。在別的態樣 中，導入口及導出口，是直接設在充塡容器的開口部也可 以。 在本發明的有機金屬化合物供給裝置中，阻擋板，是 位於支撐板及載體氣體的導出口之間的托板。其結果，位 φ 於阻擋板的正上部的有機金屬化合物的領域通過且下降的 載體氣體的整體流動（實質上垂直下方或是接近其方向的 流動），因爲是與阻擋板衝突，或是欲衝突，所以如此的 載體氣體的流動方向是藉由阻擋板朝別的方向改變。例如 ，朝不是垂直下方的流動方向流動。更具體而言，往朝向 充塡容器的側壁的方向（例如水平方向或是傾斜下方向） 流動。其後，如此的載體氣體，是繞過阻擋板的周邊部， 朝向位於其下位置的載體氣體導出口流動》 Ο 爲了防止因載體氣體的集中在載體氣體導出口的周邊 而使載體氣體流速變大，加大載體氣體流動的配管的徑等 地加大導出口是有效的。且，將大流量的載體氣體流動時 ，被充塡的固體有機金屬化合物因爲有可能直接以固體通 過配管而被排出容器外，所以考慮此的話，載體氣體導出 口不可過度變大，而適度縮小較佳。一般，載體氣體導出 管雖是使用外徑1 程度以下的配管，但是藉由安裝比 配管徑更大的阻擋板就可繞過阻擋板使載體氣體從充塡容 器被導出。由此’也有更多載體氣體流往充塡容器的側壁 -13- 200945479 周邊部，可以抑制載體氣體不經由充塡容器的側壁周邊部 直接朝載體氣體導出管的先端部分集中。 在本說明書中，阻擋板的形狀及尺寸，是在比支撐板 更下方將作爲阻擋板構成的構造物對於充塡容器的胴體的 長度方向（鉛直方向）正投射在垂直的面的形狀和尺寸的 意思。阻撓板的形狀及尺寸是具有：將阻擋板的正投射圖 重疊在載體氣體導出口的正投射圖的話，阻擋板的正投射 圖是覆蓋導出口的正投射圖的全部，從載體氣體導出口的 正投射圖的周圍朝向外延伸的部分的形狀及尺寸較佳。在 本發明中，對於此意思，記載成爲「比載體氣體導出口的 口徑更大的阻擋板」。且，在本發明中，一般，阻擋板的 效果，是使對於容器胴體的長度方向（或是上下方向）由 垂直的方向將阻擋板正投射的情況時所得的圖形，同樣地 將導出口正投射的情況時所得的圖形，且，藉由從其朝外 側延伸而獲得。因此，如第12圖所示，阻擋板，是對於 充塡容器胴體的長度方向垂直，且不一定需要在同一平面 上延伸，例如對於長度方向傾斜，或是被安裝成不同平面 也可以。 且，即使阻擋板是被安裝於載體氣體導出管的周圍的 態樣（即，如後述的第4圖所示，導出管貫通阻擋板的態 樣），也如上述可以抑制載體氣體不經由充塡容器的側壁 周邊部而朝載體氣體導出管的先端部分直接集中。在此態 樣中，阻擋板的形狀及尺寸，是假定導出管不存在（即， 導出管未貫通阻擋板）的情況的阻擋板的形狀及尺寸的意 -14- 200945479 思。 阻擋板的尺寸是過度地變大且接近充塡容器胴體的直 徑的話，在充塡容器底部’載體氣體是集中於側壁的周邊 部，在阻擋板的上方的載體氣體導出管的周圍載體氣體不 易流動，位於阻擋板的上方的固體有機金屬化合物的消耗 不易被引起。且，阻擋板的直徑’是對於充塡容器內徑約 10%〜75%，較佳是推薦約20%〜60%的尺寸。且，阻擋板 φ 的形狀及充塡容器的剖面不是圓形的情況時，上述的阻擋 板的直徑及充塡容器的內徑’是依據水力相當直徑。 阻擋板的材質，是對於固體有機金屬化合物不活性的 話無特別限定，使用玻璃、金屬、陶瓷等也可以，但是從 熱傳導性的觀點金屬製者較佳，特別是不鏽鋼製者較佳。 阻擋板的形狀無特別限定，可舉例多角形狀、圓形狀、橢 圓形狀等，但是從對稱性的觀點圓形狀者特別佳。 阻擋板位於遠離固體有機金屬化合物的位置，是比位 〇 於固體有機金屬化合物中更佳。因爲，阻擋板的位置是比 支撐板更上方或與支撐板相同位置時，在阻擋板的正上部 分因爲載體氣體的流動容易被遮斷，所以固體有機金屬化 合物的消耗不易被引起。另一方面，阻擋板的位置是比支 撐板更下方時，因爲固體有機金屬化合物是不存在於阻擋 板正上部的載體氣體的流動容易被遮斷的領域，所以固體 有機金屬化合物不易被消耗的領域可以減小。 進一步，安裝阻擋板、載體氣體導出口及阻擋板的高 度（或是層級）的充塡容器的水平方向的圓形剖面是略同 -15- 200945479 心，即，這些的中心是實質上位於相同的鉛直線上較佳。 即使不是同心也可獲得某程度的效果，但是因爲藉由同心 使載體氣體在充塡容器內對稱地流動，所以固體有機金屬 化合物是均等地被消耗，固體有機金屬化合物的使用率可 以更提高。 在不活性載體將固體有機金屬化合物載持的方法，是 使用習知被實施的任一的方法也可以。例如被採用：在旋 轉容器中將載體及固體有機金屬化合物隨著預定的重量比 投入’接著，將這加熱將固體有機金屬化合物融解，其後 ，旋轉攪拌且漸冷的方法，在將固體有機金屬化合物加熱 融解的中將載體投入，接著取出被過剩融解的有機金屬化 合物之後，漸冷的方法等。 進行載持時，需要預先除去被包含於載體的氧和濕分 、其他的揮發性不純物。若，在載體表面上氧和濕分等存 在的話，原料固體因爲會變質及/或被污染，作爲氣相成 長用等的原料使用時’所獲得的膜的品質不只受損，也無 法達成原本目的之原料的穩定供給。爲了避免此樣的問題 ’載體是推薦：在其材料所容許的範圍的溫度進行預先加 熱且真空脫氣’然後由氮和氬等的不活性氣體將空隙部置 換。 載持在載體上的固體有機金屬化合物，通常是對於載 體100重量部約10〜100重量部，較佳是約30〜7〇重量 部的範圍。將約重量部以下載持的情況，是因爲充塡 容器的容積中的固體有機金屬化合物的量少所以必需將容 -16- 200945479 器過度地加大，多是不經濟的情況。且，將約100重量部 以上載持的情況時，每充塡容積的固體有機金屬化合物的 表面積因爲不如期待的大，所以多無法獲得充分效果。 將由充塡了本發明的固體的有機金屬化合物的充塡容 器1所形成的有機金屬化合物供給裝置的一實施態樣如第 4圖所示。在具有彎曲狀的底部的充塡容器1的下部配置 有支撐板9，可將被載持在不活性載體的有機金屬化合物 φ 8保持，且載體氣體可以通過。在充塡容器的上部連接有 載體氣體導入管2及載體氣體導出管3。載體氣體的導入 口 4是在充塡容器1的上部朝被載持在被充塡的不活性載 體的有機金屬化合物8的上方開口，載體氣體導出管3是 通過充塡容器1內部，載體氣體的導出口 5是在充塡容器 1的底部朝支撐板9的下方開口。 在圖示的態樣中，雖在載體氣體導出口 5的上方安裝 阻擋板10，但是阻擋板10，是位於與載體氣體導出口 5 ( Ο 充塡容器1的上下方向）相同層級的位置的情況，阻擋板 10，是改變朝向其漸漸降下的載體氣體的流動方向繞過阻 擋板的周圍也可以。因此，本行業者可以容易地理解：此 情況也可以達成先前說明的本發明的效果。因此’在本發 明的供給裝置中，阻擋板，是實質上位於與載體氣體導出 口及相同層級也佳，「支撐板及載體氣體導出口之間」的 記載，是包含：阻擋板是位於比載體氣體導出口更上方的 層級位置的態樣、及位於與載體氣體導出口相同層級的位 置的態樣雙方。且，在第4圖所示的態樣中’阻擋板’是 -17- 200945479 從載體氣體導出管的外壁朝向充塡容器的側壁延伸的形態 (例如具有從圓形將其中央部分作爲相當於載體氣體導出 管的外形的部分切除的圓環（或是甜甜圈）形狀）。 且，在圖示的態樣中，載體氣體導出管3雖是通過充 塡容器1內部，但是不限定於此，導出口 5是在充塡容器 1的底部在支撐板9的下方開口的話，載體氣體導出管是 配置於充塡容器1外部也可以。 且，由充塡了別的本發明中的固體的有機金屬化合物 的充塡容器所形成的有機金屬化合物供給裝置的一實施態 樣如第5圖所示。 在具有彎曲狀的底部的充塡容器1的下部，將被載持 在不活性載體的有機金屬化合物8保持，配置有載體氣體 可以通過的支撐板9。在充塡容器1的上部連接有載體氣 體導入管2。載體氣體的導入口 4是在充塡容器1的上部 在被載持在充塡的不活性載體的有機金屬化合物8的上方 開口。載體氣體導出管3是被配置於充塡容器1的外部， 載體氣體的導出口 5是在充塡容器1的底部在支撐板9的 下方開口。在載體氣體導出口 5的上部安裝阻擋板1〇。 且’在第5圖的態樣中’載體氣體導出管3皆是被配 置於充塡容器1的朝外部但是不限定於此，導出口是在充 塡容器的底部在支撐板的下方開口的話，載體氣體導出管 是被配置於充塡容器1內部也可以。 載持在不活性載體的固體有機金靨化合物8，是從供 給口（無圖示）有充塡容器1內供給所期量並充塡至支撐 -18- 200945479 板9上。且，在充塡容器1內將 物載持在不活性載體也可以。 載體氣體導入管2是與載體氣 置（無圖示）等連接，且，載體氣 度計、氣相成長裝置（無圖示）等 1放入恆溫槽使用。 藉由將氫氣體等的載體氣體從 φ 定流量供給且充塡容器1，將載體 口 4 一邊通過被載持在不活性載體 間隙一邊從充塡容器1的上方朝下 屬化合物的載體氣體從載體氣體導 出管3供給至氣相成長裝置等。 在第4圖及第5圖中，充塡容 狀者，但是底部是水平的充塡容器 ，朝載持在不活性載體的有機金屬 Φ 的充塡量（例如充塡高度，即，充 級），通常是位於比載體氣體導入 是，將載體氣體導入口 4分割，可 有機金屬化合物8的上部均一地導 況時，不限定於此。例如，可以使 的載體氣體導入口的情況的方式將 給情況時，載體氣體導入口 4的層 化合物8的上端層級是幾乎相同也 本發明的有機金屬化合物供給 上述固體有機金屬化合 體供給源、流量控制裝 體導出管3是與氣體濃 連接，例如將充塡容器 載體氣體導入管2由預 氣體經過載體氣體導入 的有機金屬化合物8的 方通過，將包含有機金 出口 5經過載體氣體導 器1的底部雖顯示彎曲 的使用當然也可以。且 化合物8的充塡容器1 塡容器的上下方向的層 口 4的層級更下方。但 在載持在不活性載體的 入載體氣體的構造的情 用分散板或是蓮蓬頭狀 載體氣體均一地分散供 級及被充塡的有機金屬 可以。 裝置，是作爲供給氣相 -19- 200945479 成長用等的原料的裝置最佳。 以下，雖顯示本發明的實施例，但是本發明不限定於 這些。 [實施例1] 阻擋板，除了安裝於導出管的先端部，即導出口的層 級的以外，是構成與第4圖同樣的本發明的有機金屬化合 物供給裝置。充塡容器1的底部是彎曲狀且容積是約 1300cm3 (內徑：108mm，深度：147mm)，從充塡容器 的最底部的26mm的位置配設支撐板9 (開孔的大小： 2mm的金網））。在載體氣體導入口 4安裝分散板11( 圓形平板：直徑18mm)，使充塡容器1的天板與分散板 11之間的水平間隔是成爲3mm，載體氣體就可以對於容 器中心軸略垂直地導入。且，在比支撐板9更下方l〇mm 的位置開口的載體氣體導出管3 (外徑8mm，內徑6mm ) 的先端部（載體氣體導出口 5)安裝阻擋板1〇(圓形平板 :直徑30mm，但是中央貫通導出管）。 在此充塡容器1充塡平均粒徑（直徑）4.5mm的氧化 鋁球585g及三甲基銦（以下，稱爲TMI) 300g作爲不活 性載體。將已充塡的充塡容器1加熱直到約110°C爲止將 充塡容器1內的TMI熔融之後，一邊旋轉攪拌一邊直到室 溫爲止漸漸地冷卻，將TMI載持在氧化鋁球。 在此充塡容器1，作爲載體氣體是從導入管2由略一 定的速度將氫氣體以約900cm3/分（大氣壓換算，由充塡 -20- 200945479 部的每單位面積的流量：約9.5cm3/cm2 .分），將 TMI從上方朝下方通過的方式被供給，經過載體氣 口 5從載體氣體導出管將含有TMI的氫氣體取出。 由載體氣體也就是氫氣體所産生的TMI的充塡容器 出時，充塡容器1內的壓力爲40kPa (絕對壓力） 塡容器1放入恆溫槽，保持於25 °C的方式實施。 將來自充塡容器1的氫氣體中的TMI濃度，氣 φ 計是使用EPISON (商品名、超音波式）濃度計（ Swan Scientific Equipment 公司製）測量。將 TMI 期地測量，從氫氣體流量及TMI濃度，求得TMI 率（％ )。將結果如第7圖所示。TMI的濃度，是 用率成爲約87%爲止穩定，其後下降。 [實施例2] 除了安裝於載體氣體導出管3的先端部（載體 〇 出口 5)的阻擋板10(圓形平板）的直徑是5 0mm 在與實施例1同樣的充塡容器1，與實施例1同 TMI載持在氧化鋁球。 與實施例1同樣地求得TMI的使用率（％ )。 如第8圖所示。TMI的濃度，是直到使用率成爲約 止穩定，其後下降。 [實施例3] 除了安裝於載體氣體導出管3的先端部（載體 充塡的 體導出 且，從 1的導 ，將充 體濃度 Thomas 濃度定 的使用 直到使 氣體導 以外， 樣地將 將結果 8 7 %爲 氣體導 -21 - 200945479 出口 5)的阻擋板1〇(圓形平板）的直徑是80mm以外， 是在與實施例1同樣的充塡容器，與實施例1同樣地將 TMI載持在氧化鋁球。 與實施例1同樣地求得TMI的使用率（％ )。將結果 如第9圖所示。TMI的濃度，是直到使用率成爲約85 %爲 止穩定，其後下降。 [比較例1 ] 除了在載體氣體導出管3的先端部（載體氣體導出口 5)安裝阻擋板10(圓形平板）以外，是在與實施例1同 樣的充塡容器1，與實施例1同樣地將TMI載持在氧化鋁 球。 與實施例1同樣地求得TMI的使用率（％ )。將結果 如第1〇圖所示。TMI的濃度，是直到使用率成爲約83% 爲止穩定，其後下降。且，由對於充塡容器的內徑的阻擋 板尺寸的不同所産生的TMI的使用率如第11圖所示。 【圖式簡單說明】 [第1圖]將液體有機金屬化合物充塡的充塡容器的剖 面意示圖。 [第2圖]將固體有機金屬化合物充塡的充塡容器的剖 面意示圖。 [第3圖]將載持在習知的不活性載體的固體有機金屬 化合物充塡的充塡容器的剖面意示圖。 -22- 200945479 [第4圖]具有將載持在不活性載體的固體有機金屬化 合物充塡用的充塡容器的本發明的有機金屬化合物供給裝 置的1個態樣的剖面意示圖。 [第5圖]具有將供載持在不活性載體用的固體有機金 屬化合物充塡用的充塡容器的本發明的有機金屬化合物供 給裝置的另1個態樣的剖面意示圖。 [第6圖]支撐板的一例的平面意示圖（（a)顯示金網 φ 狀支撐板，（b)顯示孔盤狀支撐板）。 [第7圖]顯示實施例1中的結果的圖表。 [第8圖]顯示實施例2中的結果的圖表。 [第9圖]顯示實施例3中的結果的圖表。 [第10圖]顯示比較例中的結果的圖表。 [第11圖]顯示阻擋板尺寸影響其效果的圖表。 [第12圖]顯示阻擋板的其他的態樣的剖面意示圖（（ a)顯示圓錐狀阻擋板，（b)顯示倒圓錐狀阻擋板，（c 〇 )顯示將半圓板不同平面地安裝的阻擋板）。 【主要元件符號說明】 1 :充塡容器 2 :載體氣體導入管 3 =載體氣體導出管 4 :載體氣體導入口 5 =載體氣體導出口 6 =液體有機金屬化合物 -23- 200945479 7:固體有機金屬化合物 8:載持在不活性載體的固體有機金屬化合物 9 :支撐板 I 〇 :阻擋板 II :分散板 -24-200945479 VI. Description of the Invention: [Technical Field to Which the Invention Is Ascribed] The present invention relates to an apparatus for supplying an organometallic compound. In particular, a carrier gas is supplied to a device containing an organometallic compound which is normally a normal temperature at normal temperature and a normal pressure, and a carrier gas containing an organometallic compound is prepared from a more stable concentration, and the prepared catalyst is supplied to a device using an organometallic compound. The carrier gas, and the organometallic compound contained in the device, is used at a higher ratio to modulate the carrier gas, i.e., with respect to the organometallic compound supply device which can be modulated by higher usage. [Prior Art] An organometallic compound is used as a raw material in epitaxial growth of a compound semiconductor. In particular, an organometallic vapor phase growth method (MOCVD method) excellent in mass productivity and controllability is often used. For example, an organometallic compound which is liquid at room temperature, that is, trimethylgallium and yttrium trimethylaluminum, an organometallic compound which is solid at room temperature, that is, trimethylindium or the like, is in a high mobility electronic device, a high luminance optical device, and a large Among the components used for lasers for volumetric optical communication and lasers for high-density recording, they are used as raw materials. Further, other examples of the use of the solid organometallic compound at room temperature include, for example, dicyclopentadienyl magnesium which is used as a p-type dopant of gallium nitride when a blue light-emitting element is produced. The organometallic compound is charged in the filling vessel, and by flowing the carrier gas thereto, the organometallic compound in contact with the carrier gas is introduced as a vapor in the carrier gas, together with the carrier gas toward the outside of the filling vessel - 5-200945479 is taken out and supplied to a vapor phase growth device or the like. In such a filling container, a cylindrical shape made of stainless steel is generally used, and the structure of the bottom of the container and the carrier gas are known in order to improve the thermal efficiency, the controllability of the concentration in the carrier gas of the organometallic compound, the usage rate, and the like. A filling container having various characteristics such as an introduction tube. Moreover, from the viewpoint of productivity improvement, a larger charging device is gradually used. In the case where the normal temperature is a liquid, that is, an organometallic compound, such as trimethylgallium or trimethylaluminum, the carrier gas and the organometallic compound are easily contacted by evaporating the carrier gas in the organometallic compound, so that the organometallic compound and the organometallic compound are Together with the carrier gas, it is taken out of the filling container. The organometallic compound which is liquid at normal temperature is easily moved and moved to the bottom of the charging container in the filling container. Therefore, even if the residual amount of the organometallic compound in the filling container is reduced, it can be reliably carried out by evaporation, so that the liquid metal can be efficiently discharged. It is consumed (refer to Figure 1). On the other hand, when an organometallic compound such as trimethylindium which is solid at a normal temperature is directly charged, a part of the organometallic compound which is in direct contact with the carrier gas is more preferentially consumed than other organometallic compounds. That is, it is introduced into the carrier gas. Since the fluidity of the solid organometallic compound is poor, once part of the consumption is started, the consumption of a part thereof is continuously promoted to form a flow path in which the carrier gas flows easily. When the flow path is formed, the contact area of the carrier gas and the organometallic compound decreases, and the concentration of the organometallic compound in the carrier gas derived from the filling container gradually decreases. As a result, the organometallic compound cannot be stably supplied to a reaction furnace such as an MOCVD apparatus. -6- 200945479 Generally, when the concentration of the organometallic compound in the carrier gas starts to decrease, the use of the organometallic compound is stopped, so the solid organometallic compound that is not consumed remains in the filling container as shown in Fig. 2 . Therefore, when the organometallic compound having a solid temperature at normal temperature is directly charged, the carrier gas containing the organometallic compound at a stable concentration cannot be obtained for a long period of time, and the organometallic compound cannot be used efficiently. When the use rate of the organometallic compound of the solid remaining in the filling container is low, the productivity is lowered. Therefore, in order to supply an organometallic compound carrier gas containing a stable concentration of a solid which has been filled in a container, and to use the organometallic compound efficiently, various countermeasures have been taken to uniformly flow the carrier gas to Filled with solid organometallic compounds in the container. For example, a method of dispersing a carrier gas at the initial stage of introduction of a container, a method of using a diffuser (refer to Patent Document 1), a method of disposing a filler material on a solid organometallic compound (refer to Patent Document 2), and a carrier gas e for a container A method in which the center axis is introduced slightly vertically (refer to Patent Document 3). Further, a method of uniformly flowing a carrier gas into a solid organometallic compound to make contact with a carrier gas efficiently has been proposed: charging a solid organometallic compound carried on an inactive carrier to a filling container, A method of flowing a carrier gas downward from the upper side of the charging portion (refer to FIG. 3) (refer to Patent Document 4): a method of charging a solid organometallic compound together with a filling material (refer to Patent Document 5). By the above-described method, the solid organometallic compound 200945479 was uniformly consumed in the initial stage of introduction of the carrier gas. On the other hand, a method of deriving a carrier gas has been proposed: a container in which a tip end portion of a carrier gas discharge pipe is disposed in a solid organometallic compound (refer to Patent Document 4), and a method in which a porous body is used in a carrier gas outlet port (Patent Document 2, Patent Document 6 refers to) and the like. However, the method of deriving the carrier gas has various problems. The consumption of the solid organometallic compound proceeds sequentially from the vicinity of the introduction port of the carrier gas, and as the consumption progresses, there is a problem that the distribution of the flow velocity is uneven in the vicinity of the portion where the carrier gas is led out. For example, in the method using a carrier gas outlet tube or the like, the carrier gas is concentrated in the tip end portion of the outlet tube located at the bottom of the filling container, and the carrier gas is in the vicinity of the wall surface of the bottom portion of the filling container and in the vicinity of the carrier gas outlet port. The difference in flow rate will become larger. Therefore, the solid organometallic compound in the peripheral portion of the tip end of the carrier gas outlet pipe is more preferentially consumed than the vicinity of the wall surface of the bottom portion of the charging vessel, and a sufficient amount of solid organic is present in the peripheral portion of the tip end portion of the carrier gas outlet pipe. If the metal compound is not present, the concentration of the solid organometallic compound in the derived carrier gas is lowered. As a result, the solid organometallic compound remains in the container, and it is not possible to stably supply a gas containing the organic metal compound of the desired concentration to a reaction furnace such as a MOCVD apparatus. In order to increase the consumption of the organometallic compound by the increase in the size of the reaction furnace of the MOCVD apparatus or the like, in order to increase the size of the container filled with the solid organometallic compound, the supply amount per unit time contact is increased. 'When the amount of carrier gas introduced into the filling container is increased, the problem of -8 - 200945479 will be more significant. Namely, the carrier gas containing the organometallic compound is derived from a stable concentration for a long period of time, and it is more difficult to efficiently consume the solid organometallic compound remaining in the filling container. A method of solving the problem of deriving the carrier gas has been proposed, and a sintered metal filter and a porous container filled with a porous plate have been proposed (refer to Patent Document 7). However, when the openings of the sintered metal and the porous plate are small, the pores generated by the solid organometallic compound are clogged, and the carrier gas flowing in the solid organic metal ruthenium compound is biased to become a solid organometallic compound. Reason for being uniformly consumed. [Patent Document 1] JP-A-2007-314878 (Patent Document 3) Japanese Patent Application Publication No. 2007-225595 (Patent Document 4) Japanese Patent Laid-Open No. Hei 1-265511 [Patent Document 5] Japanese Patent Publication No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. Problem to be Solved The object of the present invention is to provide an organic metal compound supply device which can modulate a carrier gas containing a more stable concentration of an organometallic compound, particularly an organometallic compound which is solid at a normal temperature, and supply it to other devices (for example, organic The metal vapor phase growth device) further increases the utilization rate of the already filled solid organometallic compound. -9- 200945479 (Means for Solving the Problem) The inventors of the present invention conducted a review of the supply apparatus of an organometallic compound which is solid at normal temperature, especially at normal temperature and at normal pressure, and found that the following organometallic compound supply was used. The device can effectively utilize solid organometallic compounds. An organic metal compound supply device comprising: a charging container carried in an inactive carrier surrounded by an organometallic compound; and a metal-containing compound held in the charging container, particularly a lower portion thereof, and allowing the carrier gas to pass therethrough a support plate, a carrier gas introduction port located at an upper portion of the charging container, a carrier gas outlet opening at a bottom of the charging container and opening below the support plate, and a carrier gas and the carrier gas installed on the support plate and the carrier gas a blocking plate between the outlets and having a larger diameter than the carrier gas outlet, and the carrier gas is introduced into the filling container from the carrier gas inlet and passes through the organic metal held on the support plate from above. The compound is discharged from the carrier gas outlet. Therefore, the present invention is an organic metal compound supply device which has a charging container, is filled with an organometallic compound which is solid at a normal temperature, and supplies a carrier gas to sublimate the organometallic compound, and is characterized in that it further has: a support plate (9) for holding the organometallic compound (8) supported on the inactive carrier and allowing the carrier gas to pass therethrough, and a carrier gas introduction port located at the upper portion of the charging container in the crucible container (1) And a carrier gas outlet (5) located at the bottom of the filling container and opening below the support plate, and being mounted between the support plate (9) and the carrier gas outlet (5) The carrier gas outlet (5) has a larger diameter of -10-200945479. The carrier gas passes the carrier gas from above to the lower portion of the organic metal that is carried on the support plate that has been charged on the support plate. Compound [Effect of the Invention] By using the supply device of the present invention, an organometallic compound which is solid at normal temperature can be supplied together with a carrier gas at a more stable concentration, and can be increased by φ. Utilization charge to the organometallic compound Chen container. [Embodiment] The solid organometallic compound to be charged to the supply device of the present invention is useful, for example, as a raw material of a compound semiconductor produced by a vapor phase growth method, and is usually a normal temperature at normal temperature, and a normal pressure is solid. Examples thereof include trimethyl indium, dimethylchloroindium, cyclopentadiene indium, trimethylindium·trimethylphosphonium adduct, trimethylindium·trimethylphosphine adduct, and the like. Φ indium compound; zinc compound such as ethyl zinc iodide, ethyl cyclopentadienide, and cyclopentadienyl zinc; aluminum compound such as methyldichloroaluminum; methyldichlorogallium, dimethylchlorogallium a gallium compound such as dimethylbromide or the like; a bicyclocyclopentadienyl magnesium or the like. Further, the carrier carried by such an organometallic compound is not particularly limited as long as it is inactive to the solid organometallic compound. It is possible to use ceramics such as alumina, cerium oxide, mullite, glassy carbon, graphite, potassium titanate, quartz, tantalum nitride, boron nitride, tantalum carbide, etc.; stainless steel, aluminum, nickel, tungsten, etc. Metals; fluorinated resins, glass, etc. The shape of the carrier is not particularly limited, and various shapes such as an indefinite shape, a spherical shape, a fiber shape, a mesh shape, a coil shape -11 - 200945479, and a circular tube shape are possible. The carrier is preferably a fine unevenness having a surface having a smooth surface and having a size of about 100 to 2 000 //m, or a hole having a large number of pores (voids) in the carrier itself. Such a carrier can be exemplified by alumina balls, Rashi rings, Heli Pack gaskets, Dixon gaskets, stainless steel sintered bodies, glass fibers, metal cotton, and the like. As the support plate, a gold mesh or a hole plate shape as shown in Fig. 6 can be exemplified. Further, the support plate has an opening portion for the outlet pipe at the center portion thereof. The size of the opening of the support plate is such that the carrier does not fall, and is usually about 1 to 5 mm, preferably about 1.5 to 3 mm. The shape of the opening is not particularly limited, and examples thereof include a polygonal shape, a circular shape, an elliptical shape, and the like. The material of the support plate is not particularly limited as long as it is inactive against the solid organometallic compound. For example, glass, metal, ceramics or the like may be used. However, from the viewpoint of thermal conductivity, metal is preferred, and stainless steel is particularly preferred. On the other hand, although a sintered metal damper can be used as a support plate, if the opening of the sintered metal is too thin, the pressure loss is large, and the hole is clogged, and there is a possibility that the carrier gas is biased. In the organometallic compound supply device of the present invention, the carrier gas introduction port and the carrier gas outlet port are each an inlet for the carrier gas in the charging container and an outlet for the carrier gas in the charging container. In one preferred embodiment, the carrier gas introduction port and the carrier gas outlet port are openings in the end portion of the pipe for supplying the carrier gas to the inlet pipe, and the charging portion. The container discharges the carrier gas as an opening in the end of the pipe as the outlet pipe. Usually, such a gas pipe, -12-200945479 is a pipe having a circular cross section, and in this case, the shape of the inlet port and the outlet port are also circular. Needless to say, the inlet port and the outlet port may have other shapes, and the piping through which the carrier gas flows may have another cross section. In other aspects, the inlet port and the outlet port may be directly provided in the opening of the filling container. In the organometallic compound supply device of the present invention, the barrier plate is a pallet between the support plate and the outlet of the carrier gas. As a result, the position φ is in the field of the organometallic compound directly above the barrier plate and the overall flow of the descending carrier gas (substantially vertically below or near its direction), because it is in conflict with the barrier, or Conflict, so the direction of flow of such carrier gas is changed by the blocking plate in other directions. For example, it flows in a flow direction that is not vertically below. More specifically, it flows in a direction toward the side wall of the filling container (e.g., horizontal direction or oblique downward direction). Thereafter, such a carrier gas bypasses the peripheral portion of the barrier plate and flows toward the carrier gas outlet port located at a lower position thereof. Ο In order to prevent the carrier gas flow rate from being changed due to the concentration of the carrier gas at the periphery of the carrier gas outlet port It is effective to increase the diameter of the piping through which the carrier gas flows, and to increase the outlet. Further, when a large flow rate of the carrier gas flows, the solid organometallic compound to be charged may be directly discharged out of the container as a solid through the pipe. Therefore, the carrier gas outlet may not be excessively large and appropriately reduced. Preferably. Generally, although the carrier gas discharge pipe uses a pipe having an outer diameter of about 1 or less, the carrier gas can be led out from the charge container by bypassing the barrier plate by installing a blocker having a larger diameter than the pipe. Thus, more carrier gas flows to the peripheral portion of the side wall -13-200945479 of the filling container, and it is possible to suppress the carrier gas from being concentrated directly toward the tip end portion of the carrier gas outlet pipe without passing through the peripheral portion of the side wall of the charging container. In the present specification, the shape and size of the barrier plate are such that the structure formed as a barrier plate is projected on the vertical surface of the body of the filling container in the longitudinal direction (vertical direction) below the support plate. the meaning of. The shape and size of the barrier plate is such that if the positive projection of the barrier plate is superimposed on the positive projection of the carrier gas outlet, the positive projection of the barrier is the entirety of the positive projection covering the outlet, from the carrier gas outlet The shape and size of the portion extending outwardly around the front projection map is preferred. In the present invention, it is described as "a barrier plate having a larger diameter than the carrier gas outlet". Further, in the present invention, generally, the effect of the blocking plate is to obtain a pattern obtained when the blocking plate is projected in the vertical direction (or the vertical direction) of the container body in the vertical direction, and the outlet is similarly The resulting pattern in the case of projection is obtained by extending from the outside to the outside. Therefore, as shown in Fig. 12, the blocking plate is perpendicular to the longitudinal direction of the body of the filling container, and does not necessarily need to extend in the same plane, for example, it is inclined for the longitudinal direction or may be installed in a different plane. Further, even if the barrier plate is attached to the periphery of the carrier gas discharge pipe (that is, as shown in FIG. 4 to be described later, the outlet pipe penetrates the barrier plate), the carrier gas can be suppressed from being charged as described above. The peripheral portion of the side wall of the crucible is directly concentrated toward the tip end portion of the carrier gas discharge pipe. In this case, the shape and size of the barrier plate is the shape and size of the barrier plate assuming that the outlet tube is not present (i.e., the outlet tube is not penetrating the barrier plate). If the size of the barrier plate is excessively large and close to the diameter of the body of the filling container, the carrier gas at the bottom of the filling container is concentrated on the peripheral portion of the side wall, and the carrier gas around the carrier gas outlet tube above the blocking plate is not easy. The flow, the consumption of the solid organometallic compound located above the barrier plate is not easily caused. Further, the diameter of the barrier plate is about 10% to 75% of the inner diameter of the filling container, preferably about 20% to 60%. Further, when the shape of the blocking plate φ and the cross section of the filling container are not circular, the diameter of the above-mentioned blocking plate and the inner diameter of the filling container are based on the hydraulic equivalent diameter. The material of the barrier sheet is not particularly limited as long as it is inactive to the solid organometallic compound, and glass, metal, ceramics or the like may be used. However, from the viewpoint of thermal conductivity, metal is preferred, and stainless steel is preferred. The shape of the barrier plate is not particularly limited, and examples thereof include a polygonal shape, a circular shape, and an elliptical shape. However, a circular shape is particularly preferable from the viewpoint of symmetry. The barrier plate is located away from the solid organometallic compound and is more preferred than the solid organometallic compound. Since the position of the barrier plate is higher than the support plate or the same position as the support plate, the consumption of the solid organometallic compound is not easily caused because the flow of the carrier gas is easily blocked at the upper portion of the barrier plate. On the other hand, when the position of the barrier plate is lower than the support plate, since the solid organometallic compound is a field in which the flow of the carrier gas which is not present in the upper portion of the barrier plate is easily blocked, the solid organometallic compound is not easily consumed. The field can be reduced. Further, the horizontal circular cross section of the filling container in which the height of the barrier plate, the carrier gas outlet and the barrier plate are installed (or the level) is slightly the same as that of -15-200945479, that is, the centers of these are substantially the same The lead is preferred on the straight line. Even if it is not concentric, a certain degree of effect can be obtained. However, since the carrier gas flows symmetrically in the filling container by concentricity, the solid organometallic compound is uniformly consumed, and the use rate of the solid organometallic compound can be further improved. The method of carrying the solid organometallic compound in the inactive carrier is also possible by using any of the methods conventionally carried out. For example, it is employed: the carrier and the solid organometallic compound are put into a rotating weight in a predetermined weight ratio. Then, the heating is performed to melt the solid organometallic compound, and then, the method of rotating and stirring and gradually cooling is performed. The metal compound is heated and melted, and the carrier is introduced, and then the organometallic compound which has been excessively melted is taken out, followed by a method of gradually cooling. When carrying the carrier, it is necessary to remove oxygen and moisture contained in the carrier and other volatile impurities in advance. When oxygen and moisture are present on the surface of the carrier, the raw material solids are deteriorated and/or contaminated. When used as a raw material for vapor phase growth, the quality of the obtained film is not only impaired, but also cannot be achieved. Stable supply of raw materials for the purpose. In order to avoid such a problem, the carrier is recommended: preheating and vacuum degassing at a temperature within a range permitted by the material, and then the void portion is replaced by an inert gas such as nitrogen or argon. The solid organometallic compound supported on the carrier is usually in the range of about 10 to 100 parts by weight, preferably about 30 to 7 parts by weight, based on 100 parts by weight of the carrier. The case where the weight portion is downloaded is because the amount of the solid organometallic compound in the volume of the filling container is small, so that it is necessary to excessively increase the capacity of the container, which is uneconomical. Further, when the amount is about 100 parts by weight or more, the surface area of the solid organometallic compound per volume is not as large as expected, so that a sufficient effect cannot be obtained. An embodiment of the organometallic compound supply device formed by the charge container 1 filled with the solid organometallic compound of the present invention is shown in Fig. 4. A support plate 9 is disposed at a lower portion of the filling container 1 having a curved bottom portion, and the organometallic compound φ 8 carried on the inactive carrier can be held, and the carrier gas can pass therethrough. A carrier gas introduction pipe 2 and a carrier gas outlet pipe 3 are connected to the upper portion of the filling container. The introduction port 4 of the carrier gas is opened above the organometallic compound 8 carried on the charged inactive carrier in the upper portion of the filling container 1, and the carrier gas outlet pipe 3 is passed through the inside of the charging container 1, the carrier gas The outlet 5 is opened at the bottom of the filling container 1 toward the lower side of the support plate 9. In the illustrated embodiment, the barrier plate 10 is mounted above the carrier gas outlet port 5, but the barrier plate 10 is located at the same level as the carrier gas outlet port 5 (the vertical direction of the 塡 filling container 1). In other words, the blocking plate 10 may be configured to change the flow direction of the carrier gas gradually decreasing toward the periphery of the blocking plate. Therefore, those skilled in the art can easily understand that this case can also achieve the effects of the present invention described previously. Therefore, in the supply device of the present invention, the barrier plate is substantially located at the same level as the carrier gas outlet and the "level between the support plate and the carrier gas outlet", and includes: the barrier plate is located at a ratio The state of the layer position above the carrier gas outlet and the position of the position at the same level as the carrier gas outlet. Further, in the aspect shown in Fig. 4, the 'blocking plate' is a form in which the outer wall of the carrier gas outlet pipe extends from the outer wall of the carrier gas outlet pipe toward the side wall of the filling container (for example, having a central portion as a circle from the circular shape) The partially cut ring (or donut) shape of the outer shape of the carrier gas outlet tube. Further, in the illustrated embodiment, the carrier gas discharge pipe 3 passes through the inside of the charging container 1, but is not limited thereto, and the outlet 5 is opened below the support plate 9 at the bottom of the filling container 1. The carrier gas outlet pipe may be disposed outside the filling container 1. Further, an embodiment of the organometallic compound supply device formed by the filling container of the solid organometallic compound of the present invention is shown in Fig. 5. In the lower portion of the filling container 1 having a curved bottom portion, the organometallic compound 8 carried on the inactive carrier is held, and a support plate 9 through which the carrier gas can pass is disposed. A carrier gas introduction pipe 2 is connected to the upper portion of the filling container 1. The introduction port 4 of the carrier gas is opened above the organometallic compound 8 carried on the charged inactive carrier at the upper portion of the filling container 1. The carrier gas discharge pipe 3 is disposed outside the charging container 1, and the carrier gas outlet port 5 is opened below the support plate 9 at the bottom of the charging container 1. A blocking plate 1 is attached to the upper portion of the carrier gas outlet port 5. And 'in the aspect of Fig. 5', the carrier gas discharge pipe 3 is disposed outside the charging container 1 but is not limited thereto, and the outlet is opened below the support plate at the bottom of the filling container. The carrier gas outlet pipe may be disposed inside the filling container 1. The solid organic gold ruthenium compound 8 carried on the inactive carrier is supplied from the supply port (not shown) in the filled container 1 and is charged to the support -18-200945479 plate 9. Further, it is also possible to carry the substance in the infill container 1 on the inactive carrier. The carrier gas introduction pipe 2 is connected to a carrier gas (not shown) or the like, and a carrier gas meter, a vapor phase growth device (not shown), and the like are placed in a constant temperature bath. By supplying a carrier gas such as a hydrogen gas from a constant flow rate of φ and filling the container 1, the carrier port 4 is supported by a carrier gas from the upper side of the charging container 1 toward the carrier compound of the subordinate compound while being carried in the inactive carrier gap. The gas discharge pipe 3 is supplied to a vapor phase growth device or the like. In Figures 4 and 5, the filling is filled, but the bottom is a horizontal filling container, which is charged to the amount of the organic metal Φ carried on the inactive carrier (for example, the filling height, that is, recharge) In general, when the carrier gas introduction port 4 is divided into the carrier gas introduction port 4 and the upper portion of the organometallic compound 8 is uniformly guided, the present invention is not limited thereto. For example, in the case where the carrier gas introduction port can be used, the upper layer level of the layer compound 8 of the carrier gas introduction port 4 is almost the same, and the organometallic compound of the present invention is supplied to the solid organometallic compound supply source, The flow control package outlet pipe 3 is connected to the gas, for example, the urethane carrier gas introduction pipe 2 passes through the organometallic compound 8 introduced by the pregas through the carrier gas, and the organic gold outlet 5 is passed through the carrier gas guide. Although the bottom of 1 shows the use of bending, of course. Further, the filling container 1 of the compound 8 has a lower level of the layer 4 of the container in the vertical direction. However, it is possible to uniformly disperse the graded and charged organic metal in a dispersing plate or a showerhead carrier gas which is carried in the carrier gas of the inactive carrier. The device is the best device for supplying raw materials such as gas phase -19-200945479 for growth. Hereinafter, the examples of the present invention are shown, but the present invention is not limited to these. [Embodiment 1] The barrier plate is an organometallic compound supply device of the present invention which is the same as that of Fig. 4 except that it is attached to the tip end portion of the outlet pipe, that is, the level of the outlet. The bottom of the filling container 1 is curved and has a volume of about 1300 cm 3 (inner diameter: 108 mm, depth: 147 mm), and a support plate 9 is disposed from the bottom of the filling container at a position of 26 mm (the size of the opening: 2 mm of gold mesh) )). A dispersion plate 11 (a circular plate: a diameter of 18 mm) is attached to the carrier gas introduction port 4 so that the horizontal interval between the sky plate of the charging container 1 and the dispersion plate 11 is 3 mm, and the carrier gas can be slightly perpendicular to the central axis of the container. Imported. Further, a stopper plate 1 (a circular plate is attached) at a tip end portion (carrier gas outlet port 5) of the carrier gas outlet pipe 3 (outer diameter 8 mm, inner diameter 6 mm) which is opened at a position l1 mm below the support plate 9. The diameter is 30mm, but the center is through the outlet tube). The filling container 1 was filled with 585 g of an alumina sphere having an average particle diameter (diameter) of 4.5 mm and 300 g of trimethylindium (hereinafter referred to as TMI) as an inactive carrier. The charged charging vessel 1 is heated until it is about 110 ° C, and the TMI in the charging vessel 1 is melted, and then gradually cooled until the room temperature is rotated while stirring, and the TMI is carried on the alumina ball. Here, the container 1 is filled as a carrier gas, and the hydrogen gas is introduced from the introduction tube 2 at a slightly constant speed by about 900 cm 3 /min (at atmospheric pressure, the flow per unit area of the charge -20-200945479: about 9.5 cm 3 ) /cm2.), the TMI is supplied from the top to the bottom, and the hydrogen gas containing TMI is taken out from the carrier gas outlet pipe through the carrier port 5. When the charging container of the TMI generated by the carrier gas, that is, the hydrogen gas, is discharged, the pressure in the charging container 1 is 40 kPa (absolute pressure). The container 1 is placed in a constant temperature bath and held at 25 °C. The TMI concentration in the hydrogen gas from the charging container 1 was measured by using an EPISON (trade name, ultrasonic type) concentration meter (manufactured by Swan Scientific Equipment Co., Ltd.). The TMI rate (%) was obtained from the TMI period and from the hydrogen gas flow rate and the TMI concentration. The result is shown in Figure 7. The concentration of TMI was stable until the utilization rate became about 87%, and then decreased. [Example 2] The diameter of the barrier plate 10 (circular plate) attached to the tip end portion (carrier port 5) of the carrier gas discharge pipe 3 was 50 mm. The same filling container 1 as in Example 1 was implemented. Example 1 was carried on the alumina ball with TMI. The usage rate (%) of TMI was determined in the same manner as in Example 1. As shown in Figure 8. The concentration of TMI is until the usage rate becomes approximately stable and then decreases. [Example 3] Except that it is attached to the tip end portion of the carrier gas discharge tube 3 (the carrier-filled body is derived, and the concentration of the concentration of Thomas is determined from the conduction of 1 until the gas is guided, the result will be the result. In the same manner as in the first embodiment, the TIM is carried out in the same manner as in the first embodiment, except that the diameter of the barrier plate 1〇 (circular plate) of the gas guide-21 - 200945479 outlet 5) is 80 mm. Hold the alumina ball. The usage rate (%) of TMI was determined in the same manner as in Example 1. The result is shown in Figure 9. The concentration of TMI is stable until the usage rate becomes about 85%, and then decreases. [Comparative Example 1] The same filling container 1 as in Example 1 except that the blocking plate 10 (circular flat plate) was attached to the tip end portion (carrier gas outlet port 5) of the carrier gas discharge pipe 3, and Example 1 Similarly, the TMI is carried on an alumina ball. The usage rate (%) of TMI was determined in the same manner as in Example 1. The results are shown in Figure 1. The concentration of TMI is stable until the usage rate becomes about 83%, and then decreases. Further, the usage rate of TMI generated by the difference in the size of the barrier plate for the inner diameter of the filling container is as shown in Fig. 11. BRIEF DESCRIPTION OF THE DRAWINGS [Fig. 1] A cross-sectional view of a filling container in which a liquid organometallic compound is filled. [Fig. 2] A cross-sectional view of a filling container in which a solid organometallic compound is filled. [Fig. 3] A cross-sectional view of a filling container in which a solid organometallic compound supported on a conventional inactive carrier is charged. -22-200945479 [Fig. 4] Fig. 4 is a schematic cross-sectional view showing an aspect of the organometallic compound supply device of the present invention in a filling container for charging a solid organometallic compound supported on an inactive carrier. [Fig. 5] Fig. 5 is a cross-sectional view showing another aspect of the organometallic compound supply device of the present invention for charging a solid organic metal compound for inactive carrier. [Fig. 6] A plan view of an example of a support plate ((a) shows a gold mesh φ-shaped support plate, and (b) shows a hole-shaped support plate). [Fig. 7] A graph showing the results in Example 1. [Fig. 8] A graph showing the results in Example 2. [Fig. 9] A graph showing the results in Example 3. [Fig. 10] A graph showing the results in the comparative example. [Fig. 11] A graph showing the effect of the size of the barrier plate on its effect. [Fig. 12] A cross-sectional view showing other aspects of the blocking plate ((a) showing a conical blocking plate, (b) showing an inverted conical blocking plate, (c 〇) showing mounting of the semicircular plates in different planes Blocking board). [Description of main components] 1 : Filling container 2 : Carrier gas introduction tube 3 = Carrier gas outlet tube 4 : Carrier gas introduction port 5 = Carrier gas outlet 6 = Liquid organometallic compound-23 - 200945479 7: Solid organic metal Compound 8: Solid organometallic compound 9 supported on an inactive carrier: support plate I 〇: barrier plate II: dispersion plate-24-