201034955 ’ 六、發明說明: 【發明所屬之技術領域】 本案發明關於發熱裝置。特別地,關於在使四氯矽烷 與氫反應而轉化成三氯矽烷的三氯矽烷製造裝置中之發熱 裝置’及使用其的反應塔。 【先前技術】 三氯矽烷在作爲半導體或太陽電池等元件中所使用的 高純度矽之原料氣體’估計需求係愈來愈增加,向來迫切 Ο 期望以高效率來製造彼等。 —般地,作爲用於製造高純度的矽(Si:矽)之原料所使 用的三氯矽烷(SiHCl3),係可藉由使四氯矽烷(SiCl4:四氯 化矽)與氫反應而轉化來製造。 即,三氯矽烷係藉由以下反應式(1)的轉化反應來生成 〇 S1CI4+ H2 S1HCI3+ HC1 · · · (1) 此反應係藉由在碳製的反應容器中將由已氣化的四氯 Ο 矽烷與氫所構成的原料氣體加熱到約800°C〜約1 3 00°C而 進行。而且,爲了提高對三氯矽烷的轉化率,進行反應式 (1)的生成氣體之急冷。 又,目的之矽係藉由以下反應式(2)、(3)的三氯矽烷之 還原反應與熱分解反應而生成。201034955 ′. Description of the invention: [Technical field to which the invention pertains] The invention relates to a heat generating device. In particular, the heat generating device in the apparatus for producing trichloromethane which is converted into trichloromethane by reacting tetrachlorosilane with hydrogen and a reaction tower using the same. [Prior Art] The estimated demand for the raw material gas of high-purity ruthenium used as a component such as a semiconductor or a solar cell is increasing, and it has been urgent to manufacture them with high efficiency. In general, trichlorosilane (SiHCl3) used as a raw material for producing high-purity lanthanum (Si: lanthanum) can be converted by reacting tetrachloro decane (SiCl4: hafnium tetrachloride) with hydrogen. To manufacture. That is, trichloromethane is produced by the conversion reaction of the following reaction formula (1) to produce 〇S1CI4+H2S1HCI3+HC1 · (1) This reaction is carried out by gasification of tetrachloroguanidine in a carbon reaction vessel. The raw material gas composed of decane and hydrogen is heated to a temperature of from about 800 ° C to about 1 300 ° C. Further, in order to increase the conversion rate to triclosan, the formation gas of the reaction formula (1) is quenched. Further, the target is produced by a reduction reaction and a thermal decomposition reaction of trichlorosilane of the following reaction formulas (2) and (3).
SiHCl3 + H2 — Si + 3HC1 ---(2) 4SiHCl3 — Si+ 3SiCl4+ 2H2 ---(3) 例如專利文獻1中揭示一種氯矽烷與氫的反應容器, 201034955 其中發熱體所包圍的反應室具備由同心配置的2支管所形 成的外室與內室。 於該文獻中’提案經由在反應室的下部所設置的熱交 換器’由反應室的下方供應氫與四氯矽烷的供給氣體,同 時由反應室的下方排出反應後的生成氣體之反應容器。 又’專利文獻2中揭示一種三氯矽烷製造裝置,其主 要具備將四氯矽烷與氫的供給氣體供應給內部,藉由轉化 反應生成三氯矽烷與氯化氫的反應生成氣體之反應容器, Ο 配置於反應容器的周圍之將反應容器的加熱機構,以覆蓋 反應容器及加熱機構的周圍之方式所配置的絕熱材,以及 將反應容器、加熱機構及絕熱材收納的收納容器。 還有,作爲三氯矽烷製造裝置中所使用的發熱體,使 用連結於金屬製端子部的碳製發熱體。 然而,於如此的構成時,由於發熱部係約8 00 °C〜約 1 3 00 °C的高溫,故在金屬製端子部與碳製發熱體的連結部 中,發生由於熱膨脹率的不同所致的應力,在該連結部會 〇 發生破損。 [專利文獻1]日本發明專利第378 1 43 9號公報 [專利文獻2]特開2008-133175號公報 【發明內容】 本案發明之目的爲提供可高效率地冷卻發熱裝置的端 子部,可抑制構成零件的腐蝕或破損之發熱裝置。 依照本案發明,可提供由一對發熱體所構成,發熱體 具有略圓柱狀的金屬端子與略圓柱狀的碳端子和略圓柱狀 201034955 的發熱部,金屬端子的下端部與碳端子的上端部連結,碳 端子的下端部與發熱部的上端部連結,金屬端子在其內部 具有通水路,用於加熱將含四氯矽烷與氫的氣體供應給內 部而生成含三氯矽烷與氯化氫的氣體之反應容器的發熱裝 置。 依照本案發明的發熱裝置’可高效率地冷卻端子部, 可抑制構成零件的破損。 【實施方式】 〇 實施發明的最佳形態 以下’邊參照圖面邊說明本案發明的發熱裝置之具體 實施態樣。 首先,本實施形態的發熱裝置1係如圖1〜3所示地, 爲用於加熱將含四氯矽烷與氫的氣體供應給內部而生成含 三氯矽烷與氯化氫的氣體之反應容器的發熱裝置1,其特 徵爲:上述發熱裝置1係由一對發熱體2所構成,上述發 熱體2具有略圓柱狀的金屬端子3與略圓柱狀的碳端子4 β 和略圓柱狀的發熱部5,上述金屬端子3的下端部與上述 碳端子4的上端部連結’上述碳端子4的下端部與上述發 熱部5的上端部連結,上述金屬端子3在其內部具有通水 路6。 由上述構成所成的發熱裝置1係如圖2或圖3所示地 ,由於在金屬端子3內部設置特徴的通水路6,例如即使 在約800 °C〜約1300 °C的高溫中,也可高效率地冷卻端子 部,可抑制構成零件的腐蝕或破損。 201034955 [金屬端子] 金屬端子3係與習用者同樣,如圖2或圖3所示地, 從耐熱性的方面來看,典型地具有略圓柱狀的外徑。金屬 端子3的形狀係沒有特別的限定,例如可爲長方體形狀等 〇 作爲金屬端子3的材料,並沒有特別的限定,較佳爲 使用具有耐熱性·耐SCC(應力腐蝕破裂)性的SUS材等合 金材料。 作爲如此的材料,例如較佳爲英高鎳(inconel) 600等的 耐SCC性高之合金》 (連結部) 金屬端子3的下端部係連結於後述碳端子4的上端部 。因此,在金屬端子3的下端部,設有用於連結碳端子4 的連結手段(連結部7)。 例如,作爲連結手段,如圖2或圖3地,上述金屬端 子3具有陽螺紋部8,上述碳端子4具有陰螺紋部9,上述 金屬端子3與上述碳端子4較佳係成爲在上述陽螺,紋^ 8 及上述陰螺紋部9互相螺合的構造。 藉由成爲如此的構成,視需要可容易地進行金屬@ + 3及碳端子4的拆卸·交換。 [通水路] 上述金屬端子3係在其內部設有通水路6。 該通水路6係使冷卻水循環以便冷卻金屬端子3者, 如圖2或圖3所示地,具備沿著略圓柱狀的金屬端子3之 201034955 內部的軸方向所形成的空洞部、與連接於該空洞部的冷卻 水用之流入口 1 〇和排出口 π。 通水路6的形狀係沒有特別的限定’較佳爲可有效率 地循環冷卻水之圓柱狀的空洞狀。 又,該通水路6亦可單純地在金屬端子3設有流入口 10與排出口 11者,較佳爲如圖2或圖3地,設有抵達通 水路6的通水路之底部12的冷卻水用注入管13之構造》 於成爲如此的構造時,冷卻水係通過該注入管1 3而流 〇 到通水路6的下端,由上端的排出口 11排出。於由如此構 造所成的通水路6中’冷卻水係高效率地循環’可進行有 效的冷卻。 (通水路的深度) 通水路6的深度,即金屬端子3下端部的通水路6之 形成位置,較佳爲如圖2所示地,通水路6的通水路之底 部12係在抵達金屬端子3部的下端部之陽螺紋部8的位置 〇 ^ 藉由使通水路6的深度成爲如此般,特別地由於可有 效率地冷卻上述連結部,故可有效地抑制上述金屬端子3 與上述碳端子4的連結部之腐鈾。 通水路6的深度較佳爲形成到陽螺紋部8的形成寬度 之100%,更佳爲到150%的深度爲止。 再者,通水路6的深度,例如像圖3所示地,通水路 的底部12可在比金屬端子3的下端部之陽螺紋部8還上方 的位置。 201034955 (通水路的直徑) 能保持金屬端子3的充 爲金屬端子3的直徑之 6的直徑若爲金屬端子 水流速變快、總傳熱係 所示地,較佳爲在金屬 配合其直徑而變小。如 來規定通水路6的直徑 型地流動水,但例如亦 液、丙二醇水溶液等的 上端部連結於上述金屬 結於後述的發熱部5之 子3與發熱部5之間存 冷卻,而可防止將碳製 發生的破損。 述金屬端子3或發熱部 通水路6的直徑只要是設計成 分強度,則沒有特別的限制,較佳 2 0 %〜7 0 %的範圍。特別地,通水路 3的直徑之3 0 %〜5 0 %,則可得到通 數上升的效果。 又,通水路6的直徑係如圖2 端子3部的下端部之陽螺紋部8, Ο 此地,藉由配合金屬端子3的外徑 ,可更有效地進行冷卻。 再者,於上述通水路6中,典 可流動氯化鈣水溶液、乙二醇水溶 冷卻液、或冷卻氮等的冷卻氣體。 [碳端子] 碳端子4係如圖1所示地,其 端子3的下端部,而且其下端部連 0上端部。 如此的碳端子4係介於金屬端 在,藉由將金屬端子3及碳端子4 的發熱體直接連接於金屬端子時所 (碳端子的直徑) 該碳端子4的直徑較佳爲比上 5的直徑還大。藉此,可得到減小發熱量的效果。 具體地,碳端子4的直徑較佳爲金屬端子3或發熱部 201034955 5的1〜2倍。由於碳端子4的直徑爲金屬端子3或發熱部 5的1〜2倍,故可得到減小發熱量的效果。 [發熱部] 發熱部5係如圖1所示地’其上端部連結於上述碳端 子4的下端部,該發熱部5與碳端子4較佳例如是藉由螺 牙來螺合。 又,上述碳端子4及/或發熱部5的碳較佳係石墨。 由於爲石墨,可得到提高耐熱性的效果。 〇 (被膜處理) 較佳爲在碳端子4及發熱部5的表面上形成碳化矽被 膜。 上述碳端子4及發熱部5,由於以碳當作主材料,經 由在高溫的空氣中之水等,遭受組織的減薄或脆化。由於 對於如此的化學分解,碳化矽被膜之耐性極高,故可防止 碳組織的化學浸蝕。 碳化矽被膜係沒有特別的限制,典型地可藉由CVD法 〇 v 來蒸鍍而形成。 爲了藉由CVD法在碳端子4及發熱部5的表面上形成 碳化矽被膜’例如可使用:用如四氯矽烷或三氯矽烷的鹵 化矽化合物與甲烷或丙烷等的烴化合物之混合氣體的方法 ,或邊以氫將如甲基三氯矽烷、三苯基氯矽烷、甲基二氯 砍院、二甲基二氯矽烷、三甲基氯矽烷之具有烴基的鹵化 政化合物熱分解,邊在經加熱的碳端子4及發熱部5之表 面上沈積碳化矽的方法。 -10- 201034955 碳化矽被膜的厚度較佳爲10〜5 00μιη,更佳爲30〜 3 0 0 μπι。 碳化矽被膜的厚度若爲ΙΟμπι以上,則可充分抑制高 溫的空氣中之水等所致的碳端子4及發熱部5之腐蝕,而 若爲5 0 0 μπι以下,則亦不會助長碳化矽被膜的龜裂或碳端 子4及發熱部5的破裂。 所形成的碳化矽被膜係緻密均質而沒有針孔的被膜, 由於化學安定性優異,於由施有碳化矽被膜的碳端子4及 發熱部5所構成的發熱裝置1中,可減低設備的修繕頻率 ’可進一步提高作業效率。 [反應塔] 接著,說明本實施形態的具備發熱裝置1之反應塔1 4 〇 反應塔14係如圖4所示地,主要由將含四氯矽烷與氫 的氣體供應給內部而生成含三氯矽烷與氯化氫的氣體之反 應容器15、用於加熱該反應容器的發熱裝置1、與以包圍 反應容器15及發熱裝置1的方式所配置的外筒容器16所 構成。 上述反應容器15係略圓筒形狀的容器,用於在高溫環 境下使四氯矽烷與氫反應。此容器具有用於納入原料的四 氯矽烷與氫氣之氣體導入口 17、與用於導出含三氯矽烷與 氯化氫的反應生成氣體之反應生成氣體抽出口 18。 再者’於本實施形態中,雖然爲在反應容器的底部設 置氣體導入口 17,在反應容器15的上方設有反應生成氣 201034955 體抽出口 18之構成,但是關 定。 上述發熱裝置1係在反 述外筒容器1 6之間,隔著朽 發熱裝置1係如圖4所示地 置。 但是,發熱裝置的設置 所限制,例如亦可將電極當 ®直地設置。 上述外筒容器16係外 側配置有碳製的面板或耐火 容器1 6具有絕熱材性能,使 於內部,保持反應容器內1: 藉由在周圍所配置的上 容器15,使由該反應容器1 氯矽烷及氫氣在約800°C〜 〇 該反應容器15的反應生成I 反應生成物氣體之形式取出 供應給用於分離三氯矽烷的 <作用效果> 以下說明上述實施形態 上述實施形態的發熱裝 發熱體具有略圓柱狀的金屬 圓柱狀的發熱部’金屬端子 丨於此等的位置’並不受其所限 應塔14內的反應容器15與上 i定的間隔設置複數個。此處’ ,以由反應塔14懸掛的狀態設 方法係不受如上述的懸掛方式 作下側,在反應塔的底部略垂 丨!1由不銹鋼等的金屬所構成’內 磚之略圓筒狀的容器。該外筒 來自上述發熱裝置1的發熱止 5的溫度之任務。 述發熱裝置1來加熱上述反應 5的氣體導入口 17所導入的四 約1300 °C的高溫進行反應,由 氣體抽出口 18以含三氯矽烷的 。然後,上述反應生成氣體係 冷卻裝置等。 的發熱裝置1之作用效果。 置1係由一對發熱體所構成, 端子與略圓柱狀的碳端子和略 的下端部與碳端子的上端部連 -12- 201034955 結,碳端子的下端部與發熱部的上端部連結,金屬端子在 其內部具有通水路,用於加熱將含四氯矽烷與氫的氣體供 應給內部而生成含三氯矽烷與氯化氫的氣體之反應容器的 發熱裝置。 若依照由上述構成所成的發熱裝置1,由於上述金屬 端子3具有通水路6,故可高效率地冷卻由金屬端子3及 碳端子4所成的端子部,可抑制構成零件之由於熱膨脹所 致的破損。 又,於上述發熱裝置1中,在上述金屬端子3的下端 部與上述碳端子4的上端部連結的連結部7中,上述金屬 端子3具有陽螺紋部8,上述碳端子4具有陰螺紋部9,上 述金屬端子3與上述碳端子4係在上述陽螺紋部8及上述 陰螺紋部9互相螺合,故可容易地進行金屬端子3及碳端 子4的拆卸•交換。 而且,於上述發熱裝置1中,由於上述通水路的底部 1 2係抵達上述金屬端子3的陽螺紋部8爲止,可特別有效 率地冷卻上述連結部7,故可有效地抑制上述金屬端子3 與上述碳端子4的連結部之由於熱膨脹所致的破損。 又,於上述發熱裝置1中,由於上述碳端子4的直徑 爲上述金屬端子3或發熱部5的1〜2倍,可得到減低發熱 量的效果》 再者,於上述發熱裝置1中,藉由對上述碳端子4及/ 或上述發熱部5施予碳化矽被膜,可保護碳端子4及發熱 部5的表面而防止腐蝕。 -13- 201034955 還有,於上述發熱裝置1中,由於上述碳化矽被膜係 由CVD法所形成,爲厚度ΙΟμιη〜500μιη的碳化矽被膜, 故可充分抑制高溫的空氣中之水等所致的碳端子4及發熱 部5之腐蝕,亦不會助長碳化矽被膜的龜裂或碳端子4及 發熱部5的破裂。 又,於上述發熱裝置1中,由於上述碳端子4部及/或 發熱部5的碳係石墨,故可得到提高耐熱性的效果。 再者,於具備將含四氯矽烷與氫的氣體供應給內部而 ^ 生成含三氯矽烷氯化氫的氣體之反應容器15、以包圍該反 應容器15的方式所配置的上述發熱裝置1、以包圍上述反 應容器15及上述發熱裝置1的方式所配置的外筒容器16 之反應塔14中,由於上述金屬端子3具有通水路6,故可 高效率地冷卻由金屬端子3及碳端子4所成的端子部,可 抑制構成零件之由於熱膨脹所致的破損。 以上雖然說明本案發明的發熱裝置,惟本案發明不受 ^ 此等所限定。 〇 [實施例] [實施例1] 如圖3所示地,製作一種使用金屬端子的發熱裝置, 該金屬端子設有通水路。 該發熱裝置係如圖1所示地’組合2支由金屬端子(直 徑30mm)、碳端子(直徑30mm)及發熱部(直徑20mm)所構 成的發熱體而成爲一對。通水路的直徑係金屬端子的直徑 之 5 0%。 -14- 201034955 在各構件的連結部設有螺合連結手段,其互相連結。 如圖4所示地,在反應塔的內部設置上述發熱裝置, 連續地運轉2000小時後,將裝置解體而調查端子部的破損 ,結果端子部的破損少,可再運轉2 0 0 0小時。 [實施例2] 於實施例2中,碳端子及發熱部係與實施例1者同樣 ,除了如圖2所示地,使用僅加深通水路的深度而到達連 結部爲止的金屬端子以外,製作與實施例1同樣的發熱裝 置。 然後,進行與實施例1同樣的實驗,將裝置解體而調 查端子部的破損,結果端子部的破損少,再2000小時的運 轉係可能3次。 [實施例3] 於實施例3中’碳端子及發熱部係與實施例1者同樣 ’除了使用通水路的直徑爲實施例1的丨.5倍之金屬端子 以外,製作與實施例1同樣的發熱裝置。 然後,進行與實施例1同樣的實驗’將裝置解體而調 查端子部的破損,結果端子部的破損少,再2000小時的運 轉係可能3次。 [實施例4] 於實施例4中’使用實施例2的金屬晴子及發熱部 與比該金屬端子還直徑粗的碳端子(直徑4 〇mm) ’製作發熱 裝置。 然後,進行與實施例1同樣的實驗’將裝置解體而調 -15- 201034955 查端子部的破損’結果端子部的破損少,再2000小時的運 轉係可能5次。 [比較例1 ] 除了使用無通水路的金屬端子以外,製作與實施例1 同樣的發熱裝置。然而,進行運轉時,在未經過2000小時 的時間點,發熱裝置破損。進行解體,結果在碳端子與金 屬端子之連接部附近發生斷裂。 <考察> ^ 由以上的實驗結果可知,於本案發明的實施例之發熱 裝置中,端子部幾乎沒有破損,而爲耐久性優異者。特別 地,於實施例2至實施例4的發熱裝置中,即使複數次的 使用也能耐得住。 如此地,相對於實施例的發熱裝置所得到的良好結果 ,比較例中的螺紋部之破損係顯著,短時間內需要交換。 以上’以實施例爲基礎來說明本案發明。惟,此等實 施例係本案發明的例示,本業者理解其它各種變形例係可 〇 能’而且該變形例亦在本案發明的範圍內。 【圖式簡單說明】 圖1係本案發明的實施形態之發熱裝置的示意圖。 圖2係本案發明的實施形態之發熱裝置的端子部之示 意縱剖面圖。 圖3係本案發明的實施形態之發熱裝置的端子部之示 意縱剖面圖。 圖4係本案發明的實施形態之用發熱裝置的四氯矽烷 -16- 201034955 反應塔之示意圖。 【主要元件符號說明】SiHCl3 + H2 - Si + 3HC1 - - (2) 4SiHCl3 - Si + 3SiCl4 + 2H2 - (3) For example, a reaction vessel of chlorodecane and hydrogen disclosed in Patent Document 1, 201034955, wherein the reaction chamber surrounded by the heating element is provided The outer chamber and the inner chamber formed by the two tubes arranged concentrically. In this document, it is proposed to supply a supply gas of hydrogen and tetrachloromethane from the lower side of the reaction chamber via a heat exchanger provided in a lower portion of the reaction chamber, and to discharge a reaction gas for generating gas after the reaction from the lower side of the reaction chamber. Further, Patent Document 2 discloses a device for producing triclosan, which mainly comprises a reaction vessel for supplying a supply gas of tetrachlorosilane and hydrogen to the inside, and generating a gas by a reaction of trichloromethane and hydrogen chloride by a conversion reaction, Ο configuration The heating means for the reaction container around the reaction container is a heat insulating material disposed so as to cover the periphery of the reaction container and the heating means, and a storage container for accommodating the reaction container, the heating means, and the heat insulating material. Further, as the heating element used in the apparatus for producing chloroform, a carbon heating element connected to a metal terminal portion is used. However, in such a configuration, since the heat generating portion has a high temperature of about 800 ° C to about 1 300 ° C, the connection portion between the metal terminal portion and the carbon heating element is different in thermal expansion coefficient. The resulting stress is broken at the joint. [Patent Document 1] Japanese Laid-Open Patent Publication No. 378-43-95 [Patent Document 2] JP-A-2008-133175 SUMMARY OF THE INVENTION An object of the present invention is to provide a terminal portion capable of efficiently cooling a heat generating device, which can suppress A heat generating device that causes corrosion or breakage of parts. According to the invention, it is possible to provide a pair of heat generating bodies having a substantially cylindrical metal terminal, a slightly cylindrical carbon terminal, and a slightly cylindrical heat generating portion of 201034955, and a lower end portion of the metal terminal and an upper end portion of the carbon terminal. The lower end portion of the carbon terminal is connected to the upper end portion of the heat generating portion, and the metal terminal has a water passage therein for heating a gas containing tetrachlorosilane and hydrogen to the inside to generate a gas containing trichloromethane and hydrogen chloride. A heat generating device for the reaction vessel. According to the heat generating device of the present invention, the terminal portion can be efficiently cooled, and damage of the component can be suppressed. [Embodiment] BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a specific embodiment of a heat generating device according to the present invention will be described with reference to the drawings. First, the heat generating device 1 of the present embodiment is a heat generating reactor for heating a gas containing trichlorosilane and hydrogen to supply a gas containing tetrachlorosilane and hydrogen, as shown in Figs. 1 to 3, as shown in Figs. The device 1 is characterized in that the heat generating device 1 is composed of a pair of heat generating bodies 2 having a substantially cylindrical metal terminal 3 and a slightly cylindrical carbon terminal 4 β and a slightly cylindrical heat generating portion 5 The lower end portion of the metal terminal 3 is connected to the upper end portion of the carbon terminal 4. The lower end portion of the carbon terminal 4 is connected to the upper end portion of the heat generating portion 5, and the metal terminal 3 has a water passage 6 therein. As shown in FIG. 2 or FIG. 3, the heat generating device 1 formed as described above has a special water passage 6 provided inside the metal terminal 3, for example, even at a high temperature of about 800 ° C to about 1300 ° C. The terminal portion can be efficiently cooled, and corrosion or breakage of the constituent parts can be suppressed. 201034955 [Metal Terminal] The metal terminal 3 is similar to the conventional one, and as shown in FIG. 2 or FIG. 3, it has a substantially cylindrical outer diameter from the viewpoint of heat resistance. The shape of the metal terminal 3 is not particularly limited, and may be, for example, a rectangular parallelepiped shape or the like as the material of the metal terminal 3, and is not particularly limited, and it is preferable to use a SUS material having heat resistance and SCC resistance (stress corrosion cracking). Alloy materials. As such a material, for example, an alloy having a high SCC resistance such as inconel 600 is preferable. (Connecting portion) The lower end portion of the metal terminal 3 is connected to the upper end portion of the carbon terminal 4 to be described later. Therefore, a connection means (connection portion 7) for connecting the carbon terminals 4 is provided at the lower end portion of the metal terminal 3. For example, as a connecting means, as shown in FIG. 2 or FIG. 3, the metal terminal 3 has a male screw portion 8, and the carbon terminal 4 has a female screw portion 9, and the metal terminal 3 and the carbon terminal 4 are preferably formed in the above-mentioned anode. The screw, the pattern 8 and the female screw portion 9 are screwed to each other. With such a configuration, the metal @ + 3 and the carbon terminal 4 can be easily removed and exchanged as needed. [Water passage] The metal terminal 3 described above is provided with a water passage 6 therein. The water passage 6 circulates the cooling water to cool the metal terminal 3, and as shown in FIG. 2 or FIG. 3, has a hollow portion formed along the axial direction of the interior of the slightly cylindrical metal terminal 3, 201034955, and is connected to The cooling water for the hollow portion is used for the inlet 1 and the outlet π. The shape of the water passage 6 is not particularly limited. It is preferable to efficiently circulate the cylindrical hollow shape of the cooling water. Further, the water passage 6 may be provided with the inflow port 10 and the discharge port 11 in the metal terminal 3, preferably, as shown in Fig. 2 or Fig. 3, the cooling of the bottom portion 12 of the water passage leading to the water passage 6 is provided. In the structure of the water injection pipe 13, the cooling water flows through the injection pipe 13 to the lower end of the water passage 6, and is discharged from the discharge port 11 at the upper end. In the water passage 6 thus constructed, the "cooling water system is efficiently circulated" to perform effective cooling. (Depth of the water passage) The depth of the water passage 6, that is, the formation position of the water passage 6 at the lower end of the metal terminal 3, is preferably as shown in Fig. 2, and the bottom 12 of the water passage of the water passage 6 is at the metal terminal. The position of the male screw portion 8 at the lower end portion of the three portions is such that the depth of the water passage 6 is such that the above-described connecting portion can be efficiently cooled, so that the metal terminal 3 and the carbon can be effectively suppressed. The uranium of the joint of the terminal 4. The depth of the water passage 6 is preferably formed to 100% of the formation width of the male screw portion 8, more preferably to a depth of 150%. Further, the depth of the water passage 6 is, for example, as shown in Fig. 3, and the bottom portion 12 of the water passage can be positioned above the male screw portion 8 of the lower end portion of the metal terminal 3. 201034955 (diameter of water passage) The diameter of the metal terminal 3 which can be filled with the diameter of the metal terminal 3 can be as long as the metal terminal water flow rate is fast, and the total heat transfer system is shown, preferably the metal is matched with the diameter thereof. Become smaller. In the meantime, the water flowing in the diameter of the water passage 6 is defined. However, for example, the upper end portion of the liquid, the propylene glycol aqueous solution or the like is connected to the metal to be cooled between the sub-part 3 of the heat generating portion 5 to be described later and the heat generating portion 5, thereby preventing carbon from being deposited. The damage occurred. The diameter of the metal terminal 3 or the heat generating portion water passage 6 is not particularly limited as long as it is designed to be a component strength, and is preferably in the range of 20% to 70%. In particular, if the diameter of the water passage 3 is 30% to 50%, the effect of increasing the number of passages can be obtained. Further, the diameter of the water passage 6 is the male screw portion 8 at the lower end portion of the terminal 3 portion of Fig. 2, and the outer diameter of the metal terminal 3 can be blended to more effectively perform cooling. Further, in the water passage 6 described above, a calcium chloride aqueous solution, a glycol water-soluble coolant, or a cooling gas such as nitrogen may be cooled. [Carbon terminal] The carbon terminal 4 is a lower end portion of the terminal 3 as shown in Fig. 1, and its lower end portion is connected to the upper end portion. Such a carbon terminal 4 is interposed between the metal end and the heating element of the metal terminal 3 and the carbon terminal 4 (the diameter of the carbon terminal). The diameter of the carbon terminal 4 is preferably 5 The diameter is still large. Thereby, the effect of reducing the amount of heat generation can be obtained. Specifically, the diameter of the carbon terminal 4 is preferably 1 to 2 times the diameter of the metal terminal 3 or the heat generating portion 201034955 5 . Since the diameter of the carbon terminal 4 is 1 to 2 times the diameter of the metal terminal 3 or the heat generating portion 5, the effect of reducing the amount of heat generation can be obtained. [The heat generating portion] The heat generating portion 5 is connected to the lower end portion of the carbon terminal 4 as shown in Fig. 1. The heat generating portion 5 and the carbon terminal 4 are preferably screwed by screws, for example. Further, the carbon of the carbon terminal 4 and/or the heat generating portion 5 is preferably graphite. Since it is graphite, the effect of improving heat resistance can be obtained. 〇 (film treatment) It is preferable to form a tantalum carbide film on the surface of the carbon terminal 4 and the heat generating portion 5. The carbon terminal 4 and the heat generating portion 5 are subjected to thinning or embrittlement of the structure due to the use of carbon as a main material and water or the like in the high-temperature air. Since such a chemical decomposition, the ruthenium carbide film is extremely resistant, and chemical corrosion of the carbon structure can be prevented. The tantalum carbide film system is not particularly limited, and is typically formed by vapor deposition by a CVD method. In order to form a tantalum carbide film on the surface of the carbon terminal 4 and the heat generating portion 5 by the CVD method, for example, a mixed gas of a halogen compound such as tetrachlorosilane or trichloromethane and a hydrocarbon compound such as methane or propane may be used. Or thermally decomposing a halogenated compound having a hydrocarbon group such as methyltrichloromethane, triphenylchlorodecane, methyldichloromethane, dimethyldichlorodecane or trimethylchloromethane by hydrogen A method of depositing tantalum carbide on the surface of the heated carbon terminal 4 and the heat generating portion 5. -10- 201034955 The thickness of the tantalum carbide film is preferably from 10 to 500 μm, more preferably from 30 to 300 μm. When the thickness of the tantalum carbide film is ΙΟμπι or more, the corrosion of the carbon terminal 4 and the heat generating portion 5 due to water or the like in the high-temperature air can be sufficiently suppressed, and if it is 500 μm or less, the niobium carbide is not promoted. Cracking of the film or cracking of the carbon terminal 4 and the heat generating portion 5. In the heat generating device 1 including the carbon terminal 4 and the heat generating portion 5 to which the tantalum carbide film is applied, the heat-resistant device 1 having the carbonized ruthenium film and the heat generating portion 5 can be reduced in equipment. Frequency 'can further improve work efficiency. [Reaction tower] Next, the reaction tower 14 including the heat generating device 1 of the present embodiment will be described. As shown in Fig. 4, the gas is mainly supplied by supplying a gas containing tetrachlorosilane and hydrogen to the inside. A reaction vessel 15 for a gas of chlorosilane and hydrogen chloride, a heat generating device 1 for heating the reaction vessel, and an outer cylinder container 16 disposed to surround the reaction vessel 15 and the heat generating device 1. The above reaction vessel 15 is a substantially cylindrical vessel for reacting tetrachlorosilane with hydrogen in a high temperature environment. This container has a gas introduction port 17 for introducing a raw material of tetrachlorosilane and hydrogen, and a reaction gas generation port 18 for deriving a reaction product gas containing trichloromethane and hydrogen chloride. In the present embodiment, the gas introduction port 17 is provided at the bottom of the reaction container, and the reaction product generation unit 2010 is provided above the reaction container 15, but the configuration is determined. The heat generating device 1 is disposed between the outer cylinder containers 16 and the heat generating device 1 is placed as shown in Fig. 4 . However, the setting of the heat generating device is limited, for example, the electrode can be set to be straight. The outer cylinder container 16 is provided with a carbon panel or a refractory container 16 having a heat insulating material performance on the outer side, and the inside of the reaction container is held inside the container 1 by the upper container 15 disposed around the reaction container 1 The chloroformane and the hydrogen gas are taken out in the form of a reaction product of the reaction vessel 15 at a temperature of about 800 ° C to I. The reaction product is supplied to the trichloromethane for separation. [Effects and Effects] The following describes the embodiment of the above embodiment. The heat-generating heating element has a substantially cylindrical metal-column heat-generating portion 'the metal terminal 丨 at the same position' and is not limited by the reaction container 15 in the column 14 at a predetermined interval. Here, the method in which the reaction tower 14 is suspended is not subjected to the lower side of the suspension method as described above, and is slightly sag at the bottom of the reaction tower! 1 is composed of a metal such as stainless steel. Shaped container. This outer cylinder comes from the task of the temperature of the heat generation 5 of the above-described heat generating device 1. The heat generating device 1 heats the four high temperature of about 1300 °C introduced by the gas introduction port 17 of the reaction 5, and the gas extraction port 18 contains trichloromethane. Then, the above reaction produces a gas system cooling device or the like. The effect of the heat generating device 1. The first unit is composed of a pair of heating elements, and the terminal and the slightly cylindrical carbon terminal and the slightly lower end portion are connected to the upper end portion of the carbon terminal -12-201034955, and the lower end portion of the carbon terminal is connected to the upper end portion of the heat generating portion. The metal terminal has a water passage inside thereof for heating a heat generating device that supplies a gas containing tetrachlorosilane and hydrogen to the inside to form a reaction vessel containing a gas of trichlorosilane and hydrogen chloride. According to the heat generating device 1 formed as described above, since the metal terminal 3 has the water passage 6, the terminal portion formed by the metal terminal 3 and the carbon terminal 4 can be efficiently cooled, and the thermal expansion of the component can be suppressed. Damage caused. Further, in the heat generating device 1, in the connecting portion 7 in which the lower end portion of the metal terminal 3 is connected to the upper end portion of the carbon terminal 4, the metal terminal 3 has a male screw portion 8, and the carbon terminal 4 has a female screw portion. 9. The metal terminal 3 and the carbon terminal 4 are screwed to each other in the male screw portion 8 and the female screw portion 9, so that the metal terminal 3 and the carbon terminal 4 can be easily removed and exchanged. Further, in the heat generating device 1, since the bottom portion 12 of the water passage reaches the male screw portion 8 of the metal terminal 3, the connecting portion 7 can be particularly efficiently cooled, so that the metal terminal 3 can be effectively suppressed. Breakage due to thermal expansion of the joint portion with the carbon terminal 4 described above. Further, in the heat generating device 1, the diameter of the carbon terminal 4 is 1 to 2 times that of the metal terminal 3 or the heat generating portion 5, and the effect of reducing the amount of heat generation can be obtained. Further, in the heat generating device 1, the heat generating device 1 By applying the tantalum carbide film to the carbon terminal 4 and/or the heat generating portion 5, the surfaces of the carbon terminal 4 and the heat generating portion 5 can be protected from corrosion. Further, in the above-described heat generating device 1, the tantalum carbide film is formed by a CVD method, and is a tantalum carbide film having a thickness of ΙΟμηη to 500 μm, so that water in a high-temperature air can be sufficiently suppressed. Corrosion of the carbon terminal 4 and the heat generating portion 5 does not contribute to cracking of the tantalum carbide film or cracking of the carbon terminal 4 and the heat generating portion 5. Further, in the heat generating device 1, the carbon-based graphite of the carbon terminal 4 and/or the heat generating portion 5 is obtained, so that the effect of improving heat resistance can be obtained. In addition, the reaction container 15 that supplies a gas containing tetrachlorosilane and hydrogen to generate a gas containing trichlorosilane hydrogen chloride, and the heat generating device 1 disposed to surround the reaction container 15 is surrounded by In the reaction tower 14 of the outer cylinder container 16 in which the reaction container 15 and the heat generating device 1 are disposed, since the metal terminal 3 has the water passage 6, the metal terminal 3 and the carbon terminal 4 can be efficiently cooled. The terminal portion can suppress breakage of the component due to thermal expansion. Although the heat generating device of the present invention has been described above, the present invention is not limited by this.实施 [Embodiment] [Embodiment 1] As shown in Fig. 3, a heat generating device using a metal terminal having a water passage is provided. As shown in Fig. 1, the heat generating device is a pair of two heat generating bodies composed of a metal terminal (diameter: 30 mm), a carbon terminal (diameter: 30 mm), and a heat generating portion (having a diameter of 20 mm). The diameter of the water passage is 50% of the diameter of the metal terminal. -14- 201034955 A screw connection means is provided in the joint portion of each member, and they are connected to each other. As shown in Fig. 4, the heat generating device was placed inside the reaction column, and after continuously operating for 2,000 hours, the device was disassembled and the terminal portion was damaged. As a result, the terminal portion was less damaged and could be operated for another 2,000 hours. [Embodiment 2] In the second embodiment, the carbon terminal and the heat generating portion are produced in the same manner as in the first embodiment except for the metal terminal that has reached the connection portion only by deepening the depth of the water passage as shown in Fig. 2 . The same heat generating device as in the first embodiment. Then, the same experiment as in the first embodiment was carried out, and the device was disassembled to examine the damage of the terminal portion. As a result, the terminal portion was less damaged, and the operation for another 2,000 hours was possible three times. [Example 3] In the third embodiment, the same as in the first embodiment, except that the diameter of the water passage was the same as that of the first embodiment, except that the metal terminal of the first embodiment was used. Heating device. Then, the same experiment as in the first embodiment was carried out. The device was disassembled and the damage of the terminal portion was examined. As a result, the terminal portion was less damaged, and the operation for another 2,000 hours was possible three times. [Embodiment 4] In the fourth embodiment, the heat generating device was produced using the metal sapphire and the heat generating portion of the second embodiment and a carbon terminal (diameter: 4 mm) having a diameter larger than the metal terminal. Then, the same experiment as in the first embodiment was carried out, and the device was disassembled and adjusted to -15-201034955. The damage of the terminal portion was observed. As a result, the damage of the terminal portion was small, and the operation for another 2,000 hours may be five times. [Comparative Example 1] A heat generating device similar to that of Example 1 was produced except that a metal terminal having no water passage was used. However, when the operation was performed, the heat generating device was broken at the time of not passing 2000 hours. Disintegration resulted in cracking in the vicinity of the joint between the carbon terminal and the metal terminal. <Review> From the above experimental results, it is understood that in the heat generating device of the embodiment of the present invention, the terminal portion is hardly damaged, and the durability is excellent. In particular, in the heat generating devices of Embodiments 2 to 4, it can withstand even a plurality of uses. As described above, with respect to the good results obtained by the heat generating device of the example, the damage of the screw portion in the comparative example was remarkable, and exchange was required in a short time. The above description is based on the embodiments to illustrate the invention. However, these embodiments are illustrative of the invention of the present invention, and those skilled in the art will understand that various other modifications are possible and that such modifications are also within the scope of the invention. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view showing a heat generating device according to an embodiment of the present invention. Fig. 2 is a schematic longitudinal cross-sectional view showing a terminal portion of a heat generating device according to an embodiment of the present invention. Fig. 3 is a schematic longitudinal sectional view showing a terminal portion of a heat generating device according to an embodiment of the present invention. Fig. 4 is a schematic view showing a tetrachlorodecane-16-201034955 reaction column using a heat generating device according to an embodiment of the present invention. [Main component symbol description]
1 發熱裝置 2 發熱體 3 金屬端子 4 碳端子 5 發熱部 6 通水路 7 連結部 8 陽螺紋部 9 陰螺紋部 10 流入口 11 排出口 12 通水路的底部 13 注入管 14 反應塔 15 反應容器 16 外筒容器 17 氣體導入口 18 反應生成氣體抽出口 -17-1 Heat generating device 2 Heating element 3 Metal terminal 4 Carbon terminal 5 Heat generating portion 6 Water passage 7 Connecting portion 8 Male screw portion 9 Female screw portion 10 Flow inlet 11 Discharge port 12 Flow path bottom 13 Injection pipe 14 Reaction column 15 Reaction vessel 16 Outer tube container 17 gas introduction port 18 reaction to generate gas extraction port -17-