200951251 六、發明說明： 【發明所屬之技術領域】 本發明是關於—種藉由切克勞斯基法（Czoehralski ^hod;以下稱為「CZ法」）來製造例如單㈣的提拉裝 置。 【先前技術】 近年，半導體積體電路元件的高集積化和伴隨著此高 ❿ 集積化之微細化的進展，非常顯著’而為了提高元件製造 的產率，強烈地要求晶圓口徑的大型化和高品質的石夕晶 圓。進而，對於有效率地製造晶圓、廉價地提供高品質晶 圓的技術，也受到關注。 通常，單晶石夕的製造，是藉由從石英㈣内㈣液， 一邊使單晶成長—邊提拉的^法來進行，而在該單晶製造 步称中，將惰性氣體供給至單晶提拉裝置内。χ，在單曰 製造中，會發切氧化物，該梦氧化物會附著在單晶㈣ 裝置的内壁上。當提拉小口徑結晶時，如第4圖所示，從 提拉腔室的上部的供給π 41(_處）供給惰性氣體。 但是，當結晶直徑變大的同時，所使用的氣體量也會 :多，只從-處供給氣體的情況，在爐内的氣體流速分布 :成為不均句’且在結晶成長中’用以提拉結晶的吊線會 發生振動。結果，需要精密地控制提拉速度，才能夠生產 的被稱為無缺时的高品f晶圓，會有生產性惡化的問題。 對於此種問題，在曰本特開昭6卜11199〇號公報中， 提出-種技術，其設置複數個氣體喷出口，對於提拉中的 200951251 單晶’往垂直於該轴的方向 J乃同，從後數個氣體噴出 地向爷線喷吹惰性氣體，來估貝® 冋時 使是此種技術，也會發生吊但是’即 振動而言，並不充分/吊線的振動，對於防止吊線發生 又，因為隨著結晶的大口徑 瓜化用以收容結晶之提拉 腔室的内徑也會變大，所以Λ 文人所以由於熱而發生的對流，碎氧化 物蒸氣進入提拉腔室内，且附著 117耆於杈拉腔室的壁面上的量 會變多。該氧化物，由於某此 ❹ 坩％呆些原因而落入爐内，則會妨礙 結晶成長而成為問題。 【發明内容】 因此’本發明是鑑於上述問題點而開發出來，其目的 在於提供-種單晶提拉裝置，以能防止吊線發生㈣且$ 少堆積在提拉腔室内壁上的矽氧化物的方式，提供惰性氣 體。 為了達成上述目的，本發明是一種單晶提拉裝置，至 ® 少、具有：容納掛禍之主腔室；以及被連接在該主腔室的上 部，用以收容被提拉而成長的單晶之提拉腔室；該單晶提 拉裝置的特徵在於： 至少，在上述提拉腔室内的上方，水平配置環狀的氣 體供給管，並在該氣體供給管上，等間隔地設置複數個氣 體喷出孔，該氣體喷出口，被形成於上述氣體供給管的從 垂直下方位置至外侧水平位置之間，氣體則從上述氣體噴 出孔直接喷在上述提拉腔室的内壁上。 4 200951251 如此，在裱狀的氣體供給管上，等間隔地設置複數個 氣體噴出孔，而使氣體從這些氣體噴出口喷出，藉此，即 使增大單晶提拉裝置内的氣體流4，氣體朝向提拉腔室的 下方均勻地流動，於是在提拉腔室内的氣體流速分布，相 _ 冑於提拉腔至的中心軸’成為軸對稱，能防止吊線振動。 又，氣體朝向提拉腔室的内壁噴出，由於氣體直接喷 在提拉腔室的内壁上之後，會沿著提拉腔室的内壁流動， 所以能減少附著在提拉腔室的内壁上的矽氧化物，並能防 ©止堆積的矽氧化物落下。如此，由於能一併防止吊線振動 以及矽氧化物堆積在提拉腔室的内壁上，所以結晶的培育 不會受到妨礙，而能有效率地製造出需要高精度地控制提 拉速度的高品質單晶矽。 此時上述氣體供給管的環的内徑dr，相對於上述提 拉腔室的内徑dP，較佳是〇.46dpSdrS〇.80dP。 如此，氣體供給管的環的内徑，若是在上述範圍從 *體噴出孔喷出的氣體，由於確實地喷在提拉腔室的内壁 上’並可容易地沿著内壁流動，所以能阻止矽氧化物附著 在提拉腔室的内壁上，並能大幅地降低矽氧化物的堆積 * ’又’氣體流速分布’相對於提拉腔室的中心軸容易 成為軸對稱’能防止吊線振動。 此時上述乳體喷出孔，較佳是被形成於上述氣體供 給管的從垂直下方位置，往外側的水平方向，1〇。$ 0 。的角度位置。 耽體噴出孔，若是在上述角度位置内，從氣體喷出孔 5 200951251 喷出的氣體，由於確實地喷在提拉腔室的内壁上，並可容 易地沿著内壁流動，所以能更確實地使提拉腔室内的流速 分布，相對於提拉腔室的中心轴，成為輛對稱，並能有效 地降低矽氧化物的堆積量。又，由於氣體沒有直接喷在吊 線上，所以可更確實地防止吊線振動。 又，上述氣體喷出孔的直徑，較佳是8 〇mm以下。 如此，若氣體喷出孔的直徑，是8.0mm以下，則氣體 被喷出時的流速變大，氣體可更確實地喷在提拉腔室的内 壁上，進而由於氣體沿著内壁流動至提拉腔室的下方，所 以對於整個提拉腔室的内壁，能減少矽氧化物的堆積。 又’較佳是在上述氣體供給管上，等間隔地設有6個 以上的上述氣體喷出孔。 如此，藉由在上述氣體供給管上，等間隔地設有6個 以上的上述氣體喷出孔，氣體沿著提拉腔室的内壁流動 時，是在内壁的幾乎整個面上流動，藉此，能大幅地減少 附著在提拉腔室的内壁上㈣氧化物，進而由於能使提拉 腔至内的氣體流逮分布更均勻化，所以也能防止吊線振動。 如以上所述，若是本發明的單晶提拉裝置，在環狀的 氣體供給管上，等間隔地設置複數個氣體喷出孔，而使氣 體從這些氣體喷出口直接喷在提拉腔室的内壁上，所以被 喷出的氣體，沿著提拉腔室的内壁流動。藉此，能減少進 入提拉腔室内的石夕氧化物的蒸氣，附著在提拉腔室的内壁 上而堆積的量’進而’由於氣體從環狀的氣體供給管等間 隔地被喷出’所以能使提拉腔室内的氣體流速分布，相對 200951251 於提拉腔室的令心轴， 成為軸對稱，而能防止窄線振動〇 【實施方式】 由於在提拉單晶砂# m ^ (iit it wt 產生的吊線振動、堆積在提拉 腔至（拉技腔室）内帶 & 的矽氧化物的落下等，會妨礙結晶 成長而成為間題。縣e.f a . ± ^ . 、疋，在需要高精密地控制提拉速度， 才此夠培用無缺陷結晶的 制變困難、生產性也會變低的問題。；日拉速度的控 因此’本發明人，發頊 現下的技術知識而完成本發明， 二氣體内的上方’水平配置環狀的氣體㈣ 直接等間隔地形成氣體喷出孔，能將氣體 == 室内壁上，藉此’由於被嘴出的氣體，沿 著k拉腔至内壁流動，能減少附著在内壁上的石夕氧化物， ::於能使提拉腔室内的氣體流速分布，相對於提拉腔室 的中心軸，作成轴對稱，所以也能防止吊線振動。 以'關於本發明的單晶提拉裝置，作為實施形態的 一例，一邊參照第卜2、3圖-邊更詳細地說明，但本發 明並未被限定於此實施形態。 第2ΓΛ是表示本發明的單晶提拉裝置的—例的概略圖。 能配置在本發明的單晶提拉裝置内的氣體供 :管的-例的概略圖。第3圖是用以說明本發明的氣艘喷 出孔所形成的角度的說明圖。 如第1圖所示，本發明的單晶提拉裝置 熔液的坩堝16、23,以及用以加熱、…、料 鮮原枓的加熱器18 200951251 等，被容納於主腔室12内；在已連接於主腔室12上的提 拉腔室11的上部，設有用以提拉培育後的單晶14之提拉 機構（未圖示 從已被安裝在提拉腔室U上部的提拉機構，提拉用吊 線20被退繞而往下，在其前端連接著用來安裝晶種2丨之 晶種夾頭22，並使已被安裝在晶種夾頭22上的晶種21浸 潰於原料熔液中，然後藉由提拉機構（未圖示）捲取提拉用 吊線2 0 ’藉此在晶種21的下方形成單晶14。 _ 另外，上述坩堝16、23，是由：内側的直接收容原料 熔液之石英坩堝16、及外側的用以支持該石英坩堝之石墨 坩堝23所構成。坩堝16、23,藉由已被安裝在單晶提拉 裝置的下部之旋轉驅動機構（未圖示），而被旋轉且升降自 如地支持於掛禍旋轉轴17上’為了使結晶直徑、結晶品質 等不會由於早aak拉裝置中的熔液面的變化而改變，並為 了將溶液面保持在固定位置，一邊使結晶往相反方向旋 轉，一邊對應單晶14的提拉而使坩堝16、23上升來彌補 〇 該減少量。 又，以包圍坩堝16、23的方式，配置加熱器18;在此 加熱器18的外側，為了防止從加熱器18發散的熱量直接 輻射在主腔至12上，以包圍加熱器18的方式，設置絕熱 構件19。 另外，主腔室12與提拉腔室u，是由不銹鋼等的耐熱 性、熱傳導性優異的金屬所形成，且通過冷卻管（未圖示） 而被水冷卻。· 200951251 並且，培育單晶14時，將已被安裝在晶種夾頭22上 的晶種21，浸潰於原料熔液中之後，一邊藉由提拉機構（未 圖示）使晶種21往所期望的方向旋轉，一邊慢慢地捲起吊 線20 ’而使單晶ι4成長於晶種2ι的前端部，但是為了消 除當使晶種21接觸原料熔液時所產生的錯位，先暫時使成 長初期的結晶，縮小直徑至3mm〜5mm左右為止，消除錯 位後’增大至所期望的直徑為止，而使目標品質的單晶14 成長或者’也可以應用無錯也種晶（disi〇cat.i〇n_free seeding) © 法’不進行上述縮徑’而使用前端尖銳的晶種21，將該晶 種21慢慢地接觸原料熔液，並往下浸潰至規定直徑為止， 然後進行提拉來培育單晶丨4。 又’以使發生在爐内的矽氧化物排出爐外為目的，從 提拉腔室11的上方導入氬氣等的惰性氣體，被導入的氣 體，穿過整流筒1 5内侧，而在提拉中的單晶丨4附近被整 流’然後通過原料熔液表面，且通過坩堝16、23的上端緣 的上方’而從氣體流出口 24被排出。 ® 在本發明的單晶提拉裝置的提拉腔室内的上方水平 配置環狀的氣體供給管13,用以導入上述氬氣等的惰性氣 體；複數個氣體噴出孔25,被形成於氣體供給管13的從 垂直下方位置至外側水平位置之間，於是氣體從氣體喷出 孔25被噴出而直接喷在提拉腔室n内壁上。另外，此時， 所明的被形成於氣體供給管13的從垂直下方位置至外侧 K平位置之間，疋如第3圖（b)所示，意指氣體噴出孔的中 心被形成於位在兩者之間。 9 200951251 利用從如此的氣體供給管喷出氣體，由於氣體在圓筒 ，狀的提拉腔室11内，以環狀且等間隔地被噴出，所以單晶 提拉裝置内的氣體流速分布成為均勻；又，由於以噴向提 拉腔室11内壁的方式噴出氣體，所以氣體沿著内壁流動， 能防止穿過提拉腔室的中心位置之韦線發生振動，進而能 減少矽氧化物附著在提拉腔室的内壁而堆積的量。 如第1圖與第2圖所示，作為氣體供給管13的環的内 徑dr，相對於提拉腔室u的内徑dp，較佳是〇.46dpSdr 鲁 S G.80dp。 若是如此範圍的氣體供給管13的環的内徑，能更確實 地將氣體直接喷在提拉腔室11的内壁上；又，氣體不會直 接喷在吊線上，進而’由於氣體容易沿著提拉腔室的内壁 流動’所以能更減少矽氧化物堆積在提拉腔室的内壁上的 量’並能防止矽氧化物落入爐内。進而，也不會干擾已被 提拉上來的單晶14。 又’此時的氣體喷出孔25’較佳是被形成於氣體供給 ❿ 管13的從垂直下方位置，往外側的水平方向，1 〇。$ 0 $ 60的角度位置；更佳是被形成於2〇°$0$ 30。的角度位 .置。只要在如此的角度範圍内形成氣體喷出孔25,則在氣 體直接喷在提拉腔室的内壁上之後，氣體容易沿著内避而 往下方流動，減少矽氧化物的堆積量，並能更有效地達成 單晶提拉裝置内的氣體流速分布的均勻化。 另外’此時的氣體喷出孔的角度β，如第3圖（a)所示， 是從氣體供給管的垂直下方位置向外側的傾斜角度，如第 10 200951251 3圖（b)所示’將從垂直下方位置至氣體噴出孔的中心位置 為止的傾斜，設為0。 又，氣體喷出孔25的直徑，較佳是8 0mra以下。 如此’氣體噴出孔的直徑，若是8· 0min以下，被喷出 氣體的流速會變大’而喷在提拉腔室的内壁上，由於可更 確實地沿著内壁而到達主腔室’並使提拉腔室内的氣體流 速相對於提拉腔室的中心軸成對稱，所以能更有效地達成 防止矽氧化物附著在提拉腔室的内壁上。 又，較佳是在氣體供給管13上’等間隔地設置6個以 上的氣體喷出孔25。 如此’若設置6個以上的氣體喷出孔，在整個提拉腔 至中’能更均勻地使氣體流動’進而，在全部的提拉腔室 的内壁，能減少矽氧化物的堆積量。 此時，根據要被製造出來的單晶矽，單晶提拉裝置的 尺寸也相異，所以配合其尺寸的要被喷出的氣體流量，可 作適當的選擇’而即使是供給多達300L/min的氣體的情 況’若是本發明的單晶提拉裝置，由於能藉由提拉腔室内 的均勻的氣體流速，來防止吊線振動，所以只要在堆積不 會發生於提拉腔室的内壁上的範圍，適當地選擇氣體流量 即可。 以下，表示實施例來更具體地說明本發明，但本發8月 並未被限定於這些例子。 (實施例1〜5、比較例1〜3) 11 200951251The present invention relates to a pulling device for manufacturing, for example, a single (four) by the Czochralski method (hereinafter referred to as "CZ method"). [Prior Art] In recent years, the high integration of semiconductor integrated circuit components and the progress of miniaturization of the high-order integrated circuits have been remarkable. In order to increase the yield of device manufacturing, the size of the wafer is strongly increased. And high quality Shixi wafers. Further, attention has been paid to a technique for efficiently manufacturing wafers and providing high-quality crystals at low cost. In general, the production of a single crystal stone is carried out by a method in which a single crystal is grown and lifted from a liquid in the quartz (four), and in the single crystal manufacturing step, an inert gas is supplied to the single Inside the crystal pulling device. χ, in the manufacture of a single ,, an oxide is formed, which is attached to the inner wall of the single crystal device. When the small-diameter crystal is lifted, as shown in Fig. 4, an inert gas is supplied from the supply π 41 (where) of the upper portion of the pulling chamber. However, when the crystal diameter becomes larger, the amount of gas used is also large: only when the gas is supplied from -, the gas flow velocity distribution in the furnace: becomes an uneven sentence 'and is grown in crystal growth' The lifting wire of the pulling crystal will vibrate. As a result, it is necessary to precisely control the pulling speed to produce a high-quality f wafer which is called a defect, and there is a problem that productivity is deteriorated. In order to solve such a problem, in the publication of Japanese Patent Application Laid-Open No. Hei. No. Hei. No. 11199 No., a technique is proposed in which a plurality of gas ejection ports are provided. For the pulling of the 200951251 single crystal in the direction perpendicular to the axis J In the same way, the inert gas is sprayed from the last few gas jets to the loyalty line to estimate the ® ® 使 使 使 此种 此种 此种 估 估 估 估 估 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊 吊The hanging wire occurs again, because the inner diameter of the pulling chamber for accommodating the crystallization with the large diameter of the crystal is also enlarged, so the convection due to heat, the broken oxide vapor enters the pulling chamber. And the amount of adhesion 117 to the wall of the chamber is increased. This oxide, which falls into the furnace due to some of the defects, causes the crystal to grow and becomes a problem. SUMMARY OF THE INVENTION Therefore, the present invention has been made in view of the above problems, and an object thereof is to provide a single crystal pulling device for preventing the occurrence of a hanging wire (4) and a small amount of cerium oxide deposited on the inner wall of the pulling chamber. The way to provide inert gas. In order to achieve the above object, the present invention is a single crystal pulling device, which has a small main chamber, and a main chamber that is connected to the main chamber, and is connected to the upper portion of the main chamber for accommodating a single bed that is pulled up. a crystal pulling device; the single crystal pulling device is characterized in that at least an annular gas supply pipe is disposed horizontally above the pulling chamber, and a plurality of gas supply pipes are disposed at equal intervals on the gas supply pipe The gas discharge port is formed between the vertically downward position and the outer horizontal position of the gas supply pipe, and the gas is directly sprayed from the gas discharge hole on the inner wall of the pulling chamber. 4 200951251 In this way, a plurality of gas ejection holes are provided at equal intervals on the gas supply tube, and gas is ejected from the gas ejection ports, thereby increasing the gas flow in the single crystal pulling device. The gas flows uniformly toward the lower side of the pulling chamber, so that the gas flow velocity distribution in the pulling chamber is axially symmetrical with respect to the central axis of the pulling chamber, and the suspension wire can be prevented from vibrating. Further, the gas is ejected toward the inner wall of the pulling chamber, and since the gas is directly sprayed on the inner wall of the pulling chamber, it flows along the inner wall of the pulling chamber, so that the inner wall of the pulling chamber can be reduced. Oxide oxide, and can prevent the antimony oxide from falling down. In this way, since the vibration of the suspension wire and the deposition of the cerium oxide on the inner wall of the pulling chamber can be prevented, the cultivation of the crystal is not hindered, and the high quality which requires high-precision control of the pulling speed can be efficiently produced. Single crystal germanium. The inner diameter dr of the ring of the gas supply pipe at this time is preferably 46.46 dpSdrS 〇 80 dP with respect to the inner diameter dP of the pulling chamber. As described above, the inner diameter of the ring of the gas supply pipe can be prevented by the fact that the gas ejected from the * body discharge hole in the above range is reliably sprayed on the inner wall of the pulling chamber and can easily flow along the inner wall. The niobium oxide adheres to the inner wall of the pulling chamber and can greatly reduce the accumulation of niobium oxide. * The 'gas flow rate distribution 'is easily axisymmetric with respect to the central axis of the pulling chamber' to prevent the suspension wire from vibrating. In this case, the above-mentioned emulsion discharge hole is preferably formed in a horizontal direction from the vertically downward position to the outer side of the gas supply pipe, 1 〇. $ 0. The angular position. In the above-mentioned angular position, the gas ejected from the gas ejection hole 5 200951251 is reliably sprayed on the inner wall of the pulling chamber and can easily flow along the inner wall, so that it can be more sure The ground flow velocity distribution in the chamber is symmetric with respect to the central axis of the pulling chamber, and the amount of cerium oxide deposited can be effectively reduced. Further, since the gas is not directly sprayed on the suspension wire, the suspension wire can be more reliably prevented from vibrating. Further, the diameter of the gas ejection hole is preferably 8 mm or less. As described above, when the diameter of the gas ejection hole is 8.0 mm or less, the flow velocity at which the gas is ejected becomes large, and the gas can be more reliably sprayed on the inner wall of the pulling chamber, and the gas flows along the inner wall to the lift. The lower part of the chamber is pulled, so that the accumulation of cerium oxide can be reduced for the inner wall of the entire pulling chamber. Further, it is preferable that six or more gas discharge holes are provided at equal intervals in the gas supply pipe. As described above, by providing six or more gas discharge holes at equal intervals in the gas supply pipe, when the gas flows along the inner wall of the pulling chamber, the gas flows on almost the entire surface of the inner wall. It can greatly reduce the (4) oxide attached to the inner wall of the pulling chamber, and further can prevent the suspension wire from vibrating because the gas flow distribution of the pulling chamber can be more uniform. As described above, in the single crystal pulling apparatus of the present invention, a plurality of gas ejection holes are provided at equal intervals on the annular gas supply tube, and gas is directly sprayed from the gas ejection ports in the pulling chamber. On the inner wall, the gas that is ejected flows along the inner wall of the pulling chamber. Thereby, it is possible to reduce the amount of vapor that has entered the inner wall of the pulling chamber and adhere to the inner wall of the pulling chamber, and further the gas is ejected from the annular gas supply pipe at equal intervals. Therefore, the gas flow velocity distribution in the chamber can be made to be axisymmetric with respect to the mandrel of the pulling chamber in 200951251, and the narrow line vibration can be prevented. [Embodiment] Due to the pulling of the single crystal sand #m ^ ( The vibration of the suspension wire produced by iit it wt, the falling of the cerium oxide deposited in the pulling chamber to the (drawing chamber), etc., will hinder the growth of the crystal and become a problem. County ef a . ± ^ . In order to control the pulling speed with high precision, it is difficult to cultivate the defect-free crystal, and the productivity is also low. The control of the Japanese pull speed is therefore the inventor's current technology. With the knowledge of the present invention, the upper 'horizontal arrangement of the annular gas (4) in the two gases directly forms a gas ejection hole at equal intervals, and the gas can be placed on the indoor wall, thereby 'because of the gas discharged from the mouth, along the k pull cavity to the inner wall, can reduce The Shishi oxide attached to the inner wall, :: can make the gas flow velocity distribution in the pulling chamber, and is axisymmetric with respect to the central axis of the pulling chamber, so that the suspension wire can also be prevented from vibrating. The single crystal pulling device will be described in more detail with reference to FIGS. 2 and 3 as an example of the embodiment. However, the present invention is not limited to the embodiment. The second embodiment shows the single crystal of the present invention. A schematic view of an example of a pulling device. A schematic view of an example of a gas supply pipe that can be disposed in the single crystal pulling device of the present invention. Fig. 3 is a view for explaining the formation of the gas boat ejection hole of the present invention. An illustration of the angle. As shown in Fig. 1, the crucibles 16, 23 of the single crystal pulling device of the present invention, and the heater 18 200951251 for heating, ..., are accommodated in In the main chamber 12; on the upper portion of the pulling chamber 11 connected to the main chamber 12, a pulling mechanism for pulling up the cultivated single crystal 14 is provided (not shown from the installation has been carried out in the pulling a pulling mechanism at the upper portion of the chamber U, the lifting wire 20 is unwound and downward, at the front end thereof Next, the seed crystal chuck 22 of the seed crystal 2 is mounted, and the seed crystal 21 which has been mounted on the seed crystal chuck 22 is immersed in the raw material melt, and then pulled by a pulling mechanism (not shown). The winding wire 2 0' is taken up to form the single crystal 14 below the seed crystal 21. In addition, the above-mentioned crucibles 16, 23 are: the quartz crucible 16 which directly accommodates the raw material melt on the inner side, and the outer side. The graphite crucible 23 is supported by the quartz crucible. The crucibles 16, 23 are rotated and lifted and supported by a rotary drive mechanism (not shown) that has been attached to the lower portion of the single crystal pulling device. In order to prevent the crystal diameter, crystal quality, etc. from changing due to the change of the melt surface in the early aak drawing device, the crystal shaft diameter and the crystal quality are changed, and the crystal is rotated in the opposite direction while maintaining the solution surface at a fixed position. Corresponding to the pulling of the single crystal 14, the crucibles 16, 23 are raised to compensate for the reduction. Further, the heater 18 is disposed so as to surround the crucibles 16, 23; on the outside of the heater 18, in order to prevent the heat radiated from the heater 18 from being directly radiated on the main chamber 12 to surround the heater 18, A heat insulating member 19 is provided. Further, the main chamber 12 and the pulling chamber u are made of a metal excellent in heat resistance and thermal conductivity such as stainless steel, and are cooled by water by a cooling pipe (not shown). - 200951251 Further, when the single crystal 14 is grown, the seed crystal 21 that has been mounted on the seed chuck 22 is immersed in the raw material melt, and then the seed crystal 21 is pulled by a pulling mechanism (not shown). Rotating in the desired direction, while slowly winding up the hanging wire 20', the single crystal ι4 is grown at the tip end portion of the seed crystal 2i, but in order to eliminate the misalignment caused when the seed crystal 21 is brought into contact with the raw material melt, The crystals in the initial stage of growth are reduced to a diameter of about 3 mm to 5 mm, and after the dislocation is removed, the diameter of the single crystal 14 of the target quality is increased or the crystal can be applied without any error (disi〇). Cat.i〇n_free seeding) © Method 'Without the above-mentioned reduction diameter', using the sharp-edged seed crystal 21, the seed crystal 21 is slowly brought into contact with the raw material melt, and then immersed down to a predetermined diameter, and then Lifting to cultivate single crystal crucible 4. Further, for the purpose of discharging the niobium oxide generated in the furnace outside the furnace, an inert gas such as argon gas is introduced from above the pulling chamber 11, and the introduced gas passes through the inside of the rectifying cylinder 15 and is pulled. The vicinity of the single crystal crucible 4 is rectified 'and then passes through the surface of the raw material melt, and is discharged from the gas outflow port 24 through the upper side of the upper end edge of the crucibles 16, 23. The annular gas supply pipe 13 is horizontally disposed above the lifting chamber of the single crystal pulling apparatus of the present invention for introducing an inert gas such as argon gas or the like; a plurality of gas ejection holes 25 are formed in the gas supply The tube 13 is displaced from the vertically downward position to the outer horizontal position, so that the gas is ejected from the gas ejection hole 25 and directly sprayed on the inner wall of the pulling chamber n. Further, at this time, it is understood that the position of the gas supply pipe 13 from the vertically downward position to the outer K flat position, as shown in Fig. 3(b), means that the center of the gas discharge hole is formed in position. Between the two. 9 200951251 The gas is sprayed from such a gas supply pipe, and since the gas is ejected in a ring shape at equal intervals in the cylindrical pulling chamber 11, the gas flow velocity distribution in the single crystal pulling device becomes Further, since the gas is ejected in a manner of being sprayed toward the inner wall of the pulling chamber 11, the gas flows along the inner wall, preventing the vibration of the wavy line passing through the center position of the pulling chamber, thereby reducing the adhesion of cerium oxide. The amount deposited on the inner wall of the pulling chamber. As shown in Figs. 1 and 2, the inner diameter dr of the ring as the gas supply pipe 13 is preferably 〇.46dpSdr 鲁 S G.80dp with respect to the inner diameter dp of the pulling chamber u. If the inner diameter of the ring of the gas supply pipe 13 is in such a range, the gas can be more directly sprayed on the inner wall of the pulling chamber 11; in addition, the gas is not directly sprayed on the hanging wire, and thus the gas is easily along The inner wall of the pulling chamber flows 'so that the amount of niobium oxide accumulated on the inner wall of the pulling chamber can be further reduced' and the niobium oxide can be prevented from falling into the furnace. Further, it does not interfere with the single crystal 14 that has been pulled up. Further, the gas discharge hole 25' at this time is preferably formed in the horizontal direction of the gas supply manifold 13 from the vertically lower position to the outer side, 1 〇. An angular position of $0 $60; more preferably formed at 2〇°$0$30. The angle of the position. When the gas ejection hole 25 is formed in such an angular range, after the gas is directly sprayed on the inner wall of the pulling chamber, the gas easily flows downward along the inner side to reduce the amount of cerium oxide deposited, and The homogenization of the gas flow rate distribution in the single crystal pulling device is more effectively achieved. Further, the angle β of the gas ejection hole at this time is an inclination angle from the vertically lower position of the gas supply pipe to the outside as shown in Fig. 3(a), as shown in Fig. 10 200951251 3 (b). The inclination from the vertically downward position to the center position of the gas ejection hole is set to zero. Further, the diameter of the gas ejection hole 25 is preferably 80 m or less. If the diameter of the gas ejection hole is less than 8.0 min, the flow rate of the gas to be ejected becomes larger, and it is sprayed on the inner wall of the pulling chamber, so that it can reach the main chamber more surely along the inner wall. The gas flow rate in the pulling chamber is symmetrical with respect to the central axis of the pulling chamber, so that it is possible to more effectively prevent the niobium oxide from adhering to the inner wall of the pulling chamber. Further, it is preferable that six or more gas ejection holes 25 are provided at equal intervals on the gas supply pipe 13. Thus, if six or more gas ejection holes are provided, the gas can be more uniformly flowed throughout the pulling chamber to the middle, and the amount of cerium oxide deposited can be reduced on the inner walls of all the pulling chambers. At this time, depending on the single crystal germanium to be manufactured, the size of the single crystal pulling device is also different, so the flow rate of the gas to be ejected in accordance with the size thereof can be appropriately selected' even if it is supplied up to 300L. In the case of the gas of /min, the single crystal pulling device of the present invention can prevent the suspension wire from vibrating by the uniform gas flow rate in the pulling chamber, so that the accumulation does not occur on the inner wall of the pulling chamber. In the above range, the gas flow rate can be appropriately selected. Hereinafter, the present invention will be described more specifically by way of examples, but the present invention is not limited to these examples. (Examples 1 to 5, Comparative Examples 1 to 3) 11 200951251
首先，為了提拉直徑2〇〇mm的結晶，將提拉腔室的内 徑設為500mm。製作7個環狀氣體供給管，其環的内徑針 是400丽（0.80dp)’並以等間隔的方式形成6個直徑7 5咖 的氣體喷出孔，僅該氣體喷出孔的角度（參照第3圖）分別 相異。各自的氣體喷出孔的角度0，表示於们中。並且， 邊從运些氣體供給管，以25〇L/min的流量，使氯氣在提 拉腔室内流動’-邊分別進行無缺陷單晶料提拉。又， 作為比_ 3，—邊從第4騎示的f知的單晶提拉裝置 =-個氣體供給π ’以25GL/min的流量，使氬氣在提拉腔 ^内流動’―邊以㈣的條件進行無缺陷單晶料提拉。 將每些例子的結果表示於表1中。 [表11First, in order to lift crystals having a diameter of 2 mm, the inner diameter of the pulling chamber was set to 500 mm. Seven annular gas supply pipes were produced, the inner diameter needle of the ring was 400 liters (0.80 dp)', and six gas ejection holes having a diameter of 75 coffee were formed at equal intervals, only the angle of the gas ejection hole (Refer to Figure 3) The differences are different. The angle 0 of the respective gas ejection holes is shown in them. Further, while the gas supply pipes were transported, the chlorine gas was flowed in the pulling chamber at a flow rate of 25 〇L/min, and the defect-free single crystal material was pulled. Further, as a ratio of _3, the single crystal pulling device known from the fourth riding device is supplied with π' at a flow rate of 25 GL/min, and argon gas flows in the pulling chamber. Lifting the defect-free single crystal material under the conditions of (4). The results of each of the examples are shown in Table 1. [Table 11
如表 所示 在其氣體喷出孔位於 環的中心方向（(9 12 200951251 = -5° )的比較例1中，氣體直接喷在吊線上而發生吊線振 動’進而妙氧化物堆積而落下，顯著地降低結晶的生產性。 在比較例2中’雖然沒有發生吊線振動，但有氧化物落下； 在比較例3中’吊線振動與矽氧化物的落下，兩者都有發 生’顯著地降低結晶的生產性。 另一方面’實施例1〜5，沒有發生吊線振動，也沒有 發生發氧化物的落下’可效率佳且價廉地製造出沒有結晶 紊亂的高品質單晶矽。 ® 關於實施例卜2、4、5，雖然有發生矽氧化物的堆積， 但沒有發生堆積物的落下。在此，相較於實施例1、5( 0 =5。、 65 )’實施例2、4( 0 =15。、35。）的情況，矽氧化物的堆積 量降低’進而，在實施例3(0 =25。）中，以目視幾乎沒有 發現妙氧化物的堆積。 根據此結果，作為喷出孔的角度0，得知：較佳是被 形成10 60。的角度位置，更佳是被形成於2〇。$0 ^ 30°的角度位置。 (實施例6〜8) 首先’為了提拉直徑200mm的結晶’將提拉腔室的内 徑設為500咖。製作3個環狀氣體供給管，其以等間隔的 方式形成有6個直徑7. 5mm的氣體喷出孔’且該氣體嘴出 孔的角度0為25 ，而僅各自改變内徑dr。將各個氣體供 給管的内徑dr，表示於表2中。並且，一邊從這些氣體供 給管，以250L/min的流量，使氬氣在提拉腔室内流動，一 13 200951251 ===:=將這些…結果與賁 [表2]As shown in the table, in the comparative example 1 in which the gas ejection hole is located in the center direction of the ring ((9 12 200951251 = -5°), the gas is directly sprayed on the suspension wire, and the suspension wire vibrates, and the oxide is deposited and falls. The productivity of crystallization was remarkably lowered. In Comparative Example 2, although the suspension vibration did not occur, oxides fell; in Comparative Example 3, 'the suspension vibration and the cerium oxide fall, both occur 'significantly lower On the other hand, in Examples 1 to 5, no suspension vibration occurred and no oxide falling occurred, and high-quality single crystal germanium without crystal turbulence was efficiently and inexpensively produced. In the examples 2, 4, and 5, although the deposition of cerium oxide occurred, the deposition of the deposit did not occur. Here, in comparison with Examples 1, 5 (0 = 5, 65) 'Example 2 In the case of 4 (0 = 15 and 35), the deposition amount of cerium oxide was lowered. Further, in Example 3 (0 = 25), almost no accumulation of a wonderful oxide was observed by visual observation. As the angle 0 of the ejection hole, it is known that: It is formed at an angular position of 10 60. More preferably, it is formed at an angular position of 2 〇. $0 ^ 30°. (Examples 6 to 8) First, 'for the purpose of pulling a crystal of 200 mm in diameter, the inside of the chamber will be lifted. The diameter is set to 500. Three annular gas supply pipes are formed, and six gas discharge holes having a diameter of 7.5 mm are formed at equal intervals, and the angle 0 of the gas nozzle outlet holes is 25, and only The inner diameter dr is changed. The inner diameter dr of each gas supply pipe is shown in Table 2. And, from these gas supply pipes, argon gas flows in the pulling chamber at a flow rate of 250 L/min, a 13 200951251 ===:= put these... results with 贲 [Table 2]
在實施例6中，内徑dr小，氣體被噴出時的流速變大， 氣體喷在提拉腔室的内壁上之後，氣體會輕微地喷在吊線 上，而雖然只有輕微地喷在吊線上，也會發生吊線振動， 且雖然情沉輕微，但結晶的生產性降低。在實施例6、8中， 雖然都有矽氧化物的堆積’但沒有發生落下。實施例7、3， ® 沒有發生吊線振動，也幾乎沒有發現矽氧化物的堆積，可 效率佳且價廉地製造出沒有結晶紊亂的高品質單晶石夕。 根據此結果’作為氣體供給管的環的内徑dr，得知： 相對於提拉腔室的内徑dp’較佳是〇. 46dpS drS 0. 80dp » 另外，本發明並未被限定於上述實施形態。上述實施 形態只是例示’只要是具有與被記載於本發明的申請專利 範圍中的技術思想實質上相同的構成，能得到同樣的作用 200951251 效果者，不論為何者 皆被包含在本發明的技術範圍内。 【圖式簡單說明】 第1圖是表示本發明的單晶提拉裝置的一 W的概略闘 第2圖是表示能使用於本發明的單晶提拉裝置中。 體供給管的一例的概略圖。 的氣In the embodiment 6, the inner diameter dr is small, the flow velocity when the gas is ejected becomes large, and after the gas is sprayed on the inner wall of the pulling chamber, the gas is slightly sprayed on the hanging wire, and although it is only slightly sprayed on the hanging wire Suspension vibration also occurs, and although the severity is slight, the productivity of crystallization is lowered. In Examples 6 and 8, although there was a buildup of niobium oxide, no drop occurred. In Examples 7, 3, and ®, the suspension wire vibration did not occur, and the deposition of cerium oxide was hardly observed, and high-quality single crystal stone without crystal turbulence was efficiently and inexpensively produced. According to the result 'as the inner diameter dr of the ring of the gas supply pipe, it is known that the inner diameter dp' with respect to the pulling chamber is preferably 〇. 46dpS drS 0. 80dp » In addition, the present invention is not limited to the above Implementation form. The above-described embodiment is merely exemplified as long as it has substantially the same configuration as the technical idea described in the scope of the patent application of the present invention, and the effect of the same effect 200951251 can be obtained, regardless of why it is included in the technical scope of the present invention. Inside. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view showing a single crystal pulling device of the present invention. Fig. 2 is a view showing a single crystal pulling device which can be used in the present invention. A schematic view of an example of a body supply pipe. Gas
的噴出孔的說 明的單晶提拉 第3圖是用以說明本發明的氣體供給管 明圖；（a)、（b)是部分地表示能使用於本發 裝置中的氣體供給管的概略圖。 第4圖是表示習知的單晶提拉裝置的—例的概略圖FIG. 3 is a view for explaining the gas supply pipe of the present invention; (a) and (b) partially show the outline of the gas supply pipe that can be used in the present invention. Figure. Fig. 4 is a schematic view showing an example of a conventional single crystal pulling device.
【主要元件符號說明】 11提拉腔室 13氣體供給管 15整流筒 17坩堝旋轉軸 19絕熱構件 21晶種 23石墨坩堝 25氣體噴出孔 12主腔室 14單晶 16石英坩堝 18加熱器 20吊線 2 2晶種夾頭 24氣體流出口 15[Main component symbol description] 11 pulling chamber 13 gas supply pipe 15 rectifying cylinder 17 rotating shaft 19 insulating member 21 seed crystal 23 graphite crucible 25 gas ejection hole 12 main chamber 14 single crystal 16 quartz crucible 18 heater 20 hanging wire 2 2 seed chuck 24 gas outflow port 15