經濟部中央標準局負工消費合作社印装 4389 1 2 五、發明説明（·！） '—- 發明背景 本次發明-般而言是有關於單晶矽的製作，更確切地 說，疋與利用丘克拉斯基法（CzQehralski)，在單晶珍晶塊 成長時用來支承氧化矽坩堝之新型石墨基座相關。本發明 也與使用新型基座來製備單晶矽有關。 " 大部份用於微電子電路製作上之單晶珍是以丘克拉斯基 (C^hraUki)製程法來製備。在此製程中，單晶矽晶塊 是藉著將多晶結構之矽原料在坩堝中熔解後，摻入—晶種 至；it融石夕中，接著拉出晶種來起始單晶的成長’以得到單 晶石夕晶塊。典型上，多晶形矽是在玻璃狀氧化石夕掛瑪或是 其他以氧化矽套襯的坩堝中熔化。玻璃狀氧化矽一般是指 石英坩堝或熔凝的石英坩堝。氧化矽同時也以多種不同的 晶型存在，其中包括^與点型石英、鱗石英〇ridymite)、和 白石夕石（cristobalite)。 然而，熔化多晶形矽所需之氧化矽容器在高溫下的表現 存在著一些問題。舉例來說，隨著溫度升高，玻璃狀氧化 矽的黏度會變得較小，然後在溫度超過丨815 κ時會軟到受 到應力即變形。因此，氧化矽容器對於整體結構一致性的 損失（包括弛垂（sagging)和/或其他在單晶矽製作過程中的 變形）很敏感。所以，諸如基座或坩堝此等石墨製支承容器 通¥是被用來支持氧化矽坩堝、套襯 '或是其他多晶形矽 質熔於其中的容器。石墨製支承容器和/或氧化矽容器表面 的接觸部份可加上鍍層，例如Sic、Tic、NbC、TaC或 ZrC(JP 7089789A) ’或是玻璃狀的碳層（美國專利案號 -4 - 本紙張尺度通用令國國家標準（CNS ) Α4祕（2ΐ〇Χ297公着） 、1τ------線 • - (請先閲讀背面之注意事項再填寫本頁j 4389 1 2 五、發明説明（2 ) M7M79授予Lewis等人再者，氧切的内層和/或外層 表面也可包含-層均勻之氧切多晶層（美國專利案號 4,429,009授予Pastor等人；美國專利案號5 〇53 359授予Printed by the Central Bureau of Standards, Ministry of Economic Affairs, Consumer Cooperatives, 4389 1 2 V. Description of the Invention (·!) '--- Background of the Invention This invention-in general, is about the production of monocrystalline silicon. The CzQehralski method is used to support the new graphite base used to support the silicon oxide crucible when the single crystal ingot grows. The invention is also related to the use of novel pedestals to produce single crystal silicon. " Most of the single crystals used in the manufacture of microelectronic circuits are prepared by the C ^ hraUki process. In this process, the single crystal silicon ingot is formed by melting the polycrystalline silicon raw material in the crucible and injecting-seed crystals; it melts the stone and then pulls out the seed crystals to start the single crystal. Grow 'to get monolithic ingots. Typically, polycrystalline silicon is melted in glass-like oxidized silica or other crucibles lined with silica. Glassy silica generally refers to a quartz crucible or a fused quartz crucible. At the same time, silicon oxide also exists in many different crystal forms, including ^ and point type quartz, scaly quartz (olidymite), and cristobalite. However, there are some problems with the performance of silicon oxide vessels required for melting polycrystalline silicon at high temperatures. For example, as the temperature increases, the viscosity of glassy silica will become smaller, and then it will be soft and deformed when it is stressed above 815 κ. As a result, silicon oxide vessels are sensitive to loss of overall structural consistency, including sagging and / or other deformations during monocrystalline silicon fabrication. Therefore, graphite support containers such as pedestals or crucibles are generally used to support silica crucibles, liners, or other polycrystalline silicon containers. The contact parts of the surface of the graphite support container and / or the silicon oxide container may be plated, such as Sic, Tic, NbC, TaC, or ZrC (JP 7089789A) 'or a glass-like carbon layer (US Patent No. 4- The standard of this paper is the national standard (CNS) Α4 secret (2ΐ〇 × 297), 1τ ------ line •-(Please read the precautions on the back before filling out this page j 4389 1 2 V. Invention Note (2) M7M79 is awarded to Lewis et al. Furthermore, the inner and / or outer surface of the oxygen cut may also include a uniform oxygen cut polycrystalline layer (US Patent No. 4,429,009 to Pastor et al .; US Patent No. 5). 53 359 grant
Lesley等人），或是鍍上去玻璃化促進劑，以在原處形成一 均勻之去玻璃化層（EP 0753 605A)。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本買) 另-個與氧化矽容器高溫下的表現有關的問題是玻璃狀 氧切局部變化成乡晶形式（如白砂石）m的是非 均勻的去玻璃化作用。在氧切容器内層表面所形成各自 孤立的白石夕石小晶粒會被釋放至氧切溶液，然後融入成 長中的晶冑’因而在其中產生—些缺陷。大量非均勻的白 矽石相的成長也會致使氧化矽容器損失其結構的一致性， 這包括有彎曲（flexing)、脹凸（bulging)、以及在氧化矽容器 外形上的扭曲和變形。氧化矽的非均勻去玻璃化據說會受 到其純度以及其表面受污染的程度的影響，因為表面污染 會促使晶形氧化矽（如白矽石）的孕核，並且會如助融劑 (flux)般地作用，使晶形氧化矽變態成其他形式（如自白矽 石變為鱗石英），熔凝石英製品，通用電氣公司—般性型錄 7700，第17至18頁，（1月號，1987)。因此，將非均勻玻璃 化程度降至最小的方法，包括了増加純度和此氧化矽容器 表面的清潔度。舉例來說，曰本尺吐以第52/〇38873號就揭露 了利用氙氣燈來照射坩堝内部表層，以移除因靜電吸附在 氧化矽表面的金屬污染物。日本K〇ka^6〇/1378 利用電解法㈣金屬自氧切表面移除。 雖然已有前述的一些方法’非均勻玻璃化以及對氧化矽 -5- 本紙張尺度_ t ( CNS ) Α4ίί5Τ7ι〇χ297^ } A7 B7 > 43891 2 五、發明説明（ =結=性與零缺陷晶體成長的不利影響卻依舊是個 二非均勻去玻璃化作用的速率會隨著溫度 Π容：來裝填較多的多晶形觸，使得單晶碎晶塊： 產的工業化轉移變得更加地嚴重。在這些應用之中，所需 ===!提高相當量非均勻破璃化的可能性，這會 化夕^變形’並且最後降低了單以晶塊零 的成長。 登..明之概括鈷怵 /斤以這個發明的目的是製備品質更佳的單晶彳，特別地 =以較大量的料量來製備單_，料同㈣低氧切 4中局邵、非均勾去玻璃化作用的程度，也因此改善了 此容器結構的整體性，並且提升了其中零缺陷單晶妙成長 的程度。而以有效率節省成本的方式，對現今的商業製程 作最小的衝擊’使得單晶發同樣達到如此改良的品質也是 本發明的目的。 因此簡言之，本發明是針針由多晶形石夕質產生單晶發晶 塊=個製程。根據此製程，多晶料被裝填入一個氧化 矽谷态。此容器可以是已經處理過或未經處理過的氧化 矽此备器是由設计用來接受氧化矽容器的石墨支承容 器，以-種像是置身於巢狀石要支承容器的方式來支撐。 而此容器的外層表面至少有—部份是與支承容器的外層接 觸。這個接觸的區域即定義出了一個界面區。石墨支承容 器更進一步地是設計來使用於丘克拉斯基（cz〇chralski) -6- 本紙張尺度適用中國國家標準（CNS ) A4说格 參------1T------^ (讀先聞讀背面之注意事項再填寫本I) 經濟部中央標準局員工消費合作社印製 (210x297公釐 A3B9 1 2 A7 Β7 Μ 濟 部 中 央 榡 準 局 員 工 消 '費 合 作 社 印 製 五、發明説明（4 型抽扛器，並且可以是如已處理或未處理過石墨基座這般 的石墨支承容器。 根據此製程的一個實施例，因在石墨支承容器中存在的 鈣元素濃度相當地低，以致於在接續的步驟中可防止在氧 化矽容器界面區上大量的非均勻的去玻璃化作用。而在較 佳的一種製程中，石墨支承容器内鈣的重量濃度不會超過 約1 PPM。以其優越性漸增順序來排列，石墨支承容器内鈣 的重量濃度不超過約0.7 PPM、不超過約〇·2 ppM、以及不 超過約0.1 PPM。 根據此製程的另一個實施例，石墨製支承容器中之鹼金 族及鹼土金族元素所累積的量其重量濃度不會超過丨ppM。 而在在石墨支承容器中’挑選由鈣、鎂、鳃、鋰、鈉以及 鉀組成的群組所累積的重量濃度，最好是不超過7 PPM。 而此製程實施例的石墨支承容器中，鈣的重量濃度則是最 好不要超過0.2 PPM。 在前述任何一個實施例中’支承容器、容器、以及多晶 形碎原料均被加熱以熔化多晶形矽並且形成矽熔融液。而 此石墨支承容器在其支承容器邊緣部份内侧與氧化矽容 器外側接觸部份，可被加熱到均至少15 5 〇 (1 5 7 5 °C則更佳） 且持續至約2小時（4小時則更佳）。單晶矽晶塊即是由此熔 融5夕中抽拉而出。 本發明同時也針當自氧化矽容器中的矽熔液在產生單晶 砂晶塊之時，對如同鳥巢般支撐容器之石墨製支承容器， 像是基座或坩堝。此支承容器包括了 一個本質上由石墨組 本紙張尺度ϋ财㈣家料（CNS) A4規格（2Η)Χ297公瘦- --------ά------IT------0 * 1 (請先閱讀背面之注意事項再填寫本頁) r. ί 4 3 B 9 1 2 A7 ___B7 五、發明説明（5 ) 成的本體。 重要地是，根據其中一個石墨支承容器的實施例，石黑 本體之中所含之鈣重量濃度不超過i PPM。若以其優越性^ 增來排列’石墨本體内鈣的濃度重量為不超過約0.7 ppM、 不超過約0.2 PPM、以及不超過約0.1 PPM。 根據另一個石墨支承容器的實施例，石墨本體中之驗金 族及鹼土金族元素所累積的量其重量濃度不超過1 ppM ^而 在石墨本體之中，由鈣、鎂、鳃 '鋰、鈉以及鉀組成的群 組所累積的重量濃度最好是不超過0,7 PPM。而更佳的情沉 是，石墨本體中鈣的重量濃度最好不要超過0.2 ppm。 對於前述兩石墨支承容器，其中任一之石墨本體均具有 一由内側表面定義出之開放體腔，其形狀是設計來當從氧 化矽容器中的矽熔液產生單晶矽晶塊時，如鳥巢般承接該 谷器’而石墨支承容器的邊緣内側至少有一部份與氧化矽 容器的外側部份接觸。此石墨本體是設計適合用於丘克拉 斯基（Czochralski)型的晶體抽拉器。此本體基本上可全 由石墨或是由至少覆蓋本體内層表面的一層鏟層所取代。 本發明其他的特點及目的有部份是對熟悉該項技藝者很 淺顯，而部份將於後示出。 經濟部t央樣準局貝工消費合作枉印製 1_式之簡蕈說明 圖1為一空的丘克拉斯基（Czochralski)坩堝之剖面圖。 圖2為—適於承接圖1中坩堝之空的石墨基座。 圖3為一丘克拉斯基（Cz〇chralski)型晶體抽拉器，其中 包括圖I中坩堝的剖面圖置於並且由圖2之基座支承*此裝 -8- 本紙張尺度ϋ財關家縣（CNS )从胁（21()>< 297公楚） A7 rV 4389 1 2 ___ B7_ 五、發明説明（6 ) 置主要用於批次的製程上a 圖4為一丘克拉斯基（C ζ 〇 c h r a丨s k i)型晶體抽拉器，其中 包括内層坩堝的剖面圖，以及置於並且由石墨基座支承之 外層坩堝，此裝置主要用於連續的製程上。 圖5為一顯示製作石墨支承容器之示意流程圖。 圖6為一圖示，使用由辦濃度範圍在0.1 PPM到0.2 PPM或 0.8 PPM到1.7 PPM之石墨基座支承的氧化矽堝，在多次不 同次數的頸縮測試下，是否可得到零差排之單晶妙成長。 ^------ΐτ-------^ (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印裝 元件符號.說明 1 0氧化矽坩堝 3 0石墨基座 1 0'内層坩堝 30·基座 1 0 ”外層坩堝 3 2内表面 1 2内表層 3 4外表層 1 4外表層 3 5中央線 1 5中央線 3 6頂緣 1 6頂緣 3 7底層部份 1 7底層 38角落區 1 8角落區 3 9側壁區 i 9側壁區 3 9 a頂層部份 1 9 a頂層部份 3 9 b中層部份 1 9 b中層部份 .3 9 c底層部份 1 9 c底層部份 4 4開放體腔 2 4開放體腔 46基底 -9- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X29?公釐） A38912 A7 B7 五、發明説明（7 4 8熔融態矽 50丘克拉斯基（Czochralski)型晶體抽拉器 52底座 58熔液液面 5 4加熱器 本發明將於下面參考圖例作進一步地描述，其中類似的項 目將於幾個圖中標上相同的號碼。 螢明詳細說明 經濟部中央標準局員工消費合作·杜印製 (請先閲讀背面之注意事項再填寫本頁)Lesley et al.), Or plating a devitrification accelerator to form a uniform devitrification layer in situ (EP 0753 605A). Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling in this purchase). Another problem related to the performance of the silicon oxide container at high temperature is that the glassy oxygen cut locally changes to the native crystal form (such as White sandstone) m is non-uniform devitrification. The small isolated chert stones formed on the inner surface of the oxygen-cutting container will be released into the oxygen-cutting solution, and then merged into the growing crystals, thereby causing some defects. The growth of a large number of non-uniform white silica phases will also cause the silicon oxide container to lose its structural consistency, which includes flexing, bulging, and distortion and deformation in the shape of the silicon oxide container. The non-uniform devitrification of silicon oxide is said to be affected by its purity and the degree of contamination of its surface, as surface contamination promotes the nucleation of crystalline silicon oxide (such as white silica) and can act as a flux Normal action, transforming crystalline silicon oxide into other forms (such as from silica to scaly quartz), fused quartz products, General Electric Company-General Catalog 7700, pages 17-18, (January issue, 1987 ). Therefore, methods to minimize non-uniform vitrification include increasing purity and cleanliness of the surface of the silica container. For example, the Japanese ruler No. 52 / 〇38873 disclosed that a xenon lamp was used to illuminate the inner surface of the crucible to remove metal contaminants adsorbed on the surface of silicon oxide due to static electricity. Japan K〇ka ^ 6〇 / 1378 metal is removed from the oxygen cut surface by electrolytic method. Although some of the aforementioned methods have been used for non-uniform vitrification and silicon oxide, the paper size _ t (CNS) Α4ίί5Τ7ι〇χ297 ^} A7 B7 > 43891 2 V. Description of the invention (= knot = sex and zero defects The adverse effect of crystal growth is still a non-uniform devitrification rate that will increase with the temperature and volume: more polymorphic contacts will make the single crystal fragmentation: the industrialization of production becomes more serious. In these applications, it is necessary to ===! Increase the possibility of considerable non-uniform glass breaking, which will reduce the deformation and reduce the growth of the single crystal block at zero. The purpose of this invention is to prepare single-crystal osmium with better quality, in particular, to prepare single-crystal with a larger amount of material. The material is the same as that of low-oxygen cutting. Therefore, the integrity of the container structure is improved, and the degree of wonderful growth of the zero defect single crystal is improved. In an efficient and cost-effective manner, the smallest impact on the current commercial process is achieved, so that the single crystal hair also reaches So improved It is also the object of the present invention. Therefore, in short, the present invention is to produce a single crystal hair crystal block from a polycrystalline stone by a needle = a process. According to this process, the polycrystalline material is filled into a silicon oxide valley state. This container It can be treated or untreated silicon oxide. This device is supported by a graphite support container designed to receive a silicon oxide container, in a manner that supports the container like a nested stone. The outer surface of this container is at least partly in contact with the outer layer supporting the container. This contact area defines an interface area. The graphite-supported container is further designed for use in czochralski -6- This paper size is applicable to Chinese National Standards (CNS) A4 said Gatseng ----- 1T ------ ^ (Read the notes on the back first and then fill out this I) Central Bureau of Standards, Ministry of Economic Affairs Printed by an employee consumer cooperative (210x297 mm A3B9 1 2 A7 Β7 Μ Printed by the staff of the Central Ministry of Economic Affairs of the Ministry of Economic Affairs of the People's Republic of China) Printed by the cooperative V. Invention description (Type 4 pumping device, and can be processed or untreated graphite Pedestal like Ink support container. According to an embodiment of this process, the concentration of calcium element present in the graphite support container is relatively low, so that a large number of non-uniform de-glassing at the interface area of the silicon oxide container can be prevented in subsequent steps. In a preferred process, the weight concentration of calcium in the graphite support container will not exceed about 1 PPM. In order of increasing strength, the calcium concentration in the graphite support container will not exceed about 0.7 PPM. , Not more than about 0.2 ppM, and not more than about 0.1 PPM. According to another embodiment of this process, the accumulated amount of alkali gold and alkaline earth gold elements in the graphite-made support container will not exceed the weight concentration ppM. In the graphite-supported container, the weight concentration accumulated in the group consisting of calcium, magnesium, gill, lithium, sodium, and potassium is preferably not more than 7 PPM. In the graphite-supported container of this process example, the weight concentration of calcium is preferably not more than 0.2 PPM. In any of the foregoing embodiments, the 'support container, the container, and the polycrystalline crushed raw material are heated to melt the polycrystalline silicon and form a silicon melt. The graphite support container can be heated to a temperature of at least 15 5 ° (preferably 1 5 7 5 ° C) at the inside of the edge portion of the support container and the outer portion of the silicon oxide container, and lasted for about 2 hours (4 Hours is better). The monocrystalline silicon ingot is pulled out from this melting. At the same time, when the silicon melt in the self-oxidizing silicon container generates a single crystal sand crystal block, the invention also supports a graphite support container, such as a base or a crucible, which supports the container like a bird's nest. This support container includes a graphite set of paper-size paper (CNS) A4 size (2Η) × 297 male thin --------- ά ------ IT --- --- 0 * 1 (Please read the precautions on the back before filling out this page) r. Ί 4 3 B 9 1 2 A7 ___B7 5. The description of the invention (5). Importantly, according to one embodiment of the graphite-supported container, the weight concentration of calcium contained in the stone black body does not exceed i PPM. If it is arranged according to its superiority, the concentration of calcium in the graphite body is not more than about 0.7 ppM, not more than about 0.2 PPM, and not more than about 0.1 PPM. According to another embodiment of the graphite supporting container, the weight of the gold group and alkaline earth metal group elements in the graphite body is not more than 1 ppM. In the graphite body, calcium, magnesium, gill, lithium, The cumulative weight concentration of a group consisting of sodium and potassium is preferably not more than 0,7 PPM. A better feeling is that the weight concentration of calcium in the graphite body should not exceed 0.2 ppm. For the two graphite-supported containers described above, either of the graphite bodies has an open body cavity defined by the inside surface, and its shape is designed to generate single crystal silicon ingots from a silicon melt in a silicon oxide container, such as a bird's nest. It generally receives the trough, and at least a part of the inner side of the edge of the graphite supporting container is in contact with the outer part of the silicon oxide container. This graphite body is designed for use with Czochralski crystal pullers. The body can be replaced entirely by graphite or by a shovel layer covering at least the inner surface of the body. Other features and objects of the present invention are partly obvious to those skilled in the art, and part will be shown later. Printed by the Ministry of Economic Affairs and the Central Bureau of Quasi-Continental Bureau, Consumers' Cooperative Printing 1_ Explanation of the simple mushroom Figure 1 is a cross-sectional view of an empty Czochralski crucible. Figure 2-A graphite base suitable for receiving the empty crucible in Figure 1. Figure 3 is a Czochralski type crystal puller, including the cross-section view of the crucible in Figure I placed on and supported by the base of Figure 2. * This equipment Home County (CNS) Congxue (21 () > < 297 Gongchu) A7 rV 4389 1 2 ___ B7_ V. Description of the Invention (6) It is mainly used in the batch processa Figure 4 is a Chuklas Basic (C ζ chra 丨 ski) type crystal puller, which includes a cross-sectional view of the inner crucible, and an outer crucible placed on and supported by a graphite base. This device is mainly used in continuous processes. FIG. 5 is a schematic flowchart showing the manufacture of a graphite support container. Figure 6 is a graph showing whether a homogeneous silicon oxide pot can be obtained under different necking tests using a silicon oxide pot supported by a graphite base with a concentration range of 0.1 PPM to 0.2 PPM or 0.8 PPM to 1.7 PPM. The row of single crystals grows wonderfully. ^ ------ ΐτ ------- ^ (Please read the notes on the back before filling out this page) Symbols for printed components of the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. Description 1 0 Silicon oxide crucible 3 0 Graphite base 10 'Inner crucible 30 · Base 10 0 ”Outer crucible 3 2 Inner surface 1 2 Inner surface layer 3 4 Outer surface layer 1 4 Outer surface layer 3 5 Central line 1 5 Central line 3 6 Top edge 1 6 Top edge 3 7 bottom part 1 7 bottom part 38 corner area 1 8 corner area 3 9 side wall area i 9 side wall area 3 9 a top part 1 9 a top part 3 9 b middle part 1 9 b middle part. 3 9 c Bottom part 1 9 c Bottom part 4 4 Open body cavity 2 4 Open body cavity 46 Base-9-This paper size applies to Chinese National Standard (CNS) A4 specification (210X29? Mm) A38912 A7 B7 V. Description of the invention (7 4 8 Molten silicon 50 Czochralski crystal puller 52 base 58 molten liquid level 5 4 heater The present invention will be further described below with reference to the legend, wherein similar items will be marked in several figures The same number is used. Firefly details the consumer cooperation and printing by the Central Bureau of Standards of the Ministry of Economic Affairs. Notes on filling out this page)
根據本發明，於單晶矽在丘克拉斯基（c z 0 c h r a丨s k丨）型結 晶抽拉器内的製作過程中，在一個石墨製支承容器（如基座） 體内或表面所含的鹼土金族和鹼金族元素濃度（特別是鈣）會 嚴重地影響到一個氧化矽容器（如坩堝），在由此支承容器支 持時的非均勻去玻璃化作用的發生與程度。如果不受理論的 約束’使用具低濃度之鹼金族及鹼土金族雜質之支承容器， 可降低了雜質自支承容器擴散至氧化矽外層表面的程度，這 減低了局部結晶化孕核位置的數目，也因此降低了氧化珍容 器上非均句去玻璃化的程度。單晶矽可以用含相當低之鈣濃 度（重量濃度最好小於等於0.7 PPM)之石墨支承容器來製 作，而在玻璁狀氧化矽容器内沒有發生嚴重的非均勻玻璃化 作用，即使是產自高容量的裝填下也一樣。降低玻璃狀氧化 秒容器内之局域化結晶可改善此氧化矽容器整體的結構性； 此外’也改良了包含增進零缺陷成長在内之矽結晶品質D 如同在此處所用的，「容器」一詞是特別是指包含可於其 中形成一池（pool)熔融矽’且可用於在丘克拉斯基 10- 本紙張尺度適用中國國家標準（CNS ) A4規格{ 210X297公瘦） .¾1 4389 1 2 A7 B7 羥濟都中央橾準局員工消費合作社印製 五、發明説明（8 ) (Czochralski)型晶體抽拉器中製備單晶矽晶塊之坩堝、套 襯j或其他種類的谷器。而「支承容器」一詞則是專門用在 包含用於支承一容器之基座、坩堝、或其他種類的容器。而 多晶形矽」一詞是指包括不限制形狀，樣式或是製造方洼 之多晶粒之矽質，其中包含了像是標準上由Siemens型製程 製備义塊狀（chuck)多晶矽，以及-般由流體床反應製程所 製備的顆粒狀多晶矽。 多晶形碎被裝填人適合於用在接合本發明中石f支承容器 =氧化矽容器中’以便以丘克拉斯基（Cz〇chraUki)法製備 單时矽。此氧化矽容器可以是未經處理過，完全由氧化矽組 成之玻璃狀氧化石夕容器，或可替代以由玻璃狀氧切所组成 的已處理過之氧化石夕容器，其内外層表面中，至少有一部份 的氧切容器内層和/或外層表面，是根據目前所知或未來 將於該項技藝中所發展出之方法加以處理。舉例來說，這樣 的處理目前包括有在表面形成外鍍層(如_，或於此位置 上直接成長鍍層。一般較好的方式是在表面上形成一均勻之 去玻璃化氧料層，或是均勻地塗上—層去玻璃化促進劑以 增進均勻之去玻璃化層㈣成。料切容器表面上形成利 用均勾的去玻璃化層與本發明中所汲汲於防止之非均勾去玻 璃化作用，在去玻璃化整個程序的控制程度上和最終去玻璃 ，之氧切層均勾和非均勻的本性上是有所不同的。益論該 奋益疋否經過處理，氧化矽容器.整體内部基本上最好是完全 不含鹼土金屬、鹼金屬、或其他雜質成份 ： 之内外層表面基本上最好也完全不含分佈不均二土夕：二 11 i------IT------^ • V (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適财國國家標準7^5 ) ( 2[〇χ29?公楚 A7 B7 V 43891 2 五、發明説明（9) 或鹼金屬雜質。適當品皙> ^ , 界臾圪田印資疋乳化矽容器商業產品有許多不同 的來源，例如包括通用電氣（General Eieetrk c。）之石 品部門（俄亥俄州，克里夫蘭市）。 雖然氧切容器並不絕對受限於特殊的幾何形狀，但此容 為-般是杯狀，並且其内層與外層表面至少定義一個能夠包 含，容納這樣的嫁㈣質之封閉結構。對照以，代表例中 的氧化矽合器疋一個未經處理過的氧化矽坩堝1 〇。該坩蜗 10-般具有-内表層12 ’ 一外表層14，一中央線15及頂緣 16。該内層12定義出一開放體腔“，而多晶形矽可被充填 於其中。甜蜗ίο分別包含一底層17，一角落區18及以一側 壁區19,參考圖中底層17，角落區“與側壁區〗9。在此圖 示的實施例中，側壁區丨9基本上是垂直的而底層17基本上 則是水平的。更確切地說，側壁區19定義出一垂直環繞區 域，其中包括一頂層部份19a，一中層部份19b，及以一底層 部份19c。而頂、中、底層部份19a、19b、丨“每一層包含整 個側壁區1 9約1 /3的表面積。頂、中、底層各部份19a、 I9b、19c其間大致上的分界是以虛線21表示。底層17是呈 拋物面，其斜率是水平部份遠超過垂直部份。而角落區Η 是一呈彎曲角度，在側壁19與底層17交會區附近的邊緣區 域。此角落區18與側壁區19在角落區18曲率終止處交會， 在圖中以線22表示。角落區ι8之曲率半徑小於底層丨7，並 且於底層17曲率半徑轉變的地方交會。此角落區18具有上 與下兩部，而每一半約包含著整個角落區表面積的一 半’其上半部接近側壁區19而下半部則接近底層17。坩堝 -12- 本紙伕尺度適用中國國家標準（CNS ) Α4規格（2丨0><297公釐） ----------私衣------1T------^ ί請先聞讀背面之注意事項再填寫本頁) 經濟部中央標準局負工消費合作社印31 43891 2 五、發明説明（10) ' 〜 〗〇的中央線15是與側壁區19平行，而交會於底層17的幾何 中心。 石墨、支承容器在石夕燦於其中成形，和於自炼融珍中製作單 晶树支撐著氧切容器a此石墨支承容器可以是經過或未 經過處理的容器…個未經處理之石墨支承容器完全是由石 墨形式之碳所组成。而一個已經處理過之石墨支承容器包含 一全由石墨组成之角錐形容器以及其内表層和/或外表層至 少一部份是經過是根據目前所知或即將於該項技藝中所發展 出之方法加以處理（如鍍層）。這樣的處理目前包括像是在表 面上形成Sic、TiC、NbC、TaC、ZrC、BN或是玻璃f的碳， 或是於角錐容器表面原處成長嫂層。 經濟部中央梂準局員工消费合作社印装 雖然氧化矽容器並不絕對受限於特殊的幾何形狀，但此容 器一般是杯狀，並且其内層與外層表面至少定義一結構，其 適於接受諸如置身於石墨支承巢的方式來支撐之氧化矽容 器》而此容器的外層表面至少有一部份是與支承容器的外層 接觸。這個接觸的區域即定義出了一個界面區。石墨支承容 器更是設計來適用於丘克拉斯基（CzochraUki)型柚拉器。 對照圖2，代表例的石墨支承容器是一個未經處理過的石墨 基座30。该基座30有一内表面32，一外表層34，一中央線 35及頂緣36。該基座30之内層32定義出—開放體腔44，並 且分別包含一底層部份3 7，一角落區3 8及以一側壁區3 9， 參考圖中底層37,角落區38與甸壁區39。在此圖示的實施 例中，基座底層3 7基本上則是水平的而側壁區3 9基本上是 垂直的。更確切地說，底層37是呈拋物面，其斜率是水平 -13- 本紙張尺度適用中國國家榡準（CNS ) ΑΊ規袼（210X297公着} A7 B7 ”43891 2 五、發明説明（n ) 過垂直部份1壁區39則定義出一垂直環繞區 或、其中包括一頂層部份39a，一中層部份m，及以一底層 :伤39C而k頂、中、底層部份39a、39b、39c每-層約佔 正個側壁區39約1/3的表面積。頂、中、底層各部份39a、 现、39e其間約略的分界是以虛線41表示。基座侧壁㈣ 的厚度是向開口些微地逐漸變小，而非真正垂直，所以基座 3〇頂緣36處之侧壁區39的直徑就要比其下部，如底側別 處：所測得來得大。這個侧壁39上直徑些微地擴大有助於 承接^禍10或是其他置入開放空腔44之氧化石夕容器a而基 座角落38疋一主幫曲角度，在侧壁區39與底層交會區附 近的邊緣區域。而泫基座角落區38與側壁區在角落區Μ 曲率終止處交會，在圖中是以虛線42表示。角落區38之曲 率半徑小於底層3 7，並且於底層3 7曲率半徑轉變的地方交 會。此角落區38具有上與下兩部，而每一半約包含著整個 角落區38表面積的一半，其上半部接近侧壁區39而下半部 則接近底層3 7 »基座3 0之中央線3 5實質上與侧壁區3 9平行 並交於底層37之幾何中心點。基座3〇並包括一位於内表面 32之底層部份37下方之基底46。基底46利於連接丘克拉斯 基（Czochralski)型晶體抽拉器之可移動的底座52。 圖3疋一置入丘克拉斯基（Czochralski)型晶體抽拉器5〇 中的基座30，並且由其支托住之坩堝丨〇。此抽拉器基座 之基底46是接附至可移動之底座52。此裝置主要用於整批 次丘克拉斯基（Czochralsk丨）型的單晶矽製程上。此基座 由底層37、角落區38和侧壁區39之底層3 9b所定義出之内 -14- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ----------^------ (請先閱讀背面之注意事項再填寫本頁) 經濟部中央橾準局員工消費合作.社印裝 --------------------According to the present invention, during the manufacturing process of single crystal silicon in a cz 0 chra 丨 sk 丨 type crystal puller, a graphite support container (such as a base) contains Alkaline earth metal group and alkali metal group element concentration (especially calcium) will seriously affect a silicon oxide container (such as a crucible), and the occurrence and extent of non-uniform devitrification when supported by the support container. If it is not bound by theory, the use of supporting containers with alkali metal and alkaline earth metal impurities at a low concentration can reduce the degree of diffusion of impurities from the supporting container to the outer surface of the silicon oxide, which reduces the location of the localized crystallization nuclei. The number also reduces the degree of devitrification of the uneven sentence on the container. Monocrystalline silicon can be made from a graphite-supported container with a relatively low calcium concentration (preferably less than or equal to 0.7 PPM by weight), and no serious non-uniform vitrification occurs in the glass-like silicon oxide container, even if it is produced. The same is true for high-capacity loading. Reducing the localized crystals in the glass-like oxidation seconds container can improve the overall structure of the silicon oxide container; in addition, 'the quality of silicon crystals including the promotion of zero defect growth has also been improved. As used herein, the "container" The term refers in particular to the inclusion of molten silicon in which a pool can be formed and which can be used in Chuklaski 10- This paper size applies the Chinese National Standard (CNS) A4 specification {210X297 male thin). ¾ 1 4389 1 2 A7 B7 Printed by the Consumers' Cooperative of the Central Hypothecary Bureau of Hydroxid. V. Description of the invention (8) (Czochralski) type crystal extractor for the production of crucibles, sleeves or other types of troughs for monocrystalline silicon ingots. The term "supporting container" is used specifically to include a base, crucible, or other type of container for supporting a container. The term "polycrystalline silicon" refers to polysilicon that includes unrestricted shapes, patterns, or square depressions. It includes polycrystalline silicon (chuck) polycrystalline silicon prepared by standard Siemens processes, and- The granular polycrystalline silicon is generally prepared by a fluid bed reaction process. The polymorphic crusher is suitable for use in the bonding of the present invention with a stone support container = a silicon oxide container 'in order to prepare monolithic silicon by the Czochra Uki method. The silicon oxide container can be an untreated, glassy oxide container composed entirely of silicon oxide, or it can be replaced with a glassy oxide container composed of glassy oxygen cuts. At least part of the inner and / or outer surface of the oxygen-cut container is treated according to methods currently known or to be developed in the future. For example, such treatment currently includes forming an outer plating layer on the surface (such as _, or directly growing the plating layer at this position. Generally a better way is to form a uniform devitrified oxygen material layer on the surface, or Apply evenly-a layer of devitrification accelerator to improve the formation of uniform devitrification layer. A uniform devitrification layer is formed on the surface of the material cutting container and the non-uniform devitrification glass drawn in the present invention is used to prevent it. The chemical action is different in the degree of control of the entire devitrification process and in the final devitrification, the oxygen cut layer is uniform and non-uniform in nature. It is worthwhile to say whether the Fenyi has been treated, silicon oxide container. The whole interior is basically preferably completely free of alkaline earth metals, alkali metals, or other impurity components: the inner and outer surface is basically preferably free of uneven distribution. II soil evening: II 11 --- IT ------ ^ • V (Please read the notes on the back before filling out this page) This paper is suitable for the national standard of the rich country 7 ^ 5) (2 [〇χ29? 公 楚 A7 B7 V 43891 2 V. Invention Note (9) or an alkali metal impurity. Appropriate product > ^, 臾 圪 田There are many different sources of commercial products for Indian Silicone Emulsion Silicon Containers, such as the Stone Division (General Cie.) (Cleveland, Ohio). Although oxygen-cut containers are not absolutely limited to special Geometric shape, but this volume is generally cup-shaped, and its inner layer and outer layer surface define at least one closed structure that can contain and accommodate such a mating substance. In contrast, the silicon oxide coupler in the representative example is not Treated silicon oxide crucible 10. The crucible 10 generally has an inner surface layer 12 ', an outer surface layer 14, a center line 15, and a top edge 16. The inner layer 12 defines an open body cavity ", and the polycrystalline silicon It can be filled in. The sweet snail includes a bottom layer 17, a corner area 18, and a side wall area 19, referring to the bottom layer 17, corner area, and side wall area 9 in the figure. In the illustrated embodiment, The side wall region 9 is substantially vertical and the bottom layer 17 is substantially horizontal. To be more precise, the side wall region 19 defines a vertical surrounding area including a top layer portion 19a, a middle layer portion 19b, and Bottom part 19c The top, middle, and bottom parts 19a, 19b, and "" each layer contains the entire side wall area of about 1/3 of the surface area. The top, middle, and bottom parts 19a, I9b, and 19c are roughly delimited by dashed lines. 21 indicates. The bottom layer 17 is parabolic, and its slope is far more horizontal than the vertical portion. The corner area Η is a curved angle at the edge area near the intersection of the side wall 19 and the bottom layer 17. This corner area 18 and the side wall Zone 19 meets at the end of the curvature of corner area 18, and is represented by line 22 in the figure. The radius of curvature of corner area ι8 is smaller than that of bottom layer 丨 7, and meets where the curvature radius of bottom layer 17 changes. Each half contains approximately half of the surface area of the entire corner region ', with the upper half approaching the side wall region 19 and the lower half approaching the bottom layer 17. Crucible-12- The standard of this paper is applicable to China National Standard (CNS) Α4 specification (2 丨 0 > < 297 mm) ---------- Private clothing ------ 1T ---- -^ ί Please read the precautions on the back before filling out this page) Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives 31 43891 2 V. Description of the invention (10) '~ 〖〇 The central line 15 is connected with the side wall area 19 Parallel, but intersect at the geometric center of the bottom layer 17. The graphite and supporting container are formed in Shi Xican, and the single crystal tree is made in the self-refining smelt to support the oxygen cutting containera. This graphite supporting container can be a container with or without treatment ... an untreated graphite support The container consists entirely of carbon in the form of graphite. A treated graphite support container contains a pyramidal container made entirely of graphite and at least part of its inner surface and / or outer surface has been developed based on what is currently known or about to be developed in this technology Methods (such as plating). Such treatment currently includes, for example, carbon forming Sic, TiC, NbC, TaC, ZrC, BN, or glass f on the surface, or growing a puppet layer in situ on the surface of the pyramid container. Printed by the Consumers' Cooperatives of the Central Government Bureau of the Ministry of Economic Affairs. Although the silicon oxide container is not absolutely restricted to a special geometry, the container is generally cup-shaped, and its inner and outer surfaces define at least one structure, which is suitable for receiving The silicon oxide container is supported by being placed in a graphite supporting nest. At least a part of the outer surface of the container is in contact with the outer layer of the supporting container. This contact area defines an interface area. The graphite support container is designed to be suitable for CzochraUki type grapefruit puller. Referring to Fig. 2, a representative graphite supporting container is an untreated graphite base 30. As shown in Figs. The base 30 has an inner surface 32, an outer surface layer 34, a center line 35 and a top edge 36. The inner layer 32 of the base 30 defines an open body cavity 44 and includes a bottom layer 37, a corner region 38 and a side wall region 39, respectively. Referring to the bottom layer 37, the corner region 38 and the Dianbi region in the figure 39. In the illustrated embodiment, the base layer 37 is substantially horizontal and the sidewall region 39 is substantially vertical. More specifically, the bottom layer 37 is parabolic, and its slope is horizontal. -13- This paper is scaled to the Chinese National Standard (CNS) ΑΊΊ (210X297)} 43891 2 V. Description of the invention (n) The vertical wall 1 area 39 defines a vertical surrounding area or, including a top layer portion 39a, a middle layer portion m, and a bottom layer: injury 39C and k top, middle, and bottom portions 39a, 39b, Each layer of 39c occupies about 1/3 of the surface area of the side wall area 39. The approximate boundaries between the top, middle, and bottom parts 39a, present, and 39e are indicated by dashed lines 41. The thickness of the side wall of the base is The opening becomes slightly smaller, rather than being truly vertical, so the diameter of the side wall region 39 at the top edge 36 of the base 30 is greater than the lower part, such as elsewhere on the bottom side: as measured. This side wall 39 The slightly enlarged diameter helps to accept the blaze 10 or other oxidized stone container a placed in the open cavity 44 and the corner 38 of the base is a major angle of the corner, near the edge of the side wall area 39 and the bottom intersection area The corner area 38 of the pedestal meets the side wall area at the end of the curvature M in the corner area. Dashed line 42 indicates that the radius of curvature of the corner region 38 is smaller than the bottom layer 37 and meets where the curvature radius of the bottom layer 37 changes. This corner region 38 has upper and lower parts, and each half contains approximately the entire surface area of the corner region 38. Half of which the upper half is close to the side wall area 39 and the lower half is close to the bottom layer 3 7 »The center line 3 5 of the base 30 is substantially parallel to the side wall area 39 and intersects the geometric center point of the bottom layer 37. Base The seat 30 includes a base 46 located below the bottom portion 37 of the inner surface 32. The base 46 facilitates connection to a movable base 52 of a Czochralski-type crystal puller. Figure 3 Czochralski-type crystal puller 50 in the base 30 and the crucible supported by it. The base 46 of this puller base is attached to the movable base 52. This The device is mainly used for the entire batch of Czochralsk single-crystal silicon process. This base is defined by the bottom layer 3 9b of the bottom layer 37, the corner region 38 and the side wall region -14- This paper size applies to China National Standard (CNS) A4 (210X297 mm) --------- -^ ------ (Please read the precautions on the back before filling out this page) The Consumer Cooperation of the Central Procurement Bureau of the Ministry of Economic Affairs. ----
I - I I 經濟部令央樣準局員工消費合作杜印製 43891 2 A7 _ B7 五、發明説明（12) 表層32部份是與坩堝10中相對應之部份门、18、和i9b之外 層14接觸。此容器一支承容器系統的界面區是由這坩堝與 基座間接觸的面積來定出的。然而，一般的情形中，此界面 區之範圍及位置將隨對氧化矽容器和石墨支承容器的特殊設 計而有所不同。這般的設計通常是基於結構上的支承以及熱 量轉移的考量。再者，對於批次化的製程而言，定義界面區 的接觸面積會隨晶體成長製程期間時間的變化而變。參考圖 3，在矽熔液於氧化矽坩堝10形成之後，低於熔液液面”之 熔融態矽48會側壁區19，角落區18以及底層口施以—液態 (重力）壓。因為受熱之氧化矽容器在熔點溫度時會軟化，所 以液靜壓/重力會迫使已軟化的氧化矽容器擠向石墨支承容 器β然而，在批次製程中，當矽晶塊形成時，熔融矽的液高 會降低，而施於側壁區丨9，角落區！ 8以及底層丨7之液靜壓 也就因為單晶矽塊的拉出而降低β最後則因此使得侧壁19、 39的上部19a ' 3 9a間彼此分開，這致使了當單晶拉出時，坩 堝側壁區1 9之外層表面1 4與支承容器側壁區丨9的内表面3 2 之間的接觸面積下降。因此，一般來說是有可能以氧化矽容 器與支承容器間接觸時間的長短來定義界面區的次級區域： (1) 一個基本上位於起始熔解線之上的非接觸區（即是位於熔 融矽4 8表面5 8的最初位置之上）；（2)位於起始熔解線下但 在最終熔解線之上的暫時接觸區域；以及（3)在整個單晶拉 出過程中，一個連續接觸的區域_,其上液靜壓和/或氧化矽 的重量施力迫使已軟化的氧化矽容器擠向石墨支承容器。對 於圖1至圖4中此容器/支承容器系統，該非接觸區大致上與 -15- 匚奶）八峨格（21〇父297公釐） ------ΐτ------.^ (請先閱讀背面之注意事項再填寫本頁) A7 B7 1 43891 2 五 '發明説明（13) 壁與石墨基座間1/3的界面區有關，如圖中該 ? 7奋器壁义19咖39&區所示。而暫時接觸區則與例 =2/3和角落上半部份相關。舉例來說，在圖I至圖4中 勺暫時接觸區可包括側壁區19b、19c、⑽、伙及角落區 18、38的上半部。而連績區一般是與底層η、η及角落區 18、38的下半部有關。 长囷1和3分別中所示之坩堝10與基座3〇是代表例e其 乳化矽容器和石墨支承容器的幾何形狀是會與圖例中的實施 例不同’可是卻仍在本發明的範圍之内。-種氧化矽容器和 石墨支承容器的替代性設計顯示在圖4。在該設計中，一個 置於石墨支承容器(基座30，)且由其支撐之雙容器系統，系 統是2—内層坩堝10·和外層坩堝1〇"所構成，此組態裝置典 型上是用在使用連續型丘克拉斯基（Cz〇chralski)製程方式 來製備單晶矽上。 無論該石墨支承容器是否經過處理，也無論這支承容器的 头何形狀多特殊，石墨支承容器整個内部基本上最好是完全 不含鹼土金屬、鹼金屬、或其他雜質成份，而該氧化矽容器 之内外層表面基本上最好也完全不含分佈不均勻的鹼土金屬 或齡金屬雜雜《在石墨本體和其表面上，由鈣、鎂、總、 鋰、鈉以及鉀組成的群組所累積的重量濃度應當相當低，以 防止當多晶形矽熔化且單晶矽晶塊自其中抽拉出之時，於氧 化矽界面區發生嚴重的非均勻去滅璃化作用。正如在這裡所 用的凋彙’ 「厫重地非均勾去玻璃化」所指的是破璃質氧化 矽局部結晶作用，這使致了此氧化矽容器中，在商業價值上 -16 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公董） 餐-- (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局M3；工消費合作社印聚 -1T. .I - I ____I _ _ _I-II Ministry of Economic Affairs, Central Bureau of Standards and Procurement, employee printing cooperation Du Duan 43891 2 A7 _ B7 V. Description of the invention (12) The surface layer 32 is the part corresponding to the crucible 10, 18, and i9b outer layer 14 contacts. The interface area of the container-supporting container system is determined by the contact area between the crucible and the base. However, in general, the range and location of this interface area will vary depending on the special design of the silica container and graphite support container. Such designs are usually based on structural support and consideration of heat transfer. Furthermore, for batch processes, the contact area defining the interface area will change with time during the crystal growth process. Referring to FIG. 3, after the silicon melt is formed in the silicon oxide crucible 10, the molten silicon 48 “below the melt liquid level” applies pressure to the side wall region 19, the corner region 18, and the bottom port—liquid (gravity) pressure. The silicon oxide container will soften at the melting temperature, so hydrostatic pressure / gravity will force the softened silicon oxide container to squeeze to the graphite support container. However, in the batch process, when the silicon crystal block is formed, the liquid of molten silicon The height will decrease, and the hydrostatic pressure applied to the side wall area 9 and the corner area 8 and the bottom layer 7 will also decrease β due to the pull-out of the single crystal silicon block. Finally, the upper part 19a of the side wall 19, 39 will therefore be caused. 3a and 9a are separated from each other, which causes the contact area between the outer surface 14 of the crucible side wall region 19 and the inner surface 3 2 of the side wall region 9 of the supporting container to decrease when the single crystal is pulled out. Therefore, in general, It is possible to define the secondary area of the interface area by the length of the contact time between the silicon oxide container and the support container: (1) a non-contact area substantially above the initial melting line (that is, located on the surface of the molten silicon 4 8 5 8 above the initial position); (2) located A temporary contact area below the initial melting line but above the final melting line; and (3) a continuous contact area _ during the entire single crystal pull-out process, on which the hydrostatic pressure and / or the weight of the silicon oxide force Force the softened silica container to the graphite support container. For this container / support container system in Figures 1 to 4, the non-contact zone is approximately -15- 匚 milk)） 格 (21〇 parent 297 mm) ------ ΐτ ------. ^ (Please read the notes on the back before filling in this page) A7 B7 1 43891 2 Five 'invention description (13) 1/3 interface between wall and graphite base The area is related to this area, as shown in the figure 7 and 39, and the temporary contact area is related to the example = 2/3 and the upper half of the corner. For example, in Figures 1-4 The temporary contact area of the middle spoon may include the side walls 19b, 19c, ⑽, and the upper half of the corner areas 18, 38. The continuous performance area is generally related to the bottom layer η, η and the lower half of the corner areas 18, 38. The crucibles 10 and the base 3 shown in Changji 1 and 3 are representative examples. The geometry of the emulsified silicon container and graphite support container is the same as the example in the illustration. The same but still within the scope of the present invention.-An alternative design of a silicon oxide container and a graphite support container is shown in Fig. 4. In this design, one is placed on the graphite support container (base 30,) and consists of The two-vessel system supported by it is composed of an inner crucible 10 · and an outer crucible 10 ". This configuration device is typically used to prepare using a continuous Czochralski process. Monocrystalline silicon. Regardless of whether the graphite support container is treated or not, and no matter how special the shape of the head of the support container, the entire interior of the graphite support container is preferably completely free of alkaline earth metals, alkali metals, or other impurities. The inner and outer surfaces of the silicon oxide container are basically preferably free of unevenly distributed alkaline earth metals or age metals. The graphite body and its surface are composed of calcium, magnesium, total, lithium, sodium, and potassium. The weight concentration accumulated in the group should be quite low to prevent serious non-uniform destruction at the silicon oxide interface region when polycrystalline silicon melts and single crystal silicon blocks are pulled out of it. Vitrification. As used here, the term "heavy non-uniform devitrification" refers to the local crystallization of glass-breaking silica, which has led to the commercial value of this silica container -16-this paper Standards are applicable to Chinese National Standard (CNS) A4 specifications (210X297). Meal-(Please read the notes on the back before filling out this page) Central Bureau of Standards, Ministry of Economic Affairs, M3; Industrial and Consumer Cooperatives Co.-1T. .I-I ____I _ _ _
.I I m I 經濟部中央標準局員工消費合作社印装 ；f'V 43891 2 A7 _______B7 五、發明説明（） 重要的整體結構性有所下降(像{:尖突(Cusping)'熔融 (fluxing)孔！虫（pming)、滕凸（bulging)、寶曲（b㈣【叫）與 / 或其他的變形）’與/或在從氧化妙容器中㈣溶液抽拉成長 之零差排塊的長度這個商業的重要性的下降。零差 排長度的下降可接受度的優劣順序為低於1〇%、5%、1%、 以及最佳的〇.5%。雖然零差排長度下降率低於G 5%在商業 上被認為是重要的，但更低的下降率在未來也非重要。重大 的非均句去玻璃化通常是以幾個可見的特點來界定（像是形 成過量的白色粉末，扮隨著多量的孔蝕、尖突和/或熔融）。 溶融與氧化妙容器局部性軟化有關，而其證據是該容器外層 表面出現閃亮的外表β溶融特別適合作為^質化非均勾去玻 璃化指標。因此’在石墨支承容器巾，由鈣、鎂、鳃、鋰、 鈉以及鉀組成的群組所累積的重量濃度最好是相當的低，以 避免炫融的*積起過1 Cm2;料濃度低到只有低於〇5咖2 面積溶融則更好。 一般來說，則述與非經處理過之氧化矽容器共同使用之非 處理石墨支承容器之雜質的濃度（特別是鈣），相對於組成支 承容器之石墨材料的重量（例如參考例丨）’最好是等於或少 於1.0 PPM。以述所言石墨支承容器内雜質的濃度重量，若 以其優越性漸增來排列，為不超過約〇 7 ppM、不超過約〇 5 PPM、不超過約0.2 PPM、以及最佳之不超過約〇1 ppM。當 支承4器内層或氧化矽外層表面其中之一經過處理，如前面 所述，也就是至少一面的界面區受到了處理，而因此可容忍 較高濃度之鹼金屬及鹼土金屬雜質，特別是鈣，而不出現嚴 -17- 本紙乐尺度適用中國國家標準（CNS)A4規格（2丨0><297公楚） --------—^------.π------Φ. (請先聞請背面之注意事項再填寫本頁) Α7 Β7 4389 1 2 五 '發明説明（15) 2的非均勻去玻璃化。隨著包含氧化矽容器和/或石墨支承 :器表面的清潔度、所使用的特殊坩堝尺寸及充填量之加熱 區的溫度分怖曲線（溫度與時間）、氧化矽容器與/或石墨支 承谷器疋否經過過處理等在内的因素變化，確切避開會產生 不良非均勻去玻璃化之鹼金屬及鹼土金屬雜質濃度即有所不 同°但是’若根據前面所設之引導及適當之濃度限度即可得 到改良品質之單晶矽。 旦多晶形的矽裝填入一個合適的氧化矽容器/石墨支承 容器系統’該坩堝即可置入一傳統的丘克拉斯基 (Czochralski)單晶矽成長裝置，而多晶形矽可加熱熔化直 到在在氧化矽容器中形成了一小池的熔融矽。升溫曲線並不 是那麼地絕對’而是通常隨著充填種類（即塊狀、粒狀、或 疋溫合填充）、堆禍的尺寸與設計、單晶成的大小及形式等 等之變化而有所改變》在典型的裝設中，參考圖3與4中所 示之掛禍/支承容器系統，支持支承容器30之基底46的底座 5 2被裝置以使掛禍1 〇的底層1 7貼近加熱器5 4的頂端。該时 禍1 〇慢慢地被放入加熱器5 4的内部空間。而婿瑪1 〇慢慢地 非常接加熱器5 4的速度，以及其他影響熔解多晶形矽等因 素價值，像是加熱器粉末、甜禍的旋轉與系統壓力、則為在 該項技藝中眾所皆知。 通常，對於直徑為1 8英吋（約4 6公分），内裝約6 〇公斤之 多晶形矽的坩堝，位於最初4小時的熔化區間内，該坩堝}〇 與支承容器30内角落區18、38之間接觸區域的溫度至少有 1500t ;而另一種類型是對於同直徑之坩堝，内裝70公斤 -18- 本紙張尺度逋射賴家料（CNS ) Μ規格（加以财笼） --------—，------.1T------^ L 一 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作杜印裝 經濟部中央標準局貝工消背合作'社印製 ^ 4389 1 2 A7 --- B7 五、發明説明（16) — <多晶形矽，於最於4小時到6個小時的熔化區間内，其接 觸區域的溫度至少有丨55〇。而較高的溫度（最好至少有 1 575°C、1600°C或1625°C)也可以用於像是18吋/6〇公斤或是 18吋/70公斤系統中以得到較短的熔化區間，但卻又不會劣 化氧化矽或石墨支承容器結構的整體性。本發明的優點特別 就是在使用了較大直徑與/或較大充填量的氧化矽容器。舉 例來說，對於直杈為2 2英吋（約5 6公分），内裝約1 〇〇公斤之 多晶形矽的坩堝，位於最初七小時到十小時的熔化區間内 (或是更高充填量120公斤’熔化區間約十小時），在其高熱 通量之角落區其溫度最好至少要l6〇〇»c。然而，對於像是 22吋/120公斤的系統，可以用更高的溫度（至少1675ΐ或 1700 C )，來影響等量大小的熔化區間（如自六到八小時的範 固）。對於較大之氧化矽容器，像是可裝14〇公斤多晶形矽， 直徑24英吋（61公分）的坩堝，其角落區域溫度最好至少要 有1650 C、1675°C或是1700°C。至於這樣24吋/140公斤系統 所需之溶化區間會隨著溫度而改變，但在1 6 5 〇 t時，通常範 圍是從10到12小時，而在溫度於i675t至17〇〇°c之間時， 其範圍一般是8到1 0個小時。在另一個例子中，一個可裝填 1 60至200公斤多晶形矽’直徑為3 2英吋（約8 1公分）之坩堝 其角落區可至少被加熱到1650 °C，而1675 °C或1700°C則更 好。這些較高的溫度可使得像是這種有商業價值的3 2吋 / 160-200公斤系統之熔化區間落在丨2到1 5個小時之間。前 面所講的氧化矽容器直徑、裝填量、熔化區間、以及特別像 是這些參數與不同溫度的組合只是被列舉成為本發明優點的 -19- 本紙掁尺度適用中國國家標準（CNS > A4規格（210X297公釐） 威------1T------線 (請先聞讀背面之注意事項再填寫本頁) 經濟部中央標準局負工消費合作.杜印策 43891 2 五、發明説明（17) 代表例，而並是想要如發明範園般地加上限制。熟悉該項技 藝者將會很快地覺察到前述的低雜質支承容器可容許（通常 是）氧化矽容器加熱到較高的溫度而無於已知系統的單晶成 長中相關的劣質化影響。藉著更大的裝填量與，或縮短的熔 化區間，使用較高溫度的能力可以轉變成更高的生產力。 當加熱時，多晶形的矽一般暴露於迫氣氣體中，以排出一 些像是SiO及自SiO與石墨反應所生之co等不受歡迎的氣 體。該迫氣氣體一般是惰性氣體，如氬氣，並且通常是以10 I/min至300 Ι/min的流速流動，端視單晶抽拉器的種類與大 小而定。 一旦梦熔液形成，一條單晶矽晶塊就根據丘克拉斯基 (Czochralski)型製程自熔融矽中抽拉而出。參考圖3與圖 4，單晶梦晶塊5 5是從由石墨基座3 〇所支持之氧化矽坩堝 ίο内的熔融矽之中，在丘克拉斯基（Cz〇chralski)型單晶抽 拉器50内所抽拉出的。此項抽拉單晶矽晶塊之特別方式及 條件在該項技藝中已是廣為人知。當在抽拉單晶矽熔質時， 於熔融期間所升高之高溫通常是一直維持著。當本發明中之 高純度石墨支承容器（如基座3〇)被用來支承一個氧化矽容 器（如掛禍1 0)’該石墨支承容器受到最高通量及最高溫部 份（一般像是支承容器的角落區域）的溫度，於製作單晶矽晶 塊期間’可以維持在或超過150{rc的溫度而不會導致界面區 内氧化硬容器嚴重地非均勻玻璃北；如果必要的話，溫度也 可以至少維持在 1525 t ' 155(rc、1 575 〇c、16〇(rc、1625 c ' 1675°c ’或是1700°C。雖然在矽質熔化及晶體抽拉，該 -20- 本纸張尺度it财關家辟（⑽）A4· ( 21GX_着了 i------ΐτ------0 * (請先閲讀背面之注意事項再填窝本頁) 43891 2 A7 B7 五、發明説明（18) 經清部中夹梯準局貝工消费合作社印31 石墨支承容器的溫度會有所變化’並且在 間内於支承容器的不同部份間也會有局部性的改變 ^承容器的-個特殊位置上其平均時間的溫度對於具較大 谷！多晶㈣直徑較的掛蜗通常是會高—點。—春 以下任何或所有的參數上升時，石墨 ": 土金^辰度的上限將會下降：掛禍尺寸（如直徑）、裝填量 (重Ϊ)、支承容器角落徑向處的溫度 '以及溫度超過 的時間。前面所提及之濃度和溫度的價值均只是指示性的代 表例，-般來說’，任何系統或裝設中最想要的龄金屬及驗土 金屬濃度應當是相當的低’以防止當多晶形矽熔化且單晶矽 晶塊自其中抽拉出的時候，於氧切界面區發生嚴重的非均 勻反玻璃化作用，正如上面所討論的。 内含鹼金屬及鹼土金屬雜質（特別是鈣雜質），_而其濃度適 用1本發明之向純度石墨支承容器可以相同之方法來加以製 備’其中的支承容器，是選用低雜質（如約）濃度的過遽劑與 膝合劑原料’強調純化的步驟，特別用心地加以製成，以確 保鹼金屬及鹼土金屬雜質的濃度在可接受的範圍内。該製造 石墨私序的一個詳述是由T. Ishikawa與T. Nagaoki(英文編輯 者I.C. Lewis)所定訂，刊登於近代碳素科技（jEc 出版，1983 年），特別是第2 2至5 8頁。簡而言之，參照圖5，一個過濾 劑的材料（锻燒過的石油焦煤），經由粉碎、過篩 '並與相對 均勾尺寸的顆粒混合’之後再與嚴合劑（如煤炭焦油瀝青）於 揉合製程中加以综合β在與過濾劑和膠合劑混合之後，混合 物模塑或柚拉成形成想要的形狀（如塊錠狀）。這個已成形的 本紙張尺度適用中國國^7^ )·Α4規格（ ---------衣—— {請先閲讀背面之注意事項再填寫本頁) .11 0--- .II1I I · 沴 4389 1 2 A7 ________£7^ 五、發明説明（19) ，科接著是要在碳化過程中烘焙。而烘燒的材料則在直接或 :在接相步财被石墨化，在這些步驟中，該材料經由浸 …再烘焙以提升其密度與/或接下來的高溫的純化步驟。 通常這樣的純化步驟包括了在大約靡t下使得烘培過的碳 和/或石墨化的碳接受南素氣體-段相當的時間。驗金屬及 驗土金屬雜質是在石墨化步驟中移除，並μ或是經由高溫 純化過程的精煉處理將雜質除去^幹狀石墨加工成形出: 發月中之石·£支承容器。多個石墨支承容器的商用製造商 (如UCAR、Clarksburg、WVa等）均能做到本發明石墨支承容 器所需求之純度等級。 下面的例子說明本發明的原則與優點。 實例 皇:利週不同鈣濃清之石墨某庙來制祚單f功 在幾次的實驗中，單晶矽晶塊是於未經處理之玻璃狀氧化 矽坩堝内形成的矽熔融質中製造。此氧化矽坩堝是由石墨基 座支撐’其具有不同之鈣濃度（範圍自01到J 8 PPM) ο抽拉單 晶矽晶塊之頸縮測試的次數有記錄。 is濟部中央橾準局員工消費合作社印策 以下單晶矽的製造’特別注意觀測每一次實驗中的玻璃質 石英坩堝的品質’其壁層上去玻璃化的程度、孔蚀、尖突及 惊融。與高鈣濃度（自〇.8至1.7 PPM)基座一起使用之坩堝發 現出現大量的去玻璃化現象，並伴隨著相當量之壁層上的孔 蚀、尖突及熔融°相反地，與低濃度（自0]至〇2 PPM)基 座一起使用之坩堝則充其量出現輕微的反玻璃化現象，並伴 隨著最低量之壁層上的孔蝕、尖突及溶融。 -22- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 4389 1 2 五、發明説明（2〇) 貫驗中也決定出了最後單晶£夕晶塊内差排的有無a其纟士果 總知於圖6中。圖6顯不零差之單晶碎成長是經由不同數目 之頸縮測試和使用不同鈣濃度之石墨基座，如圖中分類之高 鈣濃度（範圍從0.8到1.7 PPM)或是低鈣濃度（範園從〇〗到〇 2 PPM)。圖6中的數據指出，在低頸縮測試數目之單晶石夕抽拉 實驗中’若使用低含鈣濃度之基座，零差排成長的達成率為 100°/〇 :但使用高含鈣濃度之基座則只有60%。當所有的數據 均被考量到時’但不予考處開始單晶成長所需之頸縮測試次 數，在使用低含鈣濃度基座條件下，其零差排成長的達成率 為7 2 % ;但高含飼濃度的基座卻只有4 〇 %。因此，使用低各 轉濃度之基座很明顯地影響到零差排單晶矽成長達成的^ 度。 i 根據本發明及上面所述的實例之詳細描述，可察知本發^月 的幾個目標均已達成。此處的解釋及圖例是想要使其他熟系 該項技藝者熟知本發明其原則和實際上的應用。那些熟米兮 項技藝者也許可以將本發明作許許多多的改變及應用，以對 特定的需求做最佳的調適。因此，本發明中所定之特定的實 施例並不是要來表示這是本發明全部或極限。 I I I I I ! I I I 訂 I I I ，線 .· {誚先閏讀背面之注意事項再填寫本頁) 經濟部中央標準局負工消费合作社印裝 -23- 本紙張尺度通用中國國家標準（CNS ) A4規格（210X297公釐）.II m I Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs; f'V 43891 2 A7 _______B7 V. Description of the invention () Important overall structural properties have declined (like {: cusp) 'fluxing Holes! Worms (pming), bulging, bouqu (b㈣ [called] and / or other deformations) 'and / or the length of the homogeneous row of blocks drawn from the oxidized container ㈣ solution The importance of business declines. The order of decreasing acceptability of homodyne row length is less than 10%, 5%, 1%, and the best 0.5%. Although the homodyne length reduction rate below G 5% is considered commercially important, lower decline rates are not important in the future. Significant non-homogeneous devitrification is usually defined by several visible features (such as excessive white powder formation, with large amounts of pitting, spiking, and / or melting). Melting is related to the localized softening of the oxidized container, and the evidence is that the appearance of a shiny β-melt on the outer surface of the container is particularly suitable as an indicator of heterogeneous devitrification. Therefore, in the graphite-supported container towel, the accumulated weight concentration of the group consisting of calcium, magnesium, gill, lithium, sodium, and potassium is preferably quite low, to avoid dazzling melting * accumulation of over 1 Cm2; material concentration It is even better if the melting area is as low as 0-5. Generally speaking, the concentration of impurities (especially calcium) in a non-treated graphite support container used with a non-treated silicon oxide container, relative to the weight of the graphite material constituting the support container (for example, Reference Example 丨) ' It is preferably equal to or less than 1.0 PPM. According to the concentration and weight of impurities in the graphite support container mentioned above, if it is arranged with increasing advantages, it is not more than about 07 ppM, not more than about 0.05 PPM, not more than about 0.2 PPM, and the best is not more than About 〇1 ppM. When one of the inner surface of the support or the outer surface of the silicon oxide is treated, as described above, that is, the interface area on at least one side is treated, and therefore it can tolerate higher concentrations of alkali metal and alkaline earth metal impurities, especially calcium. -17- This paper music scale is applicable to China National Standard (CNS) A4 specifications (2 丨 0 > < 297gongchu) ------------ ^ ------. Π- ----- Φ. (Please read the notes on the back before filling out this page) Α7 Β7 4389 1 2 5'Invention Note (15) 2 Non-uniform devitrification. With the silicon oxide container and / or graphite support: the cleanliness of the surface of the device, the temperature profile (temperature and time) of the heating zone of the special crucible size and filling volume used, the silicon oxide container and / or graphite support valley Changes in factors such as whether the device has been treated, etc., to avoid the occurrence of undesirable non-uniform devitrified alkali metal and alkaline earth metal impurity concentrations. However, 'if based on the guidance set above and appropriate concentration Within limits, single crystal silicon with improved quality can be obtained. Once the polycrystalline silicon is filled into a suitable silica container / graphite support container system, the crucible can be placed in a conventional Czochralski single crystal silicon growth device, and the polycrystalline silicon can be heated and melted until A small pool of molten silicon was formed in a silicon oxide container. The temperature rise curve is not so absolute, but usually varies with the type of filling (ie, lumpy, granular, or mixed-temperature filling), the size and design of the heap, the size and form of the single crystal, and so on. Modified "In a typical installation, referring to the accident / support container system shown in Figs. 3 and 4, the base 5 2 supporting the base 46 of the support container 30 is installed so that the bottom layer 17 of the accident 10 is close to Top of heater 5 4. At this time, the accident 10 is slowly put into the internal space of the heater 54. However, the speed of the heater 10 is very slowly connected to the heater 5 4 and other factors that affect the melting of polycrystalline silicon and other factors, such as heater powder, sweet rotation and system pressure, are in the art. Everyone knows. Generally, for a crucible with a diameter of 18 inches (about 46 cm) and containing about 60 kg of polycrystalline silicon, which is located in the melting zone of the first 4 hours, the crucible and the corner area 18 in the support container 30 The temperature in the contact area between ， 38 is at least 1500t; and the other type is for crucibles of the same diameter, which contains 70kg -18- this paper size radiates household materials (CNS) M specifications (plus money cage)- ------—, ------. 1T ------ ^ L I (Please read the precautions on the back before filling out this page) Employees of the Central Bureau of Standards, Ministry of Economic Affairs, Consumer Consumption, Duanzhuang Economy Printed by the Ministry of Standards and Technology of the People's Republic of China, printed by the Society ^ 4389 1 2 A7 --- B7 V. Description of the Invention (16) — < Polymorphic silicon, in the melting interval of 4 to 6 hours, The temperature in the contact area is at least 55 °. Higher temperatures (preferably at least 1 575 ° C, 1600 ° C or 1625 ° C) can also be used in systems such as 18 inch / 6 kg or 18 inch / 70 kg for shorter melting Range, but without degrading the integrity of the silicon oxide or graphite supporting container structure. An advantage of the present invention is in particular the use of silica vessels with larger diameters and / or larger filling volumes. For example, for a crucible with a straight branch of 22 inches (about 56 cm) and about 1000 kg of polycrystalline silicon, it is located in the melting interval of the first seven to ten hours (or higher filling) The amount of melting is 120 kg '(about 10 hours), and the temperature in the corner zone of its high heat flux is preferably at least 16O »c. However, for systems such as 22 inches / 120 kg, higher temperatures (at least 1675 ° F or 1700 ° C) can be used to affect the melting zone of equal size (such as the range from six to eight hours). For larger silicon oxide vessels, such as crucibles that can hold 14 kilograms of polycrystalline silicon and have a diameter of 24 inches (61 cm), the corner area temperature should be at least 1650 C, 1675 ° C, or 1700 ° C. . As for the melting range required for such a 24 inch / 140 kg system, it will change with temperature, but at 1650 t, it usually ranges from 10 to 12 hours, and at temperatures between i675t and 1700 ° c. Time ranges from 8 to 10 hours. In another example, a crucible that can hold 160 to 200 kg of polycrystalline silicon 'with a diameter of 32 inches (about 81 centimeters) can be heated to a corner area of at least 1650 ° C, and 1675 ° C or 1700 ° C is even better. These higher temperatures can make the melting range of such a commercially valuable 32-inch / 160-200 kg system fall between 2 and 15 hours. The diameter, filling volume, melting range, and especially the combination of these parameters and different temperatures mentioned above are only listed as the advantages of the present invention. -19- The paper scale is applicable to Chinese national standards (CNS > A4 specifications). (210X297 mm) Wei ------ 1T ------ line (please read the notes on the back before filling in this page) Central Laboratories of the Ministry of Economic Affairs, Consumer Cooperation, Du Yince 43891 2 5 (17) The representative example of the invention, and it is intended to add restrictions like the invention. Those skilled in the art will quickly perceive that the aforementioned low impurity support container can tolerate (usually) silicon oxide. The vessel is heated to a higher temperature without the associated degrading effects in the growth of single crystals of known systems. With larger loadings and or shorter melting intervals, the ability to use higher temperatures can be transformed into higher When heated, polycrystalline silicon is generally exposed to a forced gas to exhaust undesirable gases such as SiO and co generated from the reaction of SiO with graphite. The forced gas is generally an inert gas , Like argon, It usually flows at a flow rate of 10 I / min to 300 Ι / min, depending on the type and size of the single crystal puller. Once the dream melt is formed, a single crystal silicon block is based on Chuklaski ( Czochralski) process is drawn from the molten silicon. Referring to Figure 3 and Figure 4, the single crystal dream crystal block 5 5 is from the molten silicon in the silicon oxide crucible ο supported by the graphite base 300. The Czchralski single crystal puller 50 is pulled out. The special method and conditions for pulling single crystal silicon ingots are well known in the art. When drawing When monocrystalline silicon melts, the elevated temperature during melting is usually maintained. When the high-purity graphite support container (such as the pedestal 30) in the present invention is used to support a silicon oxide container (such as an accident) 1 0) 'The graphite support container is subjected to the highest flux and temperature of the highest temperature part (usually like the corner area of the support container). During the production of single crystal silicon ingots,' the temperature can be maintained at or exceeds 150 {rc Does not cause severe non-uniform glass north of the oxidized hard container in the interface area; if necessary Then, the temperature can also be maintained at least 1525 t '155 (rc, 1 575 ° c, 16 ° (rc, 1625 c' 1675 ° c ') or 1700 ° C. Although the silicon melts and the crystal is pulled, the- 20- It's a paper scale, it's financial (J) A4 · (21GX_ 着 i -------- ΐτ ------ 0 * (Please read the precautions on the back before filling in this page) ) 43891 2 A7 B7 V. Description of the invention (18) Printed in the Ministry of Economic Affairs of the PRC, Jiatiquan Bureau Shellfisher Consumer Cooperative 31. The temperature of the graphite support container will vary, and it will also vary between different parts of the support container in the room. There is a local change in the temperature of the average time at a special position of the bearing container. Polychrysalis are usually higher in diameter than snails—points. —When any or all of the parameters below spring rise, the upper limit of graphite will decrease: the size of the accident (such as diameter), the amount of filling (weight), and the temperature at the corner of the supporting container. And how long the temperature has exceeded. The values of concentration and temperature mentioned above are only indicative examples. In general, 'the concentration of the most desired age metal and soil test metal in any system or installation should be quite low' to prevent When polycrystalline silicon melts and single-crystal silicon ingots are pulled out of it, severe non-uniform devitrification occurs at the oxygen-cutting interface region, as discussed above. Contains alkali metal and alkaline earth metal impurities (especially calcium impurities), and its concentration is applicable. 1 The graphite purity support container of the present invention can be prepared in the same way. Among them, the support container is selected with low impurities (such as about) The concentration of overdose and knee mixture raw materials' emphasizes the purification steps, and is specially prepared to ensure that the concentration of alkali metal and alkaline earth metal impurities is within an acceptable range. A detailed description of the private sequence of manufacturing graphite was ordered by T. Ishikawa and T. Nagaoki (English editor IC Lewis), published in modern carbon technology (jEc Publishing, 1983), especially 2nd to 5th 8 page. In short, referring to FIG. 5, a filter material (calcined petroleum coke coal) is pulverized, sieved, and 'mixed with particles of a relatively uniform size' before being mixed with a strict binder (such as coal tar pitch) Synthesize β in the kneading process. After mixing with the filter and adhesive, the mixture is molded or drawn into a desired shape (such as a lumpy ingot). This formed paper size is applicable to China ^ 7 ^) · A4 specifications (--------- clothing-{Please read the precautions on the back before filling this page) .11 0 ---. II1I I · 沴 4389 1 2 A7 ________ £ 7 ^ V. Description of the Invention (19) The branch is then to be baked in the carbonization process. The baked material is graphitized directly or in successive steps. In these steps, the material is dipped and re-baked to increase its density and / or subsequent high temperature purification steps. Usually such a purification step involves allowing the roasted carbon and / or graphitized carbon to accept the southern gas for a considerable period of time at about 100 ° C. Metal and soil metal impurities are removed in the graphitization step, and μ or impurities are removed through the refining treatment of the high temperature purification process. Dry graphite is processed to form: stone in the moon. Support container. Many commercial manufacturers of graphite-supported containers (such as UCAR, Clarksburg, WVa, etc.) can achieve the purity level required by the graphite-supported containers of the present invention. The following examples illustrate the principles and advantages of the present invention. Example Emperor: Li Zhou used different temples of different concentrations of calcium and graphite to make single f work. In several experiments, single crystal silicon ingots were made from silicon melt formed in an untreated glassy silicon oxide crucible. . This silicon oxide crucible is supported by a graphite base. It has different calcium concentrations (ranging from 01 to J 8 PPM). The number of necking tests for pulling single crystal silicon blocks is recorded. is the production of the following monocrystalline silicon by the Consumers 'Cooperative of the Ministry of Economic Affairs of the Ministry of Economic Affairs of the Ministry of Economic Affairs' special attention to observe the quality of the glassy quartz crucible in each experiment. melt. Crucibles used with high calcium concentration (from 0.8 to 1.7 PPM) susceptors found a large amount of devitrification, accompanied by a considerable amount of pitting, spikes and melting on the wall layer. In contrast, Crucibles used with low-concentration (from 0] to 〇2 PPM) pedestals show slight devitrification at best, accompanied by pitting, spiking and melting on the minimum amount of wall layers. -22- This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) 4389 1 2 V. Description of the invention (2) The final single crystal was also determined during the inspection. a. Its fruit is always known in Figure 6. Fig. 6 shows that the growth of single crystals with no difference is through different numbers of necking tests and graphite bases with different calcium concentrations. As shown in the figure, the high calcium concentration (ranging from 0.8 to 1.7 PPM) or low calcium concentration (Fan Garden from 0 to 0 2 PPM). The data in Figure 6 indicates that in the low-neck test number of single crystal evening pull experiments, 'if a base with a low calcium content is used, the homogeneous row growth rate is 100 ° / 0: but using a high content The base of calcium concentration is only 60%. When all the data are taken into account, but the number of necking tests required to start the growth of the single crystal is not taken into account. When using a low calcium concentration pedestal, the achievement rate of homogeneous row growth is 72% ; But the high feed concentration of the pedestal is only 40%. Therefore, the use of a pedestal with a low spin concentration significantly affects the degree of growth achieved by homodyne silicon single crystal growth. i According to the detailed description of the present invention and the examples described above, it can be seen that several goals of the present month have been achieved. The explanations and illustrations here are intended to acquaint others skilled in the art with the principles and practical application of the invention. Those skilled in the art may be able to make many changes and applications of the present invention to make the best adaptation to specific needs. Therefore, the specific embodiments specified in the present invention are not intended to indicate that this is the whole or limit of the present invention. IIIII! III Order III, line. · {诮 Read the precautions on the back before filling out this page) Printed by the Consumers' Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs -23- This paper is in accordance with the Chinese National Standard (CNS) A4 specification ( 210X297 mm)