TWI602958B - Manufacturing method of single-crystalline silicon - Google Patents
Manufacturing method of single-crystalline silicon Download PDFInfo
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本發明是關於一種矽單結晶之製造方法,特別是關於縮頸製程,其是使用丘克拉斯基(Czochralski)法(以下稱為「CZ法」)的矽單結晶之培育步驟的一種。 The present invention relates to a method for producing a single crystal, and more particularly to a necking process which is one of the steps of cultivating a single crystal using a Czochralski method (hereinafter referred to as "CZ method").
矽單結晶多是藉由CZ法製造。在CZ法,是依序實施:觸液製程,使種結晶結觸矽融液;縮頸製程,藉由所謂的達斯縮頸(dash neck)法縮小結晶直徑;肩部培育製程,將單結晶的直徑漸次變寬至到達所要求的直徑;以及體部培育製程,一邊整體保持結晶直徑、一邊繼續培育單結晶。 Many single crystals are produced by the CZ method. In the CZ method, it is carried out in sequence: a liquid-contacting process to make the crystallized contact with the mash; the necking process, which reduces the crystal diameter by the so-called dash neck method; the shoulder cultivation process, the single The diameter of the crystal is gradually widened to reach the desired diameter; and the body cultivation process is continued while cultivating the single crystal while maintaining the crystal diameter as a whole.
縮頸製程,是為了除去因為使種結晶結觸矽融液時的熱衝擊而導入於種結晶內的高密度的滑移差排之必要的製程。藉由培育將結晶直徑縮小至5~6mm程度的一定的長度的單結晶,可將滑移差排從單結晶中除去。 The necking process is a necessary process for removing a high-density slippage row introduced into the seed crystal by thermal shock when the seed crystal is contacted with the melt. The slippage row can be removed from the single crystal by cultivating a single crystal of a certain length which reduces the crystal diameter to about 5 to 6 mm.
在專利文獻1~5揭露有各種的縮頸方法。例如在專利文獻1揭露的方法是:在縮頸製程使矽融液與矽單結晶的固液界面形狀變形而使除去困難之處的差排或可進展到矽單結晶的徑向的外側,使其成環狀而相消而除去。另外在專利文獻2揭露的方法是:在培育結晶軸方位為[110]的矽單結晶,進行使種結晶的直徑減少的縮頸操作而形成第一頸部後,在形成肩 部前使固液界面形狀從上凸變化成下凸,接下來再度進行縮頸操作而形成第二頸部,藉此除去殘留於頸部的中心軸部分的軸狀差排。 Various necking methods are disclosed in Patent Documents 1 to 5. For example, in the method disclosed in Patent Document 1, the shape of the solid-liquid interface between the mash and the single crystal is deformed in the necking process to make the difference in the difficulty of removal or to progress to the outside of the radial direction of the single crystal. It is made into a ring shape and is removed by elimination. Further, in the method disclosed in Patent Document 2, a single crystal having a crystal axis orientation of [110] is grown, and a necking operation for reducing the diameter of the seed crystal is performed to form a first neck portion, and a shoulder is formed. The shape of the solid-liquid interface is changed from the upper convex to the lower convex portion before the front portion, and then the necking operation is performed again to form the second neck portion, thereby removing the axially-shaped row remaining in the central axis portion of the neck portion.
在專利文獻3揭露的方法是:藉由在縮頸製程的最終階段複數次連續進行形成使頸部的直徑增大後縮小而成的增徑部或使頸部的直徑增大後縮小而成的減徑部,藉此使固液界面的形狀頻繁地變化,數度賦予使差排的移動方向變化的機會,有效率地除去軸狀差排。在專利文獻4揭露的方法亦是:藉由在縮頸製程交互形成變細部與擴徑部而除去滑移差排。 The method disclosed in Patent Document 3 is that the diameter-increased portion which is formed by increasing the diameter of the neck portion and increasing the diameter of the neck portion is formed by continuously forming a plurality of times in the final stage of the necking process. Thereby, the shape of the solid-liquid interface is frequently changed, and the chance of changing the moving direction of the difference row is given several times, and the axial difference row is efficiently removed. The method disclosed in Patent Document 4 is also to remove the slip difference row by forming the tapered portion and the enlarged diameter portion in the necking process.
在專利文獻5揭露的方法是:將頸部的培育速度從一般速度(例如2~5mm/min)降低到極端的低速(例如0.8mm/min)並保持一定時間,進行此操作至少一次、以三次以上為佳,使固液界面形狀反覆變化為凹形與凸形,藉此除去滑移差排。 The method disclosed in Patent Document 5 is to reduce the cultivation speed of the neck from a general speed (for example, 2 to 5 mm/min) to an extreme low speed (for example, 0.8 mm/min) for a certain period of time, and perform this operation at least once. More than three times is preferred, and the shape of the solid-liquid interface is changed to a concave shape and a convex shape in order to remove the slip difference row.
另一方面,以達斯縮頸法形成的細頸部,其用以支持因近年的矽單結晶的大口徑化而變重的矽單結晶錠的強度不足,而有在拉引矽單結晶中頸部破斷而引起使矽單結晶墜落等的重大事故之虞。因此,在專利文獻6揭露的方法是:不經縮頸製程而以無縮頸法進行矽單結晶的拉引時,將種結晶的觸液時的輻射罩與矽融液面之間的距離(間隔)設定為80mm以上,增大輻射熱而充分預熱種結晶,藉此抑制因觸液時的熱衝擊之滑移差排的發生。 On the other hand, the thin neck formed by the Darth necking method is used to support the strength of the single crystal ingot which becomes heavier due to the large diameter of the single crystal of the recent years, and there is a single crystal in the pull tab. The middle neck is broken and causes a major accident such as falling single crystals. Therefore, the method disclosed in Patent Document 6 is: the distance between the radiation cover of the seed crystal contact liquid and the liquid surface of the crucible when the drawing of the single crystal is performed without the necking process without the necking process. (Interval) is set to 80 mm or more, and the radiant heat is increased to sufficiently preheat the seed crystals, thereby suppressing the occurrence of slippage due to thermal shock at the time of liquid contact.
【專利文獻1】國際公開第2010/146853號手冊 [Patent Document 1] International Publication No. 2010/146853
【專利文獻2】日本特開2011-57460號公報 [Patent Document 2] Japanese Patent Laid-Open Publication No. 2011-57460
【專利文獻3】日本特開2009-263142號公報 [Patent Document 3] Japanese Patent Laid-Open Publication No. 2009-263142
【專利文獻4】日本特開平11-199384號公報 [Patent Document 4] Japanese Patent Laid-Open No. Hei 11-199384
【專利文獻5】日本特開2001-316198號公報 [Patent Document 5] Japanese Patent Laid-Open Publication No. 2001-316198
【專利文獻6】日本特開2005-281018號公報 [Patent Document 6] Japanese Patent Laid-Open Publication No. 2005-281018
揭露於專利文獻1揭露的習知的縮頸方法,是除去在種結晶觸液時導入之與結晶成長方向平行進展的軸狀差排之方法,但決定適用的界面形狀的手法不明確,軸狀差排存在於種結晶的中心附近時,其除去會非常困難。 The conventional necking method disclosed in Patent Document 1 is a method of removing a shaft-shaped difference which is introduced in parallel with a crystal growth direction when a crystal contact liquid is introduced, but the method of determining the applicable interface shape is not clear, and the shaft is not clear. When the difference row exists near the center of the seed crystal, it is very difficult to remove it.
揭露於專利文獻2的習知的縮頸方法亦同樣,即使固液界面形狀為下凸,其角度非常小,而且在結晶直徑急遽變粗的情況中,會有無法除去軸狀差排或是即使可以除去軸狀差排但必須形成非常長的頸部之類的問題。還有,在為了除去軸狀差排而在實施使結晶直徑變粗的製程後藉由達斯縮頸法再度縮小結晶直徑時,軸狀差排在到達單結晶的外周面而消滅之前被導回中心方向,而無法移除軸狀差排,而有特意實施的軸狀差排除去步驟變為無效之虞。揭露於專利文獻3~5揭露的習知的縮頸方法亦具有與專利文獻2同樣的問題。 Similarly, in the conventional necking method disclosed in Patent Document 2, even if the shape of the solid-liquid interface is convex, the angle is extremely small, and in the case where the crystal diameter is sharply thick, the shaft-shaped row may not be removed or Even if the shaft-shaped row is removed, it is necessary to form a problem such as a very long neck. Further, when the crystal diameter is further reduced by the Darth necking method after the process for making the crystal diameter thicker in order to remove the axial difference, the axial difference is guided before reaching the outer peripheral surface of the single crystal and being destroyed. Back to the center direction, the shaft-shaped difference row cannot be removed, and the intentionally implemented shaft-shaped difference elimination step becomes invalid. The conventional necking method disclosed in Patent Documents 3 to 5 also has the same problems as those of Patent Document 2.
因此,本發明的目的是提供一種矽單結晶之製造方法,其可在縮頸製程確實地除去軸狀差排。 SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a method for producing a single crystal which can reliably remove a shaft-shaped row in a necking process.
為了解決上述問題,根據本發明的矽單結晶之製 造方法,為使用CZ法的矽單結晶之製造方法,使種結晶接觸矽融液後,藉由拉引上述種結晶,使含頸部的矽單結晶在上述種結晶的下端成長,其特徵在於,上述頸部的培育製程包含:第一步驟,以第一拉引速度拉引已接觸上述矽融液的上述種結晶,一邊控制使固液界面形狀成為上凸,一邊形成第一頸部;以及第二步驟,以慢於上述第一拉引速度的第二拉引速度拉引上述種結晶,一邊控制使固液界面形狀成為下凸且使固液界面角度大於結晶增徑角度,一邊形成第二頸部。 In order to solve the above problems, the system of single crystal according to the present invention In the method for producing a single crystal by the CZ method, after the seed crystal is brought into contact with the mash, the above-mentioned seed crystal is pulled, and the cerium single crystal containing the neck is grown at the lower end of the seed crystal. In the above-mentioned neck cultivation process, the first step comprises: pulling the above-mentioned crystal which has contacted the mash liquid at a first pulling speed, and controlling the shape of the solid-liquid interface to be convex, and forming the first neck And a second step of pulling the seed crystal at a second drawing speed slower than the first drawing speed, while controlling the shape of the solid-liquid interface to be convex and making the solid-liquid interface angle larger than the crystal diameter increasing angle Forming a second neck.
藉由本發明,可以使第2步驟中的固液界面形狀成為適當的下凸形狀,而可以將在第一步驟無法除去的軸狀差排在第二步驟除去。因此,可以提高藉由縮頸製程將單結晶無差排化的機率,可以製造高品質的矽單結晶。 According to the present invention, the solid-liquid interface shape in the second step can be made into an appropriate downward convex shape, and the axial difference which cannot be removed in the first step can be removed in the second step. Therefore, it is possible to improve the probability that the single crystal is not poorly discharged by the necking process, and it is possible to produce a high quality single crystal.
在本發明,較佳為:上述第一拉引速度為3mm/min以上、5mm/min以下,上述第一頸部的目標直徑為4mm以上、7mm以下,上述第二拉引速度為1.5mm/min以上、4.5mm/min以下,上述第二頸部的目標直徑為7mm以上、11.5mm以下。在此情況,第一拉引速度與第二拉引速度之差為0.5mm/min。藉此,在第一步驟可藉由達斯縮頸法確實地除去主要的差排。另外,在第二步驟可以使固液界面角度大於結晶增徑角度,可以大幅提高將在對於固液界面垂直的方向進展的軸狀差排排除至單結晶的外側的機率。 In the invention, it is preferable that the first pulling speed is 3 mm/min or more and 5 mm/min or less, the target diameter of the first neck portion is 4 mm or more and 7 mm or less, and the second drawing speed is 1.5 mm/ Above min and below 4.5 mm/min, the target diameter of the second neck portion is 7 mm or more and 11.5 mm or less. In this case, the difference between the first pulling speed and the second pulling speed is 0.5 mm/min. Thereby, in the first step, the main difference row can be surely removed by the Darth necking method. Further, in the second step, the solid-liquid interface angle can be made larger than the crystal diameter increasing angle, and the probability of excluding the axial difference in the direction perpendicular to the solid-liquid interface to the outside of the single crystal can be greatly improved.
在上述第二步驟,以上述固液界面角度為4度以上、10度以下為佳,以上述結晶增徑角度為1度以上、4度以下為佳。藉此,可以將在第二步驟的固液界面形狀的界面角度設 定在適切的範圍。因此,可以提高在第二步驟除去軸狀差排的機率,可以提高第二步驟的可靠度。 In the second step, the solid-liquid interface angle is preferably 4 degrees or more and 10 degrees or less, and the crystal diameter increasing angle is preferably 1 degree or more and 4 degrees or less. Thereby, the interface angle of the solid-liquid interface shape in the second step can be set Set in the appropriate range. Therefore, the probability of removing the shaft-shaped row in the second step can be improved, and the reliability of the second step can be improved.
在本發明中,以將上述第二頸部的長度設為150mm以上為佳。另外,以將上述第一頸部的長度設為200mm以下為佳。第二頸部的長度若為150mm以上,可確實地除去軸狀差排。另外,第一頸部的長度若為200mm以下,可以防止軸狀差排在第一步驟移動至中心軸上,而可以防止成為難以除去軸狀差排的事態。 In the present invention, it is preferable that the length of the second neck portion is 150 mm or more. Further, it is preferable that the length of the first neck portion is 200 mm or less. When the length of the second neck portion is 150 mm or more, the axial difference row can be surely removed. Further, when the length of the first neck portion is 200 mm or less, it is possible to prevent the axial difference from being displaced to the central axis in the first step, and it is possible to prevent a situation in which it is difficult to remove the axial difference.
根據本發明的矽單結晶之製造方法,是以在上述矽融液的上方配置圍繞培育中的矽單結晶的熱遮蔽體而拉引上述矽單結晶的同時,將在上述第二步驟的從上述矽融液到上述熱遮蔽體的下端距離設定為小於在上述第一步驟的從上述矽融液到上述熱遮蔽體的下端距離,而培育上述第二頸部為佳。在此情況,以將在上述第二步驟的從上述矽融液到上述熱遮蔽體的下端距離設定為80mm以下,而培育上述第二頸部為佳。藉此,可以在第一步驟容易形成上凸的固液界面形狀,可容易實施將結晶直徑變細的製程。另在,可以在第二步驟加強將固液界面形狀成為下凸的傾向,可以容易地形成下凸的固液界面形狀。 According to the method for producing a single crystal of the present invention, the above-described single crystal is pulled while the heat shielding body surrounding the single crystal in the cultivation is placed above the above-mentioned molten liquid, and the second step is performed. The distance from the mash to the lower end of the heat shield is set to be smaller than the distance from the mash to the lower end of the heat shield in the first step, and the second neck is preferably incubated. In this case, it is preferable to set the second neck portion by setting the distance from the mash to the lower end of the heat shield in the second step to 80 mm or less. Thereby, the convex solid-liquid interface shape can be easily formed in the first step, and the process of making the crystal diameter thin can be easily performed. Further, in the second step, the solid-liquid interface shape tends to be convex, and the convex-solid solid-liquid interface shape can be easily formed.
根據本發明的矽單結晶之製造方法,是以上述頸部的培育製程的上述第二步驟終了後,不再度將上述單結晶的直徑變細,直接轉而進行肩部培育製程,將上述單結晶的直徑漸次變寬至到達所要求的直徑為佳。藉此,可以防止移動到外周面附近的軸狀差排回到中心附近。因此,可以防止第二步驟 的實施成為無效的事態。 According to the method for producing a single crystal of the present invention, after the end of the second step of the neck culture process, the diameter of the single crystal is not further reduced, and the shoulder cultivation process is directly performed, and the single sheet is processed. It is preferred that the diameter of the crystal gradually widens to reach the desired diameter. Thereby, it is possible to prevent the axial difference moved to the vicinity of the outer peripheral surface from being discharged back to the center. Therefore, the second step can be prevented The implementation became an invalid state of affairs.
藉由本發明,可以提供一種矽單結晶之製造方法,其可在縮頸製程確實地除去軸狀差排。 According to the present invention, it is possible to provide a method for producing a single crystal which can surely remove a shaft-shaped row in a necking process.
1‧‧‧矽單結晶拉引裝置 1‧‧‧矽Single crystal pulling device
2‧‧‧矽單結晶 2‧‧‧矽Single crystal
2a‧‧‧頸部 2a‧‧‧ neck
2a1‧‧‧第一頸部 2a 1 ‧‧‧First neck
2a2‧‧‧第二頸部 2a 2 ‧‧‧second neck
2b‧‧‧肩部 2b‧‧‧Shoulder
2c‧‧‧體部 2c‧‧‧ Body
2d‧‧‧尾部 2d‧‧‧ tail
2s‧‧‧種結晶 2s‧‧ ‧ kinds of crystal
3‧‧‧矽融液 3‧‧‧矽融液
10‧‧‧反應室 10‧‧‧Reaction room
10A‧‧‧主反應室 10A‧‧‧Main Reaction Room
10B‧‧‧拉晶室 10B‧‧‧La crystal room
11‧‧‧隔熱材 11‧‧‧Insulation
12‧‧‧石英坩堝 12‧‧‧Quartz
13‧‧‧基座 13‧‧‧Base
14‧‧‧旋轉支持軸 14‧‧‧Rotary support shaft
15‧‧‧加熱器 15‧‧‧heater
16‧‧‧熱遮蔽體 16‧‧‧Hot shield
17‧‧‧拉引用的引線 17‧‧‧ cited lead
18‧‧‧引線捲取機構 18‧‧‧Lead take-up mechanism
D‧‧‧軸狀差排 D‧‧‧Axis difference
G‧‧‧間隔寬 G‧‧‧ interval width
r0‧‧‧單結晶的半徑 r 0 ‧‧‧ radius of single crystal
r1‧‧‧軸狀差排的徑向的位置 r 1 ‧‧‧ radial position of the shaft
r2‧‧‧單結晶的半徑 r 2 ‧‧‧ radius of single crystal
S1‧‧‧單結晶的外周面 S 1 ‧‧‧Single crystal outer surface
S2‧‧‧固液界面 S 2 ‧‧‧ solid-liquid interface
S101‧‧‧觸液製程 S101‧‧‧Liquid process
S102‧‧‧縮頸製程 S102‧‧‧Necking process
S103‧‧‧肩部培育製程 S103‧‧‧Shoulder cultivation process
S104‧‧‧體部培育製程 S104‧‧‧ Body cultivation process
S105‧‧‧尾部培育製程 S105‧‧‧Tail cultivation process
S11‧‧‧第一步驟 S11‧‧‧ first step
S12‧‧‧第二步驟 S12‧‧‧ second step
θ1‧‧‧固液界面角度 θ 1 ‧‧‧ solid-liquid interface angle
θ2‧‧‧結晶增徑角度 θ 2 ‧‧ crystallization angle increase angle
【第1圖】第1圖是一示意剖面圖,顯示矽單結晶拉引裝置1的結構。 [Fig. 1] Fig. 1 is a schematic cross-sectional view showing the structure of a single crystal pulling device 1.
【第2圖】第2圖是一流程圖,顯示矽單結晶的培育製程。 [Fig. 2] Fig. 2 is a flow chart showing the cultivation process of the single crystal.
【第3圖】第3圖是一示意剖面圖,顯示矽單結晶錠的形狀。 [Fig. 3] Fig. 3 is a schematic cross-sectional view showing the shape of a single crystal ingot.
【第4圖】第4圖是一模式圖,顯示在縮頸製程的單結晶的成長過程。 [Fig. 4] Fig. 4 is a schematic view showing the growth of a single crystal in the necking process.
【第5圖】第5圖是一流程圖,用以說明縮頸製程。 [Fig. 5] Fig. 5 is a flow chart for explaining the necking process.
【第6圖】第6圖是一模式圖,顯示單結晶的頸部的剖面形狀與頸部內的軸狀差排的位置的關係。 Fig. 6 is a schematic view showing the relationship between the cross-sectional shape of the neck of the single crystal and the position of the axial dislocation in the neck.
以下,一邊參照所附圖式,一邊針對本發明的較佳實施形態作說明。 Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings.
第1圖是一示意剖面圖,顯示矽單結晶拉引裝置1的結構。 Fig. 1 is a schematic cross-sectional view showing the structure of a single crystal pulling device 1.
如第1圖所示,矽單結晶拉引裝置1具有:反應室(chamber)10;隔熱材11,配置在反應室10的內側;基座(susceptor)13,支持收容於反應室10內的石英坩堝12;旋轉支 持軸14,支持基座13而使其可升降;加熱器15,以圍繞基座13的周圍的樣態配置;大致倒圓錐台形狀的熱遮蔽體16,配置於基座13的上方;單結晶拉引用的引線(wire)17,在基座13的上方且與旋轉支持軸14同軸狀地配置;以及引線捲取機構18,配置於反應室10的上方。 As shown in Fig. 1, the single crystal pulling device 1 has a reaction chamber 10, a heat insulating material 11 disposed inside the reaction chamber 10, and a susceptor 13 supported in the reaction chamber 10. Quartz crucible 12; rotating branch The shaft 14 is supported to support the base 13 so as to be movable up and down; the heater 15 is disposed around the periphery of the base 13; and the heat shield 16 having a substantially inverted truncated cone shape is disposed above the base 13; A wire 17 referred to by the crystal pulling is disposed coaxially with the rotation support shaft 14 above the susceptor 13 and a lead winding mechanism 18 disposed above the reaction chamber 10.
反應室10是由主反應室10A與拉晶室10B構成,拉晶室10B連結於主反應室10A的上部開口,上述的石英坩堝12、基座13、旋轉支持軸14、加熱器15及熱遮蔽體16是設在主反應室10A內。熱遮蔽體16是以圍繞培育中的矽單結晶2的樣態而設於矽融液3的上方。引線捲取機構18是配置於拉晶室10B的上方,引線17是從引線捲取機構18通過拉晶室10B內而向下方延伸,引線17的前端部通達主反應室10A的內部空間。在第1圖,是顯示以引線17吊掛培育當中的矽單結晶2的狀態。 The reaction chamber 10 is composed of a main reaction chamber 10A and a crystal pulling chamber 10B. The crystal pulling chamber 10B is connected to an upper opening of the main reaction chamber 10A. The quartz crucible 12, the susceptor 13, the rotating support shaft 14, the heater 15, and the heat are provided. The shielding body 16 is provided in the main reaction chamber 10A. The heat shielding body 16 is provided above the mash liquid 3 in a state of surrounding the singular crystal 2 in the cultivation. The lead wire take-up mechanism 18 is disposed above the crystal pulling chamber 10B, and the lead wire 17 extends downward from the lead wire take-up mechanism 18 through the inside of the crystal pulling chamber 10B, and the leading end portion of the lead wire 17 passes through the internal space of the main reaction chamber 10A. In the first drawing, the state in which the single crystal 2 in the cultivation is hung by the lead wire 17 is shown.
在矽單結晶的拉引步驟,首先在基座13內設置石英坩堝12,在石英坩堝12內充填矽原料,經由種晶夾將種結晶安裝於引線17的前端部。接下來以加熱器15加熱矽原料而生成矽融液3,使種結晶降下而接觸矽融液3。其後,藉由一邊分別旋轉種結晶及石英坩堝12、一邊使種結晶緩緩上升,成長大致圓柱狀的矽單結晶2。此時,矽單結晶2的直徑,是藉由控制其拉引速度、加熱器15的功率等而控制。 In the drawing step of the single crystal, first, a quartz crucible 12 is placed in the susceptor 13, and the crucible material is filled in the quartz crucible 12, and the seed crystal is attached to the front end portion of the lead wire 17 via the seed crystal clip. Next, the crucible material is heated by the heater 15 to form the crucible liquid 3, and the seed crystal is lowered to contact the crucible liquid 3. Thereafter, the seed crystals are gradually raised while rotating the seed crystal and the quartz crucible 12, respectively, and the substantially single crystal monocrystal 2 is grown. At this time, the diameter of the single crystal 2 is controlled by controlling the drawing speed, the power of the heater 15, and the like.
第2圖是一流程圖,顯示矽單結晶的培育製程。又,第3圖是一示意剖面圖,顯示矽單結晶錠的形狀。 Figure 2 is a flow chart showing the cultivation process for single crystals. Further, Fig. 3 is a schematic cross-sectional view showing the shape of a single crystal ingot.
如第2及3圖所示,在矽單結晶2的培育,是依序實施:觸液製程(S101),使種結晶接觸矽融液;縮頸製程(S102), 形成已將結晶直徑變細的頸部2a;肩部培育製程(S103),將結晶直徑加寬為圓錐狀而形成肩部2b;體部培育製程(S104),在單結晶已成長至規定的直徑的時間點,以固定的直徑持續拉引而形成體部2c;以及尾部培育製程(S105),在拉引終了時將直徑變細,最終與液面截斷。藉由以上,完成具有頸部2a、肩部2b、體部2c及尾部2d的矽單結晶錠。 As shown in the second and third figures, the cultivation of the single crystal 2 is carried out in sequence: a liquid contact process (S101), the seed crystal is brought into contact with the crucible melt; and the necking process (S102), Forming a neck portion 2a having a reduced crystal diameter; a shoulder cultivation process (S103), widening the crystal diameter into a conical shape to form a shoulder portion 2b; and a body cultivation process (S104), in which the single crystal has grown to a predetermined value At the time point of the diameter, the body portion 2c is continuously pulled at a fixed diameter; and the tail cultivation process (S105) is made to narrow the diameter at the end of the drawing, and finally cut off with the liquid surface. By the above, a single crystal ingot having the neck portion 2a, the shoulder portion 2b, the body portion 2c, and the tail portion 2d is completed.
接下來,針對縮頸製程作說明。縮頸製程是在培育矽單結晶時將直徑細化,除去矽種結晶在接觸矽融液時導入的差排(熱衝擊差排、錯位差排(misfit dislocation))的步驟。 Next, explain the necking process. The necking process is a step of refining the diameter when cultivating the single crystal, and removing the difference (thermal shock difference row, misfit dislocation) introduced by the seed crystal when it contacts the mash.
觸液時導入的差排之中,在結晶拉引方向延伸、以達斯縮頸法等單純變化結晶直徑仍無法除去者稱為軸狀差排。由於軸狀差排是直到縮頸製程、肩部培育製程以及體部培育製程,會在結晶的成長方向連續地存在,在完成晶圓製造時,會侷限地存在於各晶圓的特定區域。另外,軸狀差排是難以藉由如達斯縮頸法的擴徑、縮徑、將頸部的長度設為一定長度以上等在形成頸部時使用的習知一般性的手法而除去。然而,在本實施形態,如以下所示將縮頸製程分成二個步驟,在第一步驟除去主要的滑移差排,在第二步驟除去軸狀差排,藉此可以謀求頸部的無差排化。 Among the difference rows introduced during the liquid contact, the crystal growth is extended in the direction of the crystal pulling, and the crystal diameter is not removed by a simple change such as the Darth necking method. Since the axial difference is until the necking process, the shoulder cultivating process, and the body cultivating process, it will continuously exist in the growth direction of the crystal, and will be limited to a specific area of each wafer when the wafer fabrication is completed. Further, the axially-shaped row is difficult to remove by a conventional method of forming a neck portion by expanding the diameter, reducing the diameter, and lengthening the neck portion by a length such as a length of the neck. However, in the present embodiment, the necking process is divided into two steps as shown below, the main slip row is removed in the first step, and the shaft row is removed in the second step, whereby the neck can be eliminated. Poorly discharged.
第4圖是一模式圖,顯示在縮頸製程的單結晶的成長過程。又,第5圖是一流程圖,用以說明縮頸製程。 Figure 4 is a schematic diagram showing the growth of a single crystal in a necking process. Further, Fig. 5 is a flow chart for explaining the necking process.
在單結晶的培育,首先使種結晶2s接觸矽融液3(第4圖(a))。此時,在種結晶2s,包含軸狀差排的多個差排被導入(第4圖(b))。其後,為了除去差排而進行縮頸製程(第4圖 (c)~第4圖(f))。 In the cultivation of a single crystal, the seed crystal 2s is first contacted with the mash 3 (Fig. 4(a)). At this time, in the seed crystal 2s, a plurality of rows including the axial difference row are introduced (Fig. 4(b)). Thereafter, the necking process is performed in order to remove the difference row (Fig. 4) (c) ~ Figure 4 (f)).
如第5圖所示,根據本實施形態的縮頸製程,是以除去軸狀差排以外的主要的差排的第一步驟S11與除去軸狀差排的第二步驟S12構成。在第4圖,第4圖(c)及(d)是顯示第一步驟S11,第4圖(e)及(f)是顯示第二步驟S12。 As shown in Fig. 5, the necking process according to the present embodiment is constituted by a first step S11 of removing the main difference row other than the axial difference row and a second step S12 of removing the axial difference row. In Fig. 4, Figs. 4(c) and (d) show the first step S11, and Figs. 4(e) and (f) show the second step S12.
在第一步驟S11,藉由以相對快的拉引速度拉引種結晶2s,培育具有細結晶直徑的第一頸部2a1(請參照第4圖(c)、(d))。第一頸部2a1的目標直徑是以4~7mm為佳。藉由如此將結晶直徑細化至4~7mm程度,可以除去從種結晶2s繼續拉晶後的單結晶中的主要的差排。 In the first step S11, the first neck portion 2a 1 having a fine crystal diameter is grown by pulling the seed crystal 2s at a relatively fast drawing speed (refer to Figs. 4(c) and (d)). The target diameter of the first neck portion 2a 1 is preferably 4 to 7 mm. By refining the crystal diameter to about 4 to 7 mm in this manner, it is possible to remove the main difference between the single crystals which continue to be crystallized from the seed crystal 2s.
在第一步驟S11的拉引速度是以3~5mm/min為佳。拉引速度快時,與單結晶的外周部比較,中心部的冷卻被加快,因此固液界面形狀成為上凸。第一頸部2a1的長度是以限制在200mm以下為佳。這是因為固液界面形狀為上凸時,由於在對固液界面垂直方向進展的軸狀差排會移動至單結晶的中心方向,若使第一頸部2a1過長則軸狀差排會完全移動至中心軸上,就變得無法在第二步驟S12除去軸狀差排。 The pulling speed in the first step S11 is preferably 3 to 5 mm/min. When the pulling speed is fast, the cooling of the center portion is accelerated as compared with the outer peripheral portion of the single crystal, and thus the shape of the solid-liquid interface becomes convex. The length of the first neck portion 2a 1 is preferably limited to 200 mm or less. This is because when the shape of the solid-liquid interface is convex, the axial difference in the vertical direction of the solid-liquid interface moves to the center direction of the single crystal, and if the first neck 2a 1 is too long, the axial difference is arranged. When it is completely moved to the center axis, it becomes impossible to remove the shaft-shaped row in the second step S12.
在第二步驟S12,以比第一步驟S11相對慢的拉引速度拉引種結晶2s,控制使固液界面形狀成為下凸(請參照第4圖(e)、(f))。另外在第二步驟S12,一邊控制拉引條件而使固液界面角度成為大於結晶增徑角度,一邊培育第二頸部2a2。在固液界面角度大於結晶增徑角度時,使與結晶成長一起向徑向的外側移動的軸狀差排趕上結晶直徑的增加,可以將軸狀差排排除至單結晶的外側。 In the second step S12, the seed crystal 2s is pulled at a pulling speed which is relatively slower than the first step S11, and the solid-liquid interface shape is controlled to be convex (refer to Figs. 4(e) and 4(f)). Further, in the second step S12, the second neck portion 2a 2 is cultivated while controlling the pulling condition so that the solid-liquid interface angle becomes larger than the crystal diameter increasing angle. When the solid-liquid interface angle is larger than the crystal diameter increasing angle, the axial difference that moves toward the outside in the radial direction together with the crystal growth increases the crystal diameter, and the axial difference can be excluded to the outside of the single crystal.
在此,固液界面角度,是指顯示固液界面相對於水平面傾斜了多少的角度;結晶增徑角度是指結晶剖面的傾斜角度,顯示單結晶的外周藉由結晶直徑的增加相對於中心軸傾斜了多少。將第二步驟開始時的結晶直徑設為R1、將第二步驟終了時的結晶直徑及結晶長度分別設為R2及L時,將結晶增徑角度定義為arctan{(R2-R1)/2L}。 Here, the solid-liquid interface angle refers to an angle indicating how much the solid-liquid interface is inclined with respect to the horizontal plane; the crystal diameter increasing angle refers to the inclination angle of the crystal cross-section, and shows that the outer circumference of the single crystal is increased relative to the central axis by the crystal diameter How much is tilted. When the crystal diameter at the start of the second step is R 1 and the crystal diameter and crystal length at the end of the second step are R 2 and L, respectively, the crystal diameter increase angle is defined as arctan {(R 2 -R 1 ) )/2L}.
在本實施形態,以固液界面角度為4~8度為佳。固液界面角度若為此範圍內,可以確實地除去軸狀差排。為了使固液界面角度為4~8度,例如將拉引速度設為1.5~4.5mm/min、將坩鍋的上升速度設為1mm/min即可。另外,第二頸部2a2的目標直徑是以設為7~11.5mm為佳。 In the present embodiment, the solid-liquid interface angle is preferably 4 to 8 degrees. If the angle of the solid-liquid interface is within this range, the axial difference row can be surely removed. In order to make the solid-liquid interface angle 4 to 8 degrees, for example, the pulling speed is set to 1.5 to 4.5 mm/min, and the rising speed of the crucible is set to 1 mm/min. Further, the target diameter of the second neck portion 2a 2 is preferably set to 7 to 11.5 mm.
另外在第二步驟S12,是以縮小從矽融液3的液面到熱遮蔽體16(請參考第1圖)的距離(間隔寬G)為佳,以設為80mm以下為特佳。這是因為若將間隔寬G窄化則成為徐冷條件,來自加熱器15的輻射熱被遮蔽,單結晶變得容易冷卻。如此抑制輻射熱的影響,由於與矽單結晶的中心部比較,外周部的冷卻被加快,可以強化使固液界面形狀成為下凸的傾向。相反地,在第一步驟S11,藉由將間隔寬G設定得比第二步驟S12時還大,可以強化使固液界面形狀成為上凸的傾向,可以促進軸狀差排的排除。 Further, in the second step S12, it is preferable to reduce the distance (interval width G) from the liquid surface of the mash liquid 3 to the heat shielding body 16 (refer to FIG. 1), and it is particularly preferable to set it as 80 mm or less. This is because if the gap width G is narrowed, it becomes a cold-cold condition, and the radiant heat from the heater 15 is blocked, and the single crystal is easily cooled. By suppressing the influence of the radiant heat as described above, the cooling of the outer peripheral portion is accelerated as compared with the central portion of the single crystal, and the solid-liquid interface shape tends to be convex. Conversely, in the first step S11, by setting the gap width G larger than that in the second step S12, it is possible to enhance the tendency of the solid-liquid interface shape to be convex, and it is possible to promote the elimination of the axial gap.
固液界面形狀,是在結晶直徑隨著結晶成長而漸次變粗時成為下凸。此時,顯示單結晶的變粗情況的結晶增徑角度θ2比固液界面角度θ1小是必要的。這是因為若單結晶急遽變粗、結晶增徑角度θ2變得過大,相對於軸狀差排向單結晶的 徑向的外側進展的速度,單結晶的直徑的增加速度會過快,因此無法使軸狀差排追出至單結晶的外側。 The shape of the solid-liquid interface is a downward convexity when the crystal diameter gradually becomes coarse as the crystal grows. At this time, it is necessary to show that the crystal sharpening angle θ 2 of the single crystal is coarser than the solid-liquid interface angle θ 1 . This is because if the single crystal is sharply thickened and the crystal diameter increasing angle θ 2 is excessively large, the rate of increase in the diameter of the single crystal is too fast with respect to the speed at which the axial difference is discharged to the outside of the radial direction of the single crystal. It is impossible to chase the axial difference to the outside of the single crystal.
第6圖是一模式圖,顯示單結晶2的頸部2a的剖面形狀與頸部2a內的軸狀差排的位置的關係。 Fig. 6 is a schematic view showing the relationship between the cross-sectional shape of the neck portion 2a of the single crystal 2 and the position of the axial difference in the neck portion 2a.
如第6圖所示,設為在第二步驟S12的開始時軸狀差排D存在於單結晶2的中心(r=0),將此位置設為圓筒座標系的原點。在第二步驟S12,固液界面S2為下凸形狀,將其傾斜角度設為固液界面角度θ1時,從原點到在結晶長度L的位置的軸狀差排D的徑向的移動位置r1成為r1=Ltanθ1。又將在原點的單結晶2的半徑設為r0,在單結晶2的半徑隨著從原點成長到結晶長度L而增加了△r時,結晶增徑角度θ2成為tanθ2=△r/L,單結晶2的半徑r2成為r2=r0+△r=r0+Ltanθ2。 As shown in Fig. 6, it is assumed that the axial displacement row D exists at the center of the single crystal 2 (r = 0) at the start of the second step S12, and this position is the origin of the cylindrical coordinate system. In the second step S12, the solid-liquid interface S 2 has a downward convex shape, and when the inclination angle thereof is the solid-liquid interface angle θ 1 , the radial difference from the origin to the axial displacement row D at the position of the crystal length L is radial. shift position becomes r 1 r 1 = Ltanθ 1. Further, the radius of the single crystal 2 at the origin is r 0 , and when the radius of the single crystal 2 increases by Δr as it grows from the origin to the crystal length L, the crystal diameter increasing angle θ 2 becomes tan θ 2 = Δr / L, 2 single crystal radius r 2 be r 2 = r 0 + △ r = r 0 + Ltanθ 2.
為了使軸狀差排D隨著結晶成長移動至徑向的外側而可以追過單結晶2的外周面S1的外側,成為r1>r2是必要的。亦即,Ltanθ1>r0+Ltanθ2是必要的。 In order to move the axial displacement row D to the outer side in the radial direction as the crystal grows, it is possible to trace the outer side of the outer peripheral surface S 1 of the single crystal 2, and it is necessary that r 1 >r 2 . That is, Ltan θ 1 > r 0 + Ltan θ 2 is necessary.
例如,在第二步驟S12的開始時的單結晶2的半徑r0=2.5mm(直徑5mm)、固液界面角度θ1=4度、結晶增徑角度θ2=0(未增徑)時,在結晶長度為35.7mm以上,軸狀差排D會追過單結晶2的外周面S1的外側而消滅。 For example, when the radius r 0 of the single crystal 2 at the start of the second step S12 is 2.5 mm (diameter: 5 mm), the solid-liquid interface angle θ 1 = 4 degrees, and the crystal diameter increasing angle θ 2 =0 (not increasing the diameter) , a length of 35.7mm or more in the crystal, dislocation D-shaped shaft can overtake the outer peripheral surface S 2 of the outer single crystal 1 extinguished.
另外,在結晶長度L增加150mm而結晶直徑從5mm增加到11.5mm時,成為tanθ2=(11.5-5)/(2×150)=0.022(結晶增徑角度θ2≒1.26度)。因此,例如在結晶增徑角度θ2=1.26度時,為了將軸狀差排D排除至單結晶2的外周面S1的外側,必要的結晶長度L如以下。 Further, the increase in the crystal length L is crystallized 150mm 5mm diameter increased from 11.5mm to become tanθ 2 = (11.5-5) / ( 2 × 150) = 0.022 ( crystal diameter by an angle θ 2 ≒ 1.26 degrees). Therefore, for example, when the crystal diameter increasing angle θ 2 = 1.26 degrees, in order to exclude the axial row D from the outer side surface S 1 of the single crystal 2, the necessary crystal length L is as follows.
L>5.75/(0.07-0.022)=119.8(mm) L>5.75/(0.07-0.022)=119.8(mm)
亦即,只要使第二頸部2a2的結晶長度L為120mm以上,可以使軸狀差排D追出單結晶的外側而消滅。不過在實際上,考慮固液界面角度θ1的誤差等,較好為成長得比理論上的結晶長度L還長30~50mm,以第二頸部2a2的結晶長度L為150mm以上為佳。 That is, as long as the crystallized neck 2a 2 of the second length L of 120mm or more, the outer axial dislocation single crystal D out chase extinguished. However, in practice, considering the error of the solid-liquid interface angle θ 1 , it is preferable to grow 30 to 50 mm longer than the theoretical crystal length L, and it is preferable that the crystal length L of the second neck portion 2a 2 is 150 mm or more. .
在縮頸製程S102的第二步驟S12終了後,以不再度將單結晶2的直徑變細,直接轉而進行肩部培育製程S103為佳。這是因為若再度將單結晶2的直徑變細,已特意移動到外周面S1附近的軸狀差排D會回到中心方向,而使進行到此的縮頸製程變為白費。由於認為即使藉由第二步驟S12無法從單結晶2中排除軸狀差排而仍存在於外周面S1附近,會有在轉而進行肩部培育製程S103後馬上移動到外周面S1的外側而排除的可能性,即使萬一未排除,還有製品加工時藉由外周研削而除去的可能性。因此,在第二步驟S12終了後,以直接轉而進行肩部培育製程S103為佳。 After the end of the second step S12 of the necking process S102, it is preferable to make the diameter of the single crystal 2 thinner and to directly perform the shoulder growing process S103. This is because if the diameter of the single crystal 2 is again made fine, the axially-displaced row D which has been intentionally moved to the vicinity of the outer peripheral surface S 1 is returned to the center direction, and the necking process to this point is in vain. Since the step S12 that even by a second single crystal can not be excluded from the second shaft-shaped dislocations still present in the vicinity of the outer peripheral surface S 1, in turn, will be moved to the shoulder incubated process S103 immediately after the outer peripheral surface S 1 of The possibility of exclusion from the outside is possible, even if it is not excluded, and there is a possibility that it is removed by peripheral grinding during the processing of the product. Therefore, after the end of the second step S12, it is preferable to perform the shoulder cultivation process S103 directly.
如以上的說明,根據本實施形態的矽單結晶的製造方法,其為了在使種結晶2s接觸矽融液3後除去差排的縮頸製程S102具有第一步驟與第二步驟,上述第一步驟是一邊將單結晶的直徑變細而使固液界面形狀成為上凸、一邊作培育,上述第二步驟是一邊增加單結晶的直徑而使固液界面形狀成為下凸且使固液界面角度θ1成為大於結晶增徑角度θ2、一邊培育單結晶,因此可以除去單結晶中的軸狀差排,而可以謀求在培育肩部前使單結晶無差排化。 As described above, according to the method for producing a single crystal of the present embodiment, the first step and the second step are performed in order to remove the difference between the seed crystals 2s and the necking process S102. The step is to make the diameter of the single crystal thinner and to make the solid-liquid interface shape convex and to cultivate. The second step is to increase the diameter of the single crystal to make the solid-liquid interface shape convex and to make the solid-liquid interface angle Since θ 1 is larger than the crystal diameter increasing angle θ 2 and the single crystal is grown, it is possible to remove the axial difference in the single crystal, and it is possible to make the single crystal undifferentiated before the shoulder is grown.
以上,已針對本發明的較佳實施形態作說明,但是本發明未受限於上述的實施形態,可以在不脫離本發明的主旨的範圍作各種變更,那些變更當然亦包含於本發明的範圍內。 The preferred embodiments of the present invention have been described above, but the present invention is not limited to the embodiments described above, and various modifications may be made without departing from the spirit and scope of the invention. Inside.
例如在上述實施形態,除了拉引速度外還變更間隔寬,會更容易地變化固液界面形狀;此外亦可變化加熱器功率而取代變化間隔寬,亦可變化其他的拉引條件。 For example, in the above embodiment, in addition to the pulling speed, the interval is widened, and the solid-liquid interface shape is more easily changed. Alternatively, the heater power may be changed instead of the variation interval, and other drawing conditions may be changed.
S11‧‧‧第一步驟 S11‧‧‧ first step
S12‧‧‧第二步驟 S12‧‧‧ second step
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