200916614 六、發明說明： 【發明所屬之技術領域】 本發明係關於用施加磁場之柴氏法（Megnetic f丨别 - 卿1ied —ski Method ;以下稱為MCZ法）之石夕單晶拉 - 起方法。 【先前技術】 作為石夕單晶之製造方法，基於可比較料地制大口徑且高 〇純度化之無移位或結晶缺陷極少之單晶，cz法及施加磁場之 MCZ法受到廣泛地使用。 於用cz法之秒單晶之製造中，例如，於圖2所示般之單晶 拉起裝置中，使由石夕單晶所構成之種晶1於室9内藉由加熱器 7及保溫體8所加熱保溫之熱區射，與填充於石英内 之原料石夕熔融液5接觸後，於邊旋轉下緩緩拉起，形成頸部2 後’形成結晶徑徐徐增加之肩部3，接著再形成怪定口徑之直 〇筒部（straight body)，經過此等形成步驟而生切單晶4。 於上述CZ法中，為排除以往於頸部之起因於種晶之移位與 因接觸魏融液時之熱衝擊所導入之移位，係僅形成為限於較 細之直徑約3mm的程度。 然而，近年來，隨著半導體裝置之高錢化、成本之降低、 =效率之提高’須要求用以得到大口徑之晶圓之高重量的矽 早曰曰之製造’如以往之小徑的頸部無法承受單晶錠之高重量而 曰折斷’致有導致發生單晶鍵之落下等重大事故之虞。 97129779 200916614 針對此點，例如，於日本專利特開平9—249842號公報（專利 文獻1)中記載有.使頸部形成時之種晶之旋轉速度定為較直 筒部形成時低之1〜12rpm，可抑制隨種晶旋轉所產生之自然對 流’使結晶生長界面之形狀更向下凸出，於頸徑不大緊縮之下 亦可排除移位。 又，於日本專利特開2004-83320號公報（專利文獻2)中記 載有：於使精形成步驟之賴旋轉速度定為_以下之同 時:於水平方向絲〇. !特雜（teslaMT之爾，於移往 增k步驟之段將該磁場停止，藉此可防止移位。 再者’於曰本專利特開平7—3〇_號公報（專利文獻3)t 記載有··使種晶所延續之錐狀之縮減部之長度定為種晶尺和 2· 5〜15倍’使此縮減部所延續之大雜定徑之緊縮部之射 =種晶尺寸之請9倍，變動寬度定為_以下, 場^之長度定為細〜6GGmm ’並施加_〜_高斯之水平超 載有.作ΓΓ 修199384顿專敝獻4)中1 之_料減之所謂括號形狀之頸部，藉由使單位1 =.聽!成為0.5_以上，可抑制移位發生。 度：晶城1中所記载般，於形成― 生長界面之θ ^，即令使結晶旋轉改變之情況，於結^ 反而於排/ 變化。而改變拉_ m X有效果，雖是如此，於形成上述㈣細心 200916614 頸部中，藉由向下凸出程度之抑制，於排除移位之效果甚小。 又’如上述專利文獻2所記_方法般，若使水平磁場之磁 場強度定為〇. i特斯拉以下，於原料石夕溶融液量較多之情況， 並無法充分_自朗敍細伴生之獅液溫度變動。 又於上述專利文獻3所記載之方法中，設置緊縮部對移位 抑制雖有效果，惟，形成上述般長的頸部，作業時間長，實用 上並非理想。又，緊縮部之直徑變動幅係意味著該表面之凹凸 幅，防止因應力集中所致之塑性變形，並僅為顯示得到足夠的 強度而已。 又’於上料散獻4所記載之方法巾，驗之變化量若增 大，於__部外表面之溫度梯度會變大，致移位密度^ 加’會有反而難以排除移位之情形。尤其，於町法中，於^ Γ液職加財卩歡航，稱為輪圈（_〇_之炫融液 表面的定期性變動會明顯地呈現，使頸徑之變化量變得過大， 致難以達成無移位化。 【發明内容】 本發明係依據下述發躺完成者，其為：為早期排除 之移位’不僅要使拉起之單晶的固液界面向下凸出之外，_ 動㈣於狀條件之範_進行頸部之生長是有效的。 亦即，本發明之目的在於，提供―種在使用之石夕單曰 之生長中，使馳之變鱗抑齡㈣範_， 二 頸部之移位_單晶拉起方法。 干捕除於 97129779 200916614 本發明之矽單晶拉起方法，係使種晶與原料矽熔融液接觸後 將其拉起’生長辆部後，使其增徑Μ長成既定的結晶徑之 單曰曰者’其特徵為’係使t述頸徑增減以生長該頸冑，其間， 於以增減之前述職之_的折曲關之義差除以前述折 曲‘.、、占間之4長之值作為麵變動率時，前述雜變動率係定為 〇.〇5以上、未滿0 5。 藉由使，員L之變動如上述般地抑制以生長頸部而可早期排 除移位。 車乂佳者為’於别述頸部生長之時，於職壁面施加剛高斯 以上之邊端磁場（cusp magnetic field)，將結晶旋轉速度定 為lrPm以上、15rpm以下，將與前述結晶以相反方向旋轉之 掛鋼旋轉速度定為大於8rPm、15rpm以下。 〇 或者，較佳者為，於前述頸部生長之時，於掛鋼壁面施加 細南斯以上之水平磁場，將結晶旋轉速度定為lrpm以上、 以下’將與前述結晶以相反方向旋轉之购旋轉速度定 為〇.5rpm以上、3rpm以下。 ^此磁場施加條件下，透過生長頸部，則可抑制影響頸根 、周期下之溫度變動，可有效抑制頸徑的變動。 如上述般，依據本發明 石夕單日吐旦“ 早日日拉起方法，於使用CZ法之 早曰曰生長中’抑制頸徑之變動率，可早期排_部中之移位。 因而，依據本㈣之拉起方法，可_部 即使因頸部 97129779 200916614 低。 【實施方式] 以下，就本發明更詳細地做說明。 本毛明之秒早晶拉起方法，係使種晶與原料贿融液接觸後 拉起，生長朗部後’使其增徑而生長成既定的結晶徑之 早晶者；其特徵為，係使前述頸徑增減以生長該頸部 頸徑變動率係定為（^以上、未滿0 5。 本發明中所謂之難變動率，係關於圖1所示之進行辦減的 頸徑—，以此頸徑之鄰接的折_…p2間之增大觀^與 細J、如k B的頸控差（A_B)除以前述折曲點p卜p2間之頭長[ 頒k於增加或減少時，最大應力會於頸料圍發生，並若超 過移位抑制的界限時，移位密度會增加，致使於頸部中移奴 排除有困難。 C/ 也以k為佳’而實際上，因原料雜融液之溫度 ’交動而無法完全抑制頸徑之變動。 匕占柄明令’藉由使上述職變動率於0.05以上、 :二5之範圍内進行頸部生長，可早期排除移位，而可於短 時間内達成無移位化。 :使糊徑變動率抑制於〇.〇5以上、未滿〇.5，對頸部 Γ觸之捕魏崎表^溫«動（尤其是_徑較有影 曰之長週期之溫度魏）一_是纽的，於未施加磁場之 97129779 200916614 cz法或於邊端磁場巾之單晶喊巾，躲峨觀度在可安 定地拉起單晶的範圍内增大是有效的。 又，於溶融液量超過贿这之町法中，在一定的頭長之間， 欲控制前述驗變解於未滿0.05，於實務上有其困難。 如上述般’就抑觸馳有較大影響之較長週期的溫度變動 之考量，為抑制矽熔融液的熱對流之目的，於前述頸部生長 時’以於掛鋼壁施加刚高斯以上之邊端磁場為佳，此情況 下，掛鋼旋轉速度叹為大於8_、15rpm以下為佳。 於則述掛鍋壁之邊端磁場為未㉟100高斯之情況’無法得到 充分的抑制炼融液對流之效果。 又，於别述坩鍋旋轉速度為8rpm以下之情況，原料矽熔融 液表面之低溫部分（所謂之輪圈圖案的帶狀之低溫區域）會變 得顯著。此低溫部分，若橫越矽原料熔融液表面的中心之頸部 生長部分，則頸徑會變動，欲維持前述頸徑變動率於〇. 5以下 會有困難’致會有頸部太粗、或反之太細而斷裂之情形。 另一方面，於頸部生長時之坩鍋旋轉速度超過15rpm之情 況’於頸部生長後之肩部及直筒部之錄時，為抑制氧濃度， 通常係使_旋轉速度降低至下，惟，因於此急遽的 旋轉速度之變化’會導致級之發生，致結晶容㈣生移位化。 或者，於前述頸部生長時所之施加磁場方式亦可為水平磁 場，此情況，為使頸徑安定，並抑制原料矽熔融液之長週期的 溫度變動，較佳者為，將磁場強度定為2000高斯以上，且坩 97129779 9 200916614 鋼旋=速妓為G.5rpm以上、_以下。 ^述磁％強度為未滿·高斯之情況，藉由磁 之抑制不足，與磁場方向平行產生之低溫部^ ΠΡ生長部分，致頸徑變動，使抑制變動率於[ο以下 困難。 令 又，於水平磁場之情況，於掛鋼旋轉速度超過3rpm之情況， 原科石夕溶融液之溫度變動會變大，致頸徑不安定，使定徑部（直 f同部）之生長亦無法安定。因此，_旋轉速度以較小為佳， 惟就單晶生長效率之考量，以〇知以上為佳。 又，與前述_相反方向旋轉之結晶的旋轉速度，無論是於 施加邊端磁場或水平磁場任一者之情況，就安定地維持_之 考量，只要為1_以上皆可。惟，於頸部生長後之肩部、直 概生長中，為抑制變形必須降低結晶旋轉，於前述旋轉逮 度超過15_之情況，隨著急遽的條件變更，移位化之可能性 會增大，故不佳。 注 [實施例] 、以下’依據實施例，就本發明更具體地做說明，惟，本發明 並不因下述實施例而受限制。 [實施例1〜6、比較例1〜5] 於直徑24忖之石英稿内，填充原料石夕熔融液麵g，用 cz法單餘起裝置，⑽平均難麵4 5_之方式生長頸 部，生長成矽單晶。 97129779 10 200916614 ;生長顯部時’係分別定為表i之實施例卜6及比較例卜5 所π：!又的；ε兹場施加、掛銷旋轉速度、結晶旋轉速度及單晶拉 速度。 刀別對各彳_定最大頸錢料、與自開始生長位置至移位 排除之位置的長度。 將此等結果彙整於表1中。 ^ Χ ’磁場強度之败值，於邊端磁場之情況，係於賴壁面， 於水平购之情況，係於中心。頸徑制游標卡尺（vernier caliper)涓丨J定 〇 3 , ，自開始生長位置至移位排除之位置的長 X係藉由用選擇餘刻液之餘刻評價（依據JIS Η _9)之移 位的目視測定而判定。200916614 VI. Description of the Invention: [Technical Field to Be Invented by the Invention] The present invention relates to a singular single crystal pull-up using a magnetic field applying a magnetic field method (Megnetic f丨- 卿1ied-ski Method; hereinafter referred to as MCZ method) method. [Prior Art] As a method for producing a single crystal, the MCZ method in which the cz method and the applied magnetic field are widely used is based on a single crystal having a large diameter and a high purity and a non-displacement or crystal defect. . In the manufacture of a single crystal using the cz method, for example, in the single crystal pulling device shown in FIG. 2, the seed crystal 1 composed of the stone single crystal is used in the chamber 9 by the heater 7 and The heat-insulating body 8 is heated and insulated by the hot zone, and after being contacted with the raw material Xixi melt 5 filled in the quartz, it is slowly pulled up while rotating, and the neck 2 is formed to form a shoulder 3 which gradually increases in crystal diameter. Then, a straight body of a strange caliber is formed, and the single crystal 4 is cut through these forming steps. In the above-mentioned CZ method, in order to eliminate the displacement caused by the shift of the seed crystal due to the seed crystal and the thermal shock when the Wei Rong liquid is contacted, it is only limited to a thickness of about 3 mm. However, in recent years, with the increase in the cost of semiconductor devices, the reduction in cost, and the improvement in efficiency, 'there is a need to obtain a high-weight wafer for the production of large-diameter wafers, as in the past. The neck can not withstand the high weight of the single crystal ingot and the crucible breaks, causing a major accident such as the fall of the single crystal bond. In the case of the formation of the neck portion, the rotation speed of the seed crystal is set to be 1 to 12 rpm lower than that at the time of formation of the straight portion, as described in Japanese Laid-Open Patent Publication No. Hei 9-249842 (Patent Document 1). It can suppress the natural convection generated by the rotation of the seed crystals, so that the shape of the crystal growth interface is more convex downward, and the displacement can be excluded under the neck diameter. In Japanese Patent Laid-Open Publication No. 2004-83320 (Patent Document 2), it is described that the rotation speed of the fine forming step is set to be _ or less: in the horizontal direction, the wire is twisted. The magnetic field is stopped in the step of moving to the step of increasing k, thereby preventing the shifting. Further, the patent is disclosed in Japanese Patent Application Laid-Open No. Hei 7-3- No. (Patent Document 3) The length of the tapered portion of the continuation is set to be a seed crystal and 2·5 to 15 times'. The squeezing portion of the large sizing diameter continued by the reduction portion = 9 times the seed crystal size, the variation width Set to _ below, the length of the field ^ is set to fine ~ 6GGmm 'and the application of _ ~ _ Gauss level overload has. 修 repair 199384 敝 special offer 4) _ material minus the so-called bracket shape of the neck, By making the unit 1 =. listening! becomes 0.5_ or more, the shift can be suppressed. Degree: As described in Jingcheng 1, when θ ^ is formed at the "growth interface", the crystal rotation is changed, and the result is changed/disposed. However, it is effective to change the pull _ m X. However, in the formation of the above (4) careful heart of the 1616614 neck, the effect of eliminating the displacement is very small by suppressing the degree of downward bulging. Further, as in the method described in the above Patent Document 2, if the magnetic field strength of the horizontal magnetic field is set to be less than i. i Tesla, the amount of the molten solution in the raw material is not sufficient, and it is not sufficient. The temperature of the associated lion fluid changes. Further, in the method described in the above Patent Document 3, the tightening portion is provided to have an effect on the displacement suppression. However, the neck portion having the above-described length is formed, and the working time is long, which is not preferable in practical use. Further, the diameter variation of the constricted portion means the unevenness of the surface, preventing plastic deformation due to stress concentration, and obtaining sufficient strength only for display. In addition, the method towel described in the 4th article is distributed. If the amount of change is increased, the temperature gradient on the outer surface of the __ part will become larger, and the displacement density will increase. situation. In particular, in the town law, in the Γ Γ 职 加 加 卩 卩 , , , , , , , , , , ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( 定期 定期 定期 定期 定期 定期 定期 定期It is difficult to achieve no shifting. SUMMARY OF THE INVENTION The present invention is based on the following: a shift for early exclusion 'not only to make the solid-liquid interface of the pulled single crystal convex downward , _ moving (four) in the condition of the conditions _ to carry out the growth of the neck is effective. That is, the purpose of the present invention is to provide "the species in the use of the stone 曰 曰 曰 曰 曰 曰 驰 驰 驰 驰 ( ( ( ( ( ( ( ( ( ( ( Fan_, the displacement of the two necks_the method of pulling up the single crystal. Dry-catching in 97129779 200916614 The method of pulling up the single crystal of the invention is to pull the seed crystal into contact with the raw material 矽 melt and pull it up. After the ministry, the person who increases the diameter and grows into a predetermined crystal diameter is characterized by 'the characteristic that the neck diameter is increased or decreased to grow the neck, and in the meantime, the above-mentioned position is increased or decreased. The difference in the difference between the two is divided by the value of the above-mentioned flexion '. 〇 〇 以上 以上 以上 未 未 未 〇 〇 〇 〇 〇 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员 员The cusp magnetic field of the Gaussian or higher is applied to the working wall, and the rotational speed of the crystal is set to be lrPm or more and 15 rpm or less, and the rotational speed of the hanging steel rotating in the opposite direction to the crystal is set to be greater than 8 rPm and 15 rpm or less. 〇 or, preferably, when the neck is growing, a horizontal magnetic field of finer than the south is applied to the wall of the steel, and the rotational speed of the crystal is set to be above 1 rpm, and the following will rotate in the opposite direction to the crystal. The rotational speed of the purchase is set to 〇5 rpm or more and 3 rpm or less. ^ Under the application of the magnetic field, the growth of the neck portion can suppress the temperature fluctuations affecting the neck root and the cycle, and the neck diameter can be effectively suppressed. According to the present invention, the "Early day pulling method", in the early growth of the CZ method, suppresses the rate of change of the neck diameter, and can be displaced in the early stage. Therefore, according to the present (4) Pull up The method can be as low as the neck 97129779 200916614. [Embodiment] Hereinafter, the present invention will be described in more detail. The method of the second-crystal early pulling of the hair of the hair is to bring the seed crystal into contact with the brittle material of the raw material. a person who grows into a radiant part and grows into a predetermined crystal diameter; it is characterized in that the neck diameter is increased or decreased to increase the neck diameter variation rate of the neck (^ above, Less than 0. 5. The difficulty rate of change in the present invention is the neck diameter which is reduced as shown in Fig. 1, and the increase between the adjacent y... p2 of the neck diameter is as follows. The neck control difference (A_B) of k B is divided by the head length between the above-mentioned bending point p and p2 [When k is increased or decreased, the maximum stress will occur in the neck circumference, and if the limit of displacement suppression is exceeded, The shift density will increase, making it difficult to remove the slaves in the neck. C/ is also preferable to k. In fact, the change in the neck diameter cannot be completely suppressed due to the temperature of the raw material amalgam.匕 匕 明 ’ ’ 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 : The rate of change of the paste diameter is suppressed to 〇. 〇5 or more, less than 〇.5, and the catch of the neck is caught by the Weiqi table. The temperature is moderate (especially the temperature of the long period with a shadow) A _ is New, in the case of the 97129779 200916614 cz method without applying a magnetic field or the single-crystal shouting of the edge magnetic field towel, it is effective to increase the degree of hiding in the range in which the single crystal can be stably pulled. In addition, in the town method in which the amount of molten liquid exceeds that of bribes, it is difficult to control the above-mentioned test solution to be less than 0.05 between a certain head length. As described above, in order to suppress the temperature fluctuation of the longer period, which has a greater influence on the touch, the purpose of suppressing the thermal convection of the crucible melt is to apply a rigid Gauss or more to the steel wall during the growth of the neck. The magnetic field at the edge is better. In this case, the rotation speed of the hanging steel is preferably greater than 8_, 15 rpm or less. In the case where the magnetic field at the side of the wall of the hanging pot is not 35,100 gauss, the effect of sufficiently suppressing the convection of the smelting liquid cannot be obtained. Further, when the crucible rotation speed is 8 rpm or less, the low temperature portion of the surface of the raw material crucible (the band-like low temperature region of the so-called rim pattern) becomes remarkable. In the low temperature portion, if the neck portion of the center of the surface of the raw material melt is traversed, the neck diameter may fluctuate, and it may be difficult to maintain the neck diameter variation rate below 〇. 5 to cause the neck to be too thick. Or vice versa if it is too thin. On the other hand, in the case where the rotation speed of the crucible is more than 15 rpm at the time of neck growth, in order to suppress the oxygen concentration during the shoulder and the straight portion after neck growth, the _ rotation speed is usually lowered to the lower side. Because of this rapid change in the rotational speed 'will lead to the occurrence of the stage, resulting in the crystallization capacity (four) shifting. Alternatively, the magnetic field applied during the growth of the neck may be a horizontal magnetic field. In this case, in order to stabilize the neck diameter and suppress the temperature fluctuation of the long period of the raw material mash melt, it is preferable to set the magnetic field strength. It is 2000 gauss or more, and 坩97129779 9 200916614 steel rotation = speed 妓 is G. 5 rpm or more, _ below. When the magnetic % intensity is less than full and Gaussian, the magnetic field is insufficiently suppressed, and the low temperature portion is generated in parallel with the direction of the magnetic field, and the neck diameter is varied, so that the suppression of the variation rate is difficult. In addition, in the case of a horizontal magnetic field, when the rotation speed of the hanging steel exceeds 3 rpm, the temperature change of the original Shishi molten liquid becomes large, and the neck diameter is unstable, so that the diameter of the sizing portion (the straight portion is the same) It is also impossible to settle. Therefore, the _ rotation speed is preferably small, but it is preferable to consider the above single crystal growth efficiency. Further, the rotation speed of the crystal which is rotated in the opposite direction to the above-mentioned θ is stable regardless of whether or not the edge magnetic field or the horizontal magnetic field is applied, and may be 1 _ or more. However, in the shoulder and straight growth after neck growth, it is necessary to reduce the crystal rotation in order to suppress the deformation. In the case where the above-mentioned rotation catch exceeds 15 mm, the possibility of shifting increases with the rapid change of conditions. Big, so it is not good. [Embodiment] Hereinafter, the present invention will be more specifically described based on the embodiments, but the present invention is not limited by the following examples. [Examples 1 to 6 and Comparative Examples 1 to 5] In a quartz paper having a diameter of 24 Å, the raw material of the molten stone surface g was filled, and the neck was grown by the cz method single-remaining device and (10) the average difficult surface 4 5_ Part, growing into a single crystal. 97129779 10 200916614 ; When the growth part is grown, the system is determined as the example of Table i and the comparison example 5 is π:! again; ε field application, pin rotation speed, crystal rotation speed and single crystal pulling speed . The length of the knife is set to the maximum neck material and the position from the start of growth to the position where the displacement is excluded. These results are summarized in Table 1. ^ Χ ‘ The value of the magnetic field strength, in the case of the magnetic field at the edge, is tied to the wall, and at the level of purchase, it is at the center. The vernier caliper 涓丨J 〇 3 , , the long X from the starting position to the position where the displacement is excluded is evaluated by the remainder of the selection of the residual fluid (according to JIS Η _9) Determined by visual measurement.
Ci 97129779 11 200916614 [表1]Ci 97129779 11 200916614 [Table 1]
可知：於施加邊端磁場之情況丁 藉由在既定條件下拉起，頸徑變動率可抑制於⑽以上^未 滿〇. 5，此情況，確認可早期排除移位。 · 【圖式簡單說明】It can be seen that when the magnetic field at the edge is applied, the rate of change of the neck diameter can be suppressed to (10) or more and less than 5% when pulled down under predetermined conditions. In this case, it is confirmed that the displacement can be eliminated early. · [Simple description]
圖1為用以說明頸徑變動率之示音圖 【==:Γ裝置—生一 A、Β 頸徑 L 頸長 PI ' P2 折曲點 L 頸長 1 種晶 2 頸部 97129779 12 200916614 3 4 5 6 7 8 9 肩部 矽單晶 石夕溶融液 坩鍋 加熱器 保溫體 室Fig. 1 is a diagram showing the change rate of the neck diameter [==: Γ device - raw one A, 颈 neck diameter L neck length PI ' P2 bending point L neck length 1 seed crystal 2 neck 97129779 12 200916614 3 4 5 6 7 8 9 Shoulder 矽 矽 夕 夕 溶 molten pot 坩 pot heater insulation room
L 97129779 13L 97129779 13