TW202415817A - Single crystal pulling device and single crystal pulling method - Google Patents

Single crystal pulling device and single crystal pulling method Download PDF

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TW202415817A
TW202415817A TW112122510A TW112122510A TW202415817A TW 202415817 A TW202415817 A TW 202415817A TW 112122510 A TW112122510 A TW 112122510A TW 112122510 A TW112122510 A TW 112122510A TW 202415817 A TW202415817 A TW 202415817A
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single crystal
brightness
crucible
silicon melt
pin member
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坪田寛之
佐佐木智紀
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日商環球晶圓日本股份有限公司
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Abstract

在利用柴可拉斯基法提拉單晶矽時,精度較佳地控制輻射屏蔽的下端與矽融液之間的距離之間隙而培育單晶矽。單晶提拉裝置係具備:升降驅動部,係使坩堝升降;加熱器,係加熱坩堝;圓筒狀之輻射屏蔽,係配置於形成於坩堝內的矽融液的上方,且包圍提拉的單晶的周圍;光透過性之銷構件,係貫穿輻射屏蔽而配置於位於輻射屏蔽的前端側之平台面,以使下部位於矽融液側且上部位於輻射屏蔽的內周側;亮度檢測計,係檢測銷構件的亮度;以及控制器,係於所檢測的銷構件的亮度超過預定臨限值時判斷為銷構件的下端接觸於矽融液並停止坩堝的上升。When growing single crystal silicon using the Czochralski method, the gap between the lower end of the radiation shield and the silicon melt is controlled with high precision to grow single crystal silicon. The single crystal pulling device comprises: a lifting drive unit for lifting and lowering the crucible; a heater for heating the crucible; a cylindrical radiation shield arranged above the silicon melt formed in the crucible and surrounding the single crystal being pulled; a light-transmitting pin member penetrating the radiation shield and arranged on a platform surface located on the front end side of the radiation shield so that the lower part is located on the silicon melt side and the upper part is located on the inner circumference side of the radiation shield; a brightness detector for detecting the brightness of the pin member; and a controller for determining that the lower end of the pin member is in contact with the silicon melt and stops the lifting of the crucible when the detected brightness of the pin member exceeds a predetermined critical value.

Description

單晶提拉裝置以及單晶提拉方法Single crystal pulling device and single crystal pulling method

本發明係關於一種單晶提拉裝置以及單晶提拉方法,尤其關於一種利用柴可拉斯基法(Czochralski method)提拉單晶矽之單晶提拉裝置以及單晶提拉方法。The present invention relates to a single crystal pulling device and a single crystal pulling method, and more particularly to a single crystal pulling device and a single crystal pulling method for pulling single crystal silicon using the Czochralski method.

利用柴可拉斯基法(CZ法)培育單晶矽係以下述方式進行:如圖5所示將原料的多晶矽填充於設置於腔(chamber)50內的石英坩堝51,利用設於前述石英坩堝51的周圍之加熱器52將多晶矽加熱並熔融而成為矽融液M。 之後,將安裝於種夾具(seed chuck)的種晶(seed crystal)P(種(seed))浸漬於矽融液M,一邊將種夾具及石英坩堝51向相同方向或相反方向旋轉,一邊提拉種夾具,藉此於輻射屏蔽(radiation shield)53的內側培育單晶C。 The Czochralski method (CZ method) is used to grow single crystal silicon in the following manner: as shown in FIG. 5 , the raw material polycrystalline silicon is filled into a quartz crucible 51 disposed in a chamber 50, and the polycrystalline silicon is heated and melted into a silicon melt M by a heater 52 disposed around the aforementioned quartz crucible 51. Afterwards, the seed crystal P (seed) mounted on the seed chuck is immersed in the silicon melt M, and the seed chuck and the quartz crucible 51 are rotated in the same direction or in the opposite direction, while the seed chuck is pulled up, thereby growing a single crystal C on the inner side of the radiation shield 53.

雖然對利用此柴可拉斯基法培育單晶矽要求無缺陷單晶,然而能製造無缺陷單晶的條件係極為苛刻。作為此製造條件的一例,有提拉速度與溫度梯度的比例。 溫度梯度是指固液界面附近的單晶的高度方向之每單位長度的溫度變化,提拉速度是指提拉單晶的速度。在將提拉速度設為V且將溫度梯度設為G時,製造單晶時形成之缺陷係依照提拉速度V與溫度梯度G的比例(V/G)而敏感地產生變化。例如,若提拉速度V與溫度梯度G的比例(V/G)過大,則形成有空位型缺陷(空隙(void)缺陷);相反地,若提拉速度V與溫度梯度G的比例(V/G)過小,則形成有晶格間矽(interstitial silicon)型缺陷(差排環(dislocation loop))。 Although the growth of single crystal silicon using this Czochralski method requires a defect-free single crystal, the conditions for producing a defect-free single crystal are extremely demanding. As an example of this production condition, there is the ratio of the pulling rate and the temperature gradient. The temperature gradient refers to the temperature change per unit length in the height direction of the single crystal near the solid-liquid interface, and the pulling rate refers to the speed of pulling the single crystal. When the pulling rate is set to V and the temperature gradient is set to G, the defects formed when producing the single crystal change sensitively according to the ratio (V/G) of the pulling rate V and the temperature gradient G. For example, if the ratio (V/G) of the pulling rate V and the temperature gradient G is too large, a vacancy type defect (void defect) is formed; on the contrary, if the ratio (V/G) of the pulling rate V and the temperature gradient G is too small, an interstitial silicon type defect (dislocation loop) is formed.

因此,為了得到品質穩定的單晶,需要高精度地控制提拉速度V與溫度梯度G的比例(V/G)。此外,由於提拉速度V係能夠進行機械性的精密控制,因此為了兼顧穩定的結晶品質與計劃生產,一般進行單晶之製造方法,該單晶之製造方法係進行將提拉速度V設為固定的控制。Therefore, in order to obtain a single crystal with stable quality, it is necessary to control the ratio (V/G) of the pulling speed V and the temperature gradient G with high precision. In addition, since the pulling speed V can be precisely controlled mechanically, in order to take into account both stable crystal quality and planned production, a single crystal manufacturing method is generally performed in which the pulling speed V is controlled to be fixed.

然而,在僅進行將提拉速度V設為固定的控制中,有時品質會於結晶長方向不均。此為由於提拉過程中溫度梯度G不固定而有變動的緣故。 作為對將溫度梯度G設為固定之控制較大影響的因素,舉出輻射屏蔽的下端與矽融液面之間的距離(稱為間隙(gap))。提拉單晶期間精度較佳地將此間隙控制為固定是很重要的。 However, when only the pulling speed V is controlled to be fixed, the quality may be uneven in the direction of the crystal length. This is because the temperature gradient G is not fixed but varies during the pulling process. As a factor that has a greater impact on the control of setting the temperature gradient G to be fixed, the distance between the lower end of the radiation shield and the silicon melt surface (called the gap) is cited. It is important to control this gap to be fixed with good accuracy during the pulling of the single crystal.

以往有例如專利文獻1揭露的間隙的設定法。此為如圖6中的(a)所示將棒狀的銷60安裝於以圖5的虛線圓包圍的輻射屏蔽53的下端53a,並使石英坩堝51上升。然後,如圖6中的(b)所示利用CCD(Charge Coupled Device;電荷耦合元件)攝影機等檢測熔合環(fusion ring)70並根據該熔合環70來設定初始間隙,該熔合環70係於銷60與矽融液M接觸時在銷60的周圍產生。 [先前技術文獻] [專利文獻] In the past, there is a method for setting the gap, such as disclosed in Patent Document 1. As shown in FIG6 (a), a rod-shaped pin 60 is installed at the lower end 53a of the radiation shield 53 surrounded by the dotted circle in FIG5, and the quartz crucible 51 is raised. Then, as shown in FIG6 (b), a fusion ring 70 is detected by a CCD (Charge Coupled Device) camera or the like, and the initial gap is set based on the fusion ring 70. The fusion ring 70 is generated around the pin 60 when the pin 60 contacts the silicon melt M. [Prior Technical Document] [Patent Document]

[專利文獻1]日本特開2011-57464號公報。[Patent Document 1] Japanese Patent Application Publication No. 2011-57464.

[發明所欲解決之課題][The problem that the invention wants to solve]

然而,如專利文獻1所揭露,由於設於輻射屏蔽53的下端之銷60的最前端部接觸於矽融液M時的熔合環70係微小且在液面上產生,因此難以精度較佳地檢測且有時還會有錯誤檢測。因此,有初始間隙的設定精度較低的疑慮,提拉單晶期間之間隙的控制精度變差,此時有高品質的無缺陷單晶的產率降低之課題。However, as disclosed in Patent Document 1, since the fusion ring 70 formed when the front end of the pin 60 provided at the lower end of the radiation shield 53 contacts the silicon melt M is very small and is generated on the liquid surface, it is difficult to detect with good accuracy and sometimes an erroneous detection may occur. Therefore, there is a concern that the setting accuracy of the initial gap is low, and the control accuracy of the gap during the pulling of the single crystal becomes poor, and there is a problem of reducing the yield of high-quality defect-free single crystals.

本發明係有鑑於上述事情而研創,目的在於提供一種單晶提拉裝置以及單晶提拉方法,係在利用柴可拉斯基法提拉單晶矽時,能精度較佳地控制輻射屏蔽的下端與矽融液之間的距離之間隙而培育單晶矽。 [用以解決課題之手段] The present invention was developed in view of the above-mentioned situation, and its purpose is to provide a single crystal pulling device and a single crystal pulling method, which can control the gap between the lower end of the radiation shield and the silicon melt with better precision when using the Czochralski method to pull single crystal silicon to cultivate single crystal silicon. [Means for solving the problem]

為了解決前述課題而研創的本發明的單晶提拉裝置,係利用柴可拉斯基法從容納於腔內的坩堝之矽融液提拉單晶;前述單晶提拉裝置係具備:升降驅動部,係使前述坩堝升降;加熱器,係加熱前述坩堝;圓筒狀之輻射屏蔽,係配置於形成於前述坩堝內的前述矽融液的上方,且包圍提拉的單晶的周圍;光透過性之銷構件,係貫穿前述輻射屏蔽而配置於位於前述輻射屏蔽的前端側之平台面(terrace face),以使下部位於前述矽融液側且上部位於前述輻射屏蔽的內周側;亮度檢測計,係檢測前述銷構件的亮度;以及控制器,係控制前述升降驅動部;前述控制器係藉由前述升降驅動部使前述坩堝上升並使前述亮度檢測計檢測前述銷構件的亮度,於所檢測的前述銷構件的亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止藉由前述升降驅動部所為的前述坩堝的上升。The single crystal pulling device of the present invention, which is developed to solve the above-mentioned problem, uses the Czochralski method to pull a single crystal from a silicon melt contained in a crucible in a chamber; the single crystal pulling device comprises: a lifting drive unit for lifting the crucible; a heater for heating the crucible; a cylindrical radiation shield disposed above the silicon melt formed in the crucible and surrounding the pulled single crystal; a light-transmissive pin member that penetrates the radiation shield and is disposed on a terrace surface (terrace) located on the front end side of the radiation shield; face) so that its lower portion is located on the silicon melt side and its upper portion is located on the inner peripheral side of the radiation shield; a brightness detector for detecting the brightness of the pin member; and a controller for controlling the lifting and driving portion; the controller causes the crucible to rise by means of the lifting and driving portion and causes the brightness detector to detect the brightness of the pin member, and when the detected brightness of the pin member exceeds a predetermined threshold value, it is determined that the lower end of the pin member is in contact with the silicon melt and the lifting of the crucible by the lifting and driving portion is stopped.

此外,較佳為,前述控制器係在停止藉由前述升降驅動部所為的前述坩堝的上升之狀態下,藉由前述升降驅動部使前述坩堝下降達至下述距離:從自前述輻射屏蔽的下端至前述矽融液為止之間隙的期望值減去自前述銷構件中之前述輻射屏蔽的下端至前述銷構件的前端為止之已知的長度所得之距離。 另外,較佳為,前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的25%以上的值所得之值。 或著,較佳為,前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的50%以上的值所得之值。 In addition, it is preferred that the controller, in a state where the lifting of the crucible by the lifting drive unit is stopped, lowers the crucible by the lifting drive unit to the following distance: the distance obtained by subtracting the known length from the lower end of the radiation shield in the pin member to the front end of the pin member from the expected value of the gap from the lower end of the radiation shield in the pin member to the front end of the pin member. In addition, it is preferred that the predetermined critical value of the brightness is a value obtained by adding a value of 25% or more of the standard brightness to the standard brightness when the pin member is not in contact with the silicon melt. Or, it is preferred that the predetermined critical value of the brightness is a value obtained by adding a value of 50% or more of the standard brightness to the standard brightness when the pin member is not in contact with the silicon melt.

根據此種構成,單晶提拉開始之前的輻射屏蔽的下端與矽融液面之間的初始間隙的設定中,使坩堝上升;於設於輻射屏蔽的下端之銷構件與矽融液接觸時之銷構件的亮度有較大變化時,停止坩堝的上升。其中,由於檢測亮度係不檢測矽融液面上的亮度而是檢測銷構件的亮度,從而錯誤檢測的疑慮較少,且得到精度較佳的檢測結果。 並且,使坩堝下降達至從所期望的間隙值減去銷構件的已知的長度所得之距離,藉此能精度較佳地設定初始間隙。 結果,能高精度地進行後續的單晶提拉工序中的間隙控制,並能夠提拉高品質的無缺陷單晶。 According to this structure, the crucible is raised during the setting of the initial gap between the lower end of the radiation shield and the silicon melt surface before the single crystal is pulled; when the brightness of the pin member provided at the lower end of the radiation shield and the silicon melt changes significantly when in contact, the rise of the crucible is stopped. Among them, since the brightness is detected not on the surface of the silicon melt but on the brightness of the pin member, there is less concern about erroneous detection and a more accurate detection result is obtained. In addition, the crucible is lowered to a distance obtained by subtracting the known length of the pin member from the desired gap value, thereby enabling the initial gap to be set with better accuracy. As a result, the gap control in the subsequent single crystal pulling process can be performed with high precision, and high-quality defect-free single crystals can be pulled.

此外,為了解決前述課題而研創的本發明的單晶提拉方法,係利用柴可拉斯基法從容納於腔內的坩堝之矽融液提拉單晶;前述單晶提拉方法係具備如下步驟:於提拉單晶之前使前述坩堝上升並檢測光透過性之銷構件的亮度,前述銷構件係從圓筒狀之輻射屏蔽的下端向下方延伸,前述輻射屏蔽係配置於形成於前述坩堝內的前述矽融液的上方且包圍提拉的單晶的周圍;以及於前述亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止前述坩堝的上升。In addition, the single crystal pulling method of the present invention, which was developed to solve the above-mentioned problem, utilizes the Czochralski method to pull a single crystal from a silicon melt contained in a crucible in a cavity; the above-mentioned single crystal pulling method comprises the following steps: before pulling the single crystal, the above-mentioned crucible is raised and the brightness of a light-transmitting pin member is detected, the above-mentioned pin member extends downward from the lower end of a cylindrical radiation shield, and the above-mentioned radiation shield is arranged above the above-mentioned silicon melt formed in the above-mentioned crucible and surrounds the pulled single crystal; and when the above-mentioned brightness exceeds a predetermined critical value, it is determined that the lower end of the above-mentioned pin member is in contact with the above-mentioned silicon melt and the raising of the above-mentioned crucible is stopped.

此外,較佳為,於前述亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止前述坩堝的上升之步驟之後,具備如下步驟:使前述坩堝下降達至下述距離:從自前述輻射屏蔽的下端至前述矽融液為止之間隙的期望值減去自前述銷構件的前述輻射屏蔽的下端至前述銷構件的前端為止之已知的長度所得之距離。 另外,較佳為,前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的25%以上的值所得之值。 或者,較佳為,前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的50%以上的值所得之值。 In addition, it is preferred that after the step of determining that the lower end of the pin member is in contact with the silicon melt when the brightness exceeds a predetermined threshold value and stopping the ascent of the crucible, the following step is provided: lowering the crucible to the following distance: the distance obtained by subtracting the known length from the lower end of the radiation shield of the pin member to the front end of the pin member from the expected value of the gap from the lower end of the radiation shield of the pin member to the front end of the pin member. In addition, it is preferred that the predetermined threshold value of the brightness is the value obtained by adding a value of 25% or more of the standard brightness to the reference brightness when the pin member is not in contact with the silicon melt. Alternatively, preferably, the predetermined threshold value of the brightness is a value obtained by adding a value greater than 50% of the reference brightness to the reference brightness when the pin member is not in contact with the silicon melt.

根據此種構成,在單晶提拉開始之前的輻射屏蔽的下端與矽融液面之間的初始間隙的設定中,使坩堝上升;於設於輻射屏蔽的下端之銷構件與矽融液接觸時之銷構件的亮度有較大變化時,停止坩堝的上升。其中,由於檢測亮度係不檢測矽融液面上的亮度而是檢測銷構件的亮度,從而錯誤檢測的疑慮較少,且得到精度較佳的檢測結果。 並且,使坩堝下降達至從所期望的間隙值減去銷構件的已知的長度所得之距離,藉此能精度較佳地設定初始間隙。 結果,能高精度地進行後續單晶提拉工序中的間隙控制,並能夠提拉高品質的無缺陷單晶。 [發明功效] According to this structure, the crucible is raised during the setting of the initial gap between the lower end of the radiation shield and the silicon melt surface before the single crystal is pulled; when the brightness of the pin member provided at the lower end of the radiation shield and the silicon melt changes significantly when the pin member is in contact with the silicon melt, the rise of the crucible is stopped. Among them, since the brightness is detected not on the surface of the silicon melt but on the brightness of the pin member, there is less concern about erroneous detection and a more accurate detection result is obtained. In addition, the crucible is lowered to a distance obtained by subtracting the known length of the pin member from the desired gap value, thereby enabling the initial gap to be set with better accuracy. As a result, the gap control in the subsequent single crystal pulling process can be performed with high precision, and a high-quality, defect-free single crystal can be pulled. [Effect of the invention]

根據本發明,在利用柴可拉斯基法提拉單晶矽時,能精度較佳地控制輻射屏蔽的下端與矽融液之間的距離之間隙而培育單晶矽。According to the present invention, when using the Czochralski method to grow single crystal silicon, the gap between the lower end of the radiation shield and the silicon melt can be controlled with better precision to grow single crystal silicon.

以下,利用圖式說明本發明的單晶提拉裝置以及單晶提拉方法。然而,說明本實施形態作為本發明的一例,本發明並不限於此。Hereinafter, the single crystal pulling device and the single crystal pulling method of the present invention will be described using drawings. However, this embodiment is described as an example of the present invention, and the present invention is not limited thereto.

圖1係顯示本發明的單晶提拉裝置的一例之剖視圖。此單晶提拉裝置1係具備於圓筒形狀的主腔10a上重疊提拉腔(pull chamber)10b而形成的爐體10;此爐體10內具備:碳坩堝(或石墨坩堝)2,係以能夠繞鉛直軸旋轉且能夠升降的方式設置;以及石英玻璃坩堝3(以下簡稱為坩堝3),係由碳坩堝2所保持。此坩堝3係能夠隨著碳坩堝2的旋轉而繞鉛直軸旋轉。FIG1 is a cross-sectional view showing an example of a single crystal pulling device of the present invention. The single crystal pulling device 1 comprises a furnace body 10 formed by stacking a pull chamber 10b on a cylindrical main chamber 10a; the furnace body 10 comprises: a carbon crucible (or graphite crucible) 2 which is arranged to be rotatable around a lead straight axis and to be able to be raised and lowered; and a quartz glass crucible 3 (hereinafter referred to as crucible 3) which is held by the carbon crucible 2. The crucible 3 can rotate around the lead straight axis as the carbon crucible 2 rotates.

此外,在碳坩堝20的下方設有:旋轉驅動部14,係旋轉馬達等,用以使此碳坩堝2繞鉛直軸旋轉;以及升降驅動部15,係使碳坩堝2升降移動。 此外,旋轉驅動控制部14a係連接於旋轉驅動部14,升降驅動控制部15a係連接於升降驅動部15。 In addition, below the carbon crucible 20, there are provided: a rotation drive unit 14, which is a rotation motor, etc., for rotating the carbon crucible 2 around the lead straight axis; and a lifting drive unit 15, which is for lifting and moving the carbon crucible 2. In addition, the rotation drive control unit 14a is connected to the rotation drive unit 14, and the lifting drive control unit 15a is connected to the lifting drive unit 15.

此外,單晶提拉裝置1係具備:電阻加熱式或高頻感應加熱方式之加熱器4,係用以將裝載於坩堝3之半導體原料(原料多晶矽)加熱而熔融並成為矽融液M。 此外,單晶提拉裝置1係具備:提拉機構9,係捲起線6並提拉培育的單晶C。於提拉機構9所具有的線6的前端安裝有種晶P。用以進行提拉機構9的旋轉驅動的控制之旋轉驅動控制部9a係連接於提拉機構9。 In addition, the single crystal pulling device 1 is equipped with a heater 4 of a resistance heating type or a high-frequency induction heating type, which is used to heat the semiconductor raw material (raw material polycrystalline silicon) loaded on the crucible 3 to melt and form a silicon melt M. In addition, the single crystal pulling device 1 is equipped with a pulling mechanism 9, which winds up the wire 6 and pulls the cultivated single crystal C. A seed crystal P is installed at the front end of the wire 6 of the pulling mechanism 9. A rotation drive control unit 9a for controlling the rotation drive of the pulling mechanism 9 is connected to the pulling mechanism 9.

此外,在形成於坩堝3內的矽融液M的上方配置有包圍單晶C的周圍之輻射屏蔽7。此輻射屏蔽7係上部與下部形成有開口,且用以遮蔽來自加熱器4、矽融液M等對培育中的單晶C的多餘的輻射熱並整流爐內的氣體流。 針對輻射屏蔽7的形狀詳細說明,如圖2所示,輻射屏蔽7係具有:錐形(taper)部7b,係從上部開口7a向矽融液M(向下方)縮徑;以及平台部7c,係從錐形部7b的下端向內側水平地延伸設置,且平台部7c係形成為環狀。以通過形成於平台部7c的內緣之下部開口7d與上部開口7a的方式提拉單晶。 In addition, a radiation shield 7 surrounding the single crystal C is arranged above the silicon melt M formed in the crucible 3. The radiation shield 7 has openings formed at the upper and lower parts, and is used to shield the excess radiation heat from the heater 4, the silicon melt M, etc. to the single crystal C being grown and to rectify the gas flow in the furnace. The shape of the radiation shield 7 is described in detail. As shown in FIG. 2, the radiation shield 7 has: a tapered portion 7b that tapers from the upper opening 7a toward the silicon melt M (downward); and a platform portion 7c that extends horizontally inward from the lower end of the tapered portion 7b, and the platform portion 7c is formed in a ring shape. The single crystal is pulled through the lower opening 7d and the upper opening 7a formed on the inner edge of the terrace portion 7c.

平台部7c的徑向的長度(寬度)係形成為例如10mm以上至150mm以下,以免矽融液M的反射或雜散光到達錐形部7b的下端附近。如圖示向下方延伸的光透過性之石英銷8(銷構件)係設於此平台部7c。亦即,此石英銷8係貫穿輻射屏蔽7而配置於位於輻射屏蔽7的前端側之平台部7c(平台面),以使下部位於矽融液M側且上部位於輻射屏蔽7的內周側。 此石英銷8係例如由直筒部8a與直徑比直筒部8a大的圓板狀之頭部8b所構成,且藉由從上方朝下方插入直筒部8a至配合直筒部8a的直徑來形成於平台部7c之孔7c1並將頭部8b卡止於平台部7c而設計。此石英銷8中,從輻射屏蔽7的下端至石英銷8的前端8a1為止的長度L係形成為例如15mm。 The radial length (width) of the platform portion 7c is formed to be, for example, more than 10 mm and less than 150 mm, so as to prevent the reflection or stray light of the silicon melt M from reaching the vicinity of the lower end of the conical portion 7b. As shown in the figure, a light-transmissive quartz pin 8 (pin member) extending downward is provided on this platform portion 7c. That is, this quartz pin 8 penetrates the radiation shield 7 and is arranged on the platform portion 7c (platform surface) located on the front end side of the radiation shield 7, so that the lower part is located on the silicon melt M side and the upper part is located on the inner circumference of the radiation shield 7. This quartz pin 8 is composed of, for example, a straight tube 8a and a disk-shaped head 8b having a larger diameter than the straight tube 8a, and is designed by inserting the straight tube 8a from the top to the bottom to form a hole 7c1 in the platform 7c that matches the diameter of the straight tube 8a and locking the head 8b to the platform 7c. In this quartz pin 8, the length L from the lower end of the radiation shield 7 to the front end 8a1 of the quartz pin 8 is formed to be, for example, 15 mm.

此外,單晶提拉裝置1係具備:光學式之直徑測定感測器(直徑測定裝置)16,係CCD攝影機等,用以測定培育中的單晶的直徑。於主腔10a的上表面部設有觀測用的小窗10a1,從此小窗10a1的外側檢測固液界面的結晶端(以虛線箭頭顯示的位置)的位置變化。In addition, the single crystal pulling device 1 is equipped with an optical diameter measuring sensor (diameter measuring device) 16, which is a CCD camera, etc., for measuring the diameter of the single crystal being grown. A small window 10a1 for observation is provided on the upper surface of the main chamber 10a, and the position change of the crystallization end (the position shown by the dotted arrow) of the solid-liquid interface is detected from the outside of the small window 10a1.

此外,單晶提拉裝置1係具備:亮度檢測計17,係CCD攝影機等,用以測定設於輻射屏蔽7的下端之石英銷8的頭部8b的亮度。如圖2所示,此亮度檢測計17係配置為測定下述亮度:配置於輻射屏蔽7的平台部7c的上表面之石英銷8的頭部8b的亮度。於主腔10a的上表面部設有與小窗10a1不同的小窗10a2,從此小窗10a2的外側檢測石英銷8的頭部8b的亮度變化。In addition, the single crystal pulling device 1 is provided with a brightness detector 17, which is a CCD camera or the like, for measuring the brightness of the head 8b of the quartz pin 8 provided at the lower end of the radiation shield 7. As shown in FIG2 , the brightness detector 17 is configured to measure the brightness of the head 8b of the quartz pin 8 provided on the upper surface of the platform portion 7c of the radiation shield 7. A small window 10a2 different from the small window 10a1 is provided on the upper surface of the main chamber 10a, and the brightness change of the head 8b of the quartz pin 8 is detected from the outside of the small window 10a2.

本實施形態中,如此檢測石英銷8的頭部8b的亮度變化是為了高精度地進行輻射屏蔽7的下端與矽融液面M1之間的初始間隙的設定。針對此初始間隙之設定方法於下文詳細描述,於石英銷8的前端8a1與矽融液M接觸時,光通過石英銷8內,石英銷8的頭部8b更高亮度地發光。利用亮度檢測計17檢測此亮度變化。 此外,石英銷8的頭部8b高亮度地發光係根據如下原理。矽融液M為橘色且相較於爐內的周邊環境還亮。於透明的石英銷8接觸於矽融液M時,藉由表面張力使環形成於石英銷8的周圍,並較接觸之前更多地接收由矽融液M所發射的可見光。因石英銷8為透明而可見光幾乎不被反射、吸收而傳播至石英銷8的頭部8b,從而高亮度地發光。 In this embodiment, the brightness change of the head 8b of the quartz pin 8 is detected in this way in order to set the initial gap between the lower end of the radiation shield 7 and the silicon melt surface M1 with high precision. The setting method of this initial gap is described in detail below. When the front end 8a1 of the quartz pin 8 contacts the silicon melt M, light passes through the quartz pin 8, and the head 8b of the quartz pin 8 emits light with higher brightness. The brightness detector 17 is used to detect this brightness change. In addition, the head 8b of the quartz pin 8 emits light with high brightness based on the following principle. The silicon melt M is orange and brighter than the surrounding environment in the furnace. When the transparent quartz pin 8 contacts the silicon melt M, a ring is formed around the quartz pin 8 due to surface tension, and receives more visible light emitted by the silicon melt M than before the contact. Since the quartz pin 8 is transparent, the visible light is hardly reflected or absorbed and is transmitted to the head 8b of the quartz pin 8, thereby emitting high brightness.

此外,此單晶提拉裝置1係具備:控制器11,係具有記憶裝置11a與運算控制裝置11b;並且,旋轉驅動控制部14a、升降驅動控制部15a、旋轉驅動控制部9a、直徑測定感測器16、亮度檢測計17係分別連接於運算控制裝置11b。In addition, the single crystal pulling device 1 is equipped with: a controller 11 having a memory device 11a and an operation control device 11b; and a rotation drive control unit 14a, a lifting drive control unit 15a, a rotation drive control unit 9a, a diameter measuring sensor 16, and a brightness detector 17 are respectively connected to the operation control device 11b.

如此構成的單晶提拉裝置1中,例如若要培育直徑300mm的單晶C,則以下述方式進行提拉。 亦即,首先將原料多晶矽(例如460kg)裝載於坩堝3,根據控制器11的記憶裝置11a所記憶的程式而開始結晶培育工序。 In the single crystal pulling device 1 thus constructed, if, for example, a single crystal C with a diameter of 300 mm is to be grown, the pulling is performed in the following manner. That is, firstly, the raw material polycrystalline silicon (for example, 460 kg) is loaded on the crucible 3, and the crystal growth process is started according to the program stored in the memory device 11a of the controller 11.

首先,爐體10內成為預定氛圍(atmosphere)(主要是氬氣等惰性氣體)。例如,形成有爐內壓為65torr、氬氣流量為90l/min的爐內氛圍。 接著,在坩堝3以預定轉速(rpm)朝預定方向旋轉動作的狀態下,裝載於坩堝3內的原料多晶矽係藉由加熱器4的加熱而熔融並成為矽融液M(圖3的步驟S1)。 First, a predetermined atmosphere (mainly inert gas such as argon) is formed in the furnace body 10. For example, a furnace atmosphere with a furnace internal pressure of 65 torr and an argon flow rate of 90 l/min is formed. Then, while the crucible 3 rotates in a predetermined direction at a predetermined speed (rpm), the raw material polycrystalline silicon loaded in the crucible 3 is melted by heating of the heater 4 and becomes silicon melt M (step S1 in Figure 3).

此外,將對加熱器4的初始供應電力、提拉速度等作為參數,調整提拉條件,種晶P係繞軸以預定轉速開始旋轉。旋轉方向係與坩堝3的旋轉方向相反的方向。 於矽融液M的液面高度穩定時,在控制器11的控制下,經由升降驅動控制部15a驅動升降驅動部15使坩堝3的高度以例如0.05mm的間隔微動(inching)(寸動)動作來上升(圖3的步驟S2)。 此外,此期間,控制器11係利用亮度檢測計17監控石英銷8的頭部8b的亮度變化(圖3的步驟S3)。此外,本實施形態中,控制器11係預先記憶石英銷8接觸於矽融液M之後的最大亮度為100%。此外,石英銷8接觸於矽融液M之前的亮度(設為基準亮度)為例如40%。 In addition, the initial power supplied to the heater 4, the pulling speed, etc. are used as parameters to adjust the pulling conditions, and the seed crystal P starts to rotate around the axis at a predetermined speed. The rotation direction is opposite to the rotation direction of the crucible 3. When the liquid level of the silicon melt M is stable, under the control of the controller 11, the lifting drive control unit 15a drives the lifting drive unit 15 to increase the height of the crucible 3 by an inching action at intervals of, for example, 0.05 mm (step S2 of Figure 3). In addition, during this period, the controller 11 uses the brightness detector 17 to monitor the brightness change of the head 8b of the quartz pin 8 (step S3 of Figure 3). In addition, in this embodiment, the controller 11 pre-memorizes the maximum brightness of the quartz pin 8 after contacting the silicon melt M as 100%. In addition, the brightness of the quartz pin 8 before it contacts the silicon melt M (set as the reference brightness) is, for example, 40%.

於藉由坩堝3的上升而使矽融液M的矽融液面M1與輻射屏蔽7的下端之石英銷8的前端8a1接觸時,石英銷8的頭部8b的亮度上升至預定臨限值以上(圖3的步驟S4)。 控制器11係藉由亮度檢測計17檢測該亮度上升並控制升降驅動部15來停止坩堝3的上升動作(圖3的步驟S5)。具體而言,控制器11係於由亮度檢測計17所檢測的亮度變化超過預定臨限值時判斷為輻射屏蔽7的下端之石英銷8與矽融液M接觸。例如,此亮度的預定臨限值是指石英銷8接觸於矽融液M之後的最大亮度為100%時在石英銷8未接觸於矽融液M之狀態下的基準亮度(此處為40%)加上該基準亮度(此處為40%)的例如25%以上(或50%以上)所得之值。 When the silicon melt surface M1 of the silicon melt M contacts the front end 8a1 of the quartz pin 8 at the lower end of the radiation shield 7 due to the rise of the crucible 3, the brightness of the head 8b of the quartz pin 8 rises to a predetermined threshold value or more (step S4 in FIG. 3 ). The controller 11 detects the brightness rise by the brightness detector 17 and controls the lifting drive 15 to stop the rising action of the crucible 3 (step S5 in FIG. 3 ). Specifically, the controller 11 determines that the quartz pin 8 at the lower end of the radiation shield 7 contacts the silicon melt M when the brightness change detected by the brightness detector 17 exceeds the predetermined threshold value. For example, the predetermined threshold value of the brightness refers to the value obtained by adding, for example, 25% or more (or 50% or more) of the reference brightness (here 40%) when the quartz pin 8 is not in contact with the silicon melt M when the maximum brightness after the quartz pin 8 is in contact with the silicon melt M is 100%.

控制器11係藉由升降驅動部15使坩堝3下降達至從所期望的間隙值減去石英銷8的長度L所得之距離(圖3的步驟S6)。藉此,高精度地設定初始間隙值。 此外,由於固定的輻射屏蔽7的高度係已知,因此能容易求出設定間隙之後之矽融液面M1的高度位置(初始液面高度)。控制器11係預先記憶此初始液面高度(圖3的步驟S7)。 The controller 11 lowers the crucible 3 by the lifting drive 15 to a distance obtained by subtracting the length L of the quartz pin 8 from the desired gap value (step S6 in FIG. 3 ). In this way, the initial gap value is set with high precision. In addition, since the height of the fixed radiation shield 7 is known, the height position (initial liquid level) of the silicon melt liquid surface M1 after setting the gap can be easily calculated. The controller 11 memorizes this initial liquid level in advance (step S7 in FIG. 3 ).

接著,使線6下降並使種晶P接觸於矽融液M,將種晶P的前端部溶解後,進行頸縮(necking)而形成有頸部(圖3的步驟S8)。 然後,結晶直徑逐漸地擴徑而形成肩部C1(圖3的步驟S9)。 此外,控制器11係藉由升降驅動控制部15a而驅動控制升降驅動部15將提拉速度固定為例如0.55mm/min,移至形成成為製品部分的直筒部C2的工序(圖3的步驟S10)。 Next, the wire 6 is lowered and the seed crystal P is brought into contact with the silicon melt M, and after the front end of the seed crystal P is dissolved, necking is performed to form a neck (step S8 in FIG. 3 ). Then, the crystal diameter gradually expands to form a shoulder C1 (step S9 in FIG. 3 ). In addition, the controller 11 drives and controls the lifting drive unit 15 to fix the pulling speed at, for example, 0.55 mm/min through the lifting drive control unit 15a, and moves to the process of forming the straight tube portion C2 that becomes the product part (step S10 in FIG. 3 ).

於形成此直筒部C2的期間,控制器11係使用直徑測定感測器16的測定結果來求出單晶矽的固化率,根據此固化率與矽融液面M1的初始高度而計算該時間點的矽融液面M1的高度位置與間隙(圖3的步驟S11)。 然後,判斷間隙的測定尺寸的變動是否為±0.1mm以內(圖3的步驟S12),若未滿足,則控制升降驅動控制部15a而藉由升降驅動部15調整坩堝3的高度位置,以滿足該條件(圖3的步驟S13)。提拉工序期間,控制為滿足步驟S12的條件,進行單晶提拉工序。 During the formation of this straight tube portion C2, the controller 11 uses the measurement result of the diameter measuring sensor 16 to obtain the solidification rate of the single crystal silicon, and calculates the height position and gap of the silicon melt surface M1 at this time point based on this solidification rate and the initial height of the silicon melt surface M1 (step S11 in Figure 3). Then, it is determined whether the change in the measured dimension of the gap is within ±0.1mm (step S12 in Figure 3). If it is not satisfied, the lifting drive control unit 15a is controlled to adjust the height position of the crucible 3 by the lifting drive unit 15 to meet the condition (step S13 in Figure 3). During the pulling process, the control is to meet the condition of step S12, and the single crystal pulling process is performed.

於直筒部C2形成至預定長度為止之後(圖3的步驟S14),移至最後的尾部工序(圖3的步驟S15)。在此尾部工序中使結晶下端與矽融液M的接觸面積逐漸地變小,將單晶C與矽融液M分離而製造單晶矽。After the straight tube portion C2 is formed to a predetermined length (step S14 in FIG. 3 ), the process proceeds to the final tailing process (step S15 in FIG. 3 ). In this tailing process, the contact area between the lower end of the crystal and the silicon melt M is gradually reduced, and the single crystal C is separated from the silicon melt M to produce single crystal silicon.

如上所述,根據本實施形態,單晶提拉開始之前的輻射屏蔽7的下端與矽融液面M1之間的初始間隙的設定中,使坩堝3以微動動作來上升;在設於輻射屏蔽7的下端之石英銷8與矽融液M接觸時之石英銷8的亮度有較大變化時停止坩堝3的上升。其中,由於檢測亮度為不檢測矽融液面M1上的亮度而是檢測石英銷8的亮度,從而錯誤檢測的疑慮較少,且得到精度較佳的檢測結果。 然後,使坩堝3下降達至從所期望的間隙值減去石英銷8的已知的長度L所得之距離,藉此能精度較佳地設定初始間隙。 結果,能高精度地進行後續單晶提拉工序中的間隙控制,並能夠提拉高品質的單晶。 As described above, according to the present embodiment, in setting the initial gap between the lower end of the radiation shield 7 and the silicon melt surface M1 before the single crystal is pulled, the crucible 3 is raised by a micro-motion; when the brightness of the quartz pin 8 provided at the lower end of the radiation shield 7 and the silicon melt M changes significantly, the rise of the crucible 3 is stopped. Among them, since the brightness is detected by detecting the brightness of the quartz pin 8 instead of the brightness on the silicon melt surface M1, there is less concern about erroneous detection, and a more accurate detection result is obtained. Then, the crucible 3 is lowered to a distance obtained by subtracting the known length L of the quartz pin 8 from the desired gap value, thereby setting the initial gap with better accuracy. As a result, the gap control in the subsequent single crystal pulling process can be performed with high precision, and high-quality single crystals can be pulled.

此外,上述實施形態中,單晶提拉期間的間隙設定中,矽融液面M1上的高度位置檢測係根據單晶的固化率而計算,然而本發明並不限於此。例如,如日本特開2008-189522號公報所揭露,可利用CCD攝影機檢測照射至矽融液面M1的雷射光的反射,並圖像處理經檢測的圖像訊號來求出矽融液M的液面高度。 此外,上述實施形態中提拉速度設為固定,然而提拉速度係可不設為固定並有變動。 In addition, in the above-mentioned embodiment, in the gap setting during the single crystal pulling period, the height position detection on the silicon melt surface M1 is calculated based on the solidification rate of the single crystal, but the present invention is not limited to this. For example, as disclosed in Japanese Patent Publication No. 2008-189522, a CCD camera can be used to detect the reflection of the laser light irradiated to the silicon melt surface M1, and the detected image signal can be processed to obtain the liquid level height of the silicon melt M. In addition, in the above-mentioned embodiment, the pulling speed is set to be fixed, but the pulling speed may not be set to be fixed and may vary.

此外,前述實施形態中,以一根石英銷8設於輻射屏蔽7的下端為例說明,然而除了石英銷8之外,亦可將較此石英銷8更短的石英銷設於輻射屏蔽7的下端。 此時,單晶提拉期間的控制中,雖然以隨著矽融液M減少而使坩堝3上升的方式控制,然而於較短的銷接觸於矽融液M時,亦可以停止坩堝3的上升或使坩堝3下降的方式進行控制,以便防止輻射屏蔽7的本體與矽融液M接觸。 In addition, in the above-mentioned embodiment, a quartz pin 8 is provided at the lower end of the radiation shield 7 as an example. However, in addition to the quartz pin 8, a quartz pin shorter than the quartz pin 8 can also be provided at the lower end of the radiation shield 7. At this time, in the control during the single crystal pulling period, although the crucible 3 is controlled to rise as the silicon melt M decreases, when the shorter pin contacts the silicon melt M, the crucible 3 can also be stopped from rising or the crucible 3 can be controlled to fall, so as to prevent the main body of the radiation shield 7 from contacting the silicon melt M.

此外,前述實施形態中,石英銷8係由直徑固定的直筒部8a與直徑比直筒部8a大的圓板狀之頭部8b所構成,然而本發明並不限於該形態。 例如,可形成為下方的直徑比上方的直徑小(上方的直徑比下方的直徑大)。亦即,石英銷8中,較輻射屏蔽7更上方的頭部8b(較輻射屏蔽7更上方的第二區域)的每長度的表面積係比較輻射屏蔽7更下方的直筒部8a(較輻射屏蔽7更下方的第一區域)還大時,更容易利用亮度檢測計17檢測亮度 (若頭部8b的表面積過小,則更容易受到擾動(disturbance)等影響導致測定精度降低)。 [實施例] In addition, in the above-mentioned embodiment, the quartz pin 8 is composed of a straight tube portion 8a with a fixed diameter and a disc-shaped head portion 8b with a larger diameter than the straight tube portion 8a, but the present invention is not limited to this form. For example, the diameter of the lower portion can be smaller than the diameter of the upper portion (the diameter of the upper portion is larger than the diameter of the lower portion). That is, in the quartz pin 8, when the surface area per length of the head portion 8b above the radiation shield 7 (the second area above the radiation shield 7) is larger than that of the straight tube portion 8a below the radiation shield 7 (the first area below the radiation shield 7), it is easier to detect the brightness using the brightness detector 17 (if the surface area of the head portion 8b is too small, it is more susceptible to disturbances, etc., resulting in reduced measurement accuracy). [Example]

針對本發明的單晶提拉裝置以及單晶提拉方法,根據實施例進一步說明。The single crystal pulling device and the single crystal pulling method of the present invention are further described according to the embodiments.

[實驗1] 實驗1中,如圖1所示的單晶提拉裝置中,將460kg的矽原料填充於直徑32英寸的石英坩堝內並形成矽融液。將矽融液熔融於坩堝內之後,使坩堝上升並驗證矽融液與設於輻射屏蔽的下端之石英銷接觸時的亮度是否有變化。 使坩堝以0.05mm的單位微動動作來上升,檢測此時的亮度。 [Experiment 1] In Experiment 1, 460 kg of silicon raw material was filled into a quartz crucible with a diameter of 32 inches in the single crystal pulling device shown in Figure 1 to form a silicon melt. After the silicon melt was melted in the crucible, the crucible was raised to verify whether the brightness changed when the silicon melt came into contact with the quartz pin at the lower end of the radiation shield. The crucible was raised in micro-movements of 0.05 mm and the brightness at that time was detected.

此實驗1的結果顯示於圖4。圖4的圖表中,左側的縱軸為相對於基準值(0mm)的坩堝變動(mm),右側的縱軸為亮度(%)。此外,縱軸的亮度(%)係將石英銷接觸於矽融液之後的最大亮度設為100%。 如圖4的圖表所示,亮度於使坩堝上升+0.4mm的位置大幅上升。藉由目測,此位置為矽融液與設於輻射屏蔽的下端之石英銷接觸的位置。亦即,確認到亮度於矽融液與設於輻射屏蔽的下端之石英銷接觸時大幅上升。 此外,從圖4的圖表確認到控制器用以判斷石英銷與矽融液接觸之臨限值為幾乎沒有因拾取擾動導致錯誤判斷的可能性之亮度50%(在石英銷與矽融液接觸之前的基準亮度40%加上該基準亮度(40%)的25%的值所得之值)以上,更確實地,較佳為60%(在石英銷與矽融液接觸之前的基準亮度40%加上該基準亮度(40%)的50%的值所得之值)以上。 The results of this experiment 1 are shown in Figure 4. In the graph of Figure 4, the left vertical axis is the crucible displacement (mm) relative to the reference value (0mm), and the right vertical axis is the brightness (%). In addition, the brightness (%) on the vertical axis is the maximum brightness after the quartz pin contacts the silicon melt as 100%. As shown in the graph of Figure 4, the brightness increases significantly at the position where the crucible is raised by +0.4mm. By visual inspection, this position is the position where the silicon melt contacts the quartz pin located at the lower end of the radiation shield. That is, it is confirmed that the brightness increases significantly when the silicon melt contacts the quartz pin located at the lower end of the radiation shield. In addition, the graph in FIG4 shows that the critical value used by the controller to judge whether the quartz pin is in contact with the silicon melt is a brightness of 50% or more (the value obtained by adding 25% of the reference brightness (40%) to the reference brightness before the quartz pin is in contact with the silicon melt), which is almost impossible to cause an erroneous judgment due to the pickup disturbance. More specifically, it is preferably 60% or more (the value obtained by adding 50% of the reference brightness (40%) to the reference brightness before the quartz pin is in contact with the silicon melt).

[實驗2] [實施例1] 實驗2中,實際實施十根單晶矽的提拉。實施例1中,與實驗1同樣地將460kg的矽原料填充於直徑32英寸的石英坩堝內並形成矽融液。 依據本實施形態,將石英銷設於輻射屏蔽的下端並設定輻射屏蔽與矽融液面之初始間隙。將此間隙設為50mm。 此外,將爐內壓設為50torr,氬氣以流量100L/min流入,藉此製作爐內環境。 然後,將坩堝轉速設為1rpm,將結晶轉速設為7rpm(與坩堝旋轉相反的方向),以提拉速度0.6mm/min將結晶直徑305mm至310mm作為目標來進行單晶培育。此外,於提拉期間將輻射屏蔽與矽融液面之間的間隙控制為50mm±0.1mm。 [Experiment 2] [Example 1] In Experiment 2, ten single crystal silicons were pulled. In Example 1, 460 kg of silicon raw material was filled into a quartz crucible with a diameter of 32 inches and a silicon melt was formed as in Experiment 1. According to this embodiment, a quartz pin was set at the lower end of the radiation shield and the initial gap between the radiation shield and the silicon melt surface was set. This gap was set to 50 mm. In addition, the furnace internal pressure was set to 50 torr, and argon gas was flowed in at a flow rate of 100 L/min to create a furnace internal environment. Then, the crucible speed was set to 1rpm, the crystallization speed was set to 7rpm (in the opposite direction of the crucible rotation), and the single crystal was grown at a pulling speed of 0.6mm/min with a crystal diameter of 305mm to 310mm as the target. In addition, the gap between the radiation shield and the silicon melt surface was controlled to 50mm±0.1mm during the pulling process.

此實施例1中,提拉單晶十根以成為無缺陷。作為無缺陷區域的評價,空隙缺陷所存在的富V(V-rich)側係確認有無LPD(Light Point Defect;光點缺陷)評價的五十張重疊圖所為的群集並判斷有無COP(Crystal Originated Particle;晶體源顆粒)。In this embodiment 1, ten single crystals were pulled to be defect-free. As an evaluation of the defect-free area, the V-rich side where the void defect exists is confirmed to be a cluster of fifty overlay images of LPD (Light Point Defect) evaluation to determine whether there is COP (Crystal Originated Particle).

富I(I-rich)側係用Cu(銅)裝飾(decoration)法判斷有無 B帶(B-band)區域,該B帶區域係容易產生氧析出物的區域。作為無缺陷結晶,定義為均無COP、B帶區域的結晶。 實施例1的結果顯示於表1。如表1所示,評價十根單晶的結果,確認到十根單晶均遍及全長而為無缺陷結晶。 The I-rich side is judged by the Cu (copper) decoration method to determine whether there is a B-band region, which is a region where oxygen precipitates are easily generated. As a defect-free crystal, it is defined as a crystal without COP and B-band region. The results of Example 1 are shown in Table 1. As shown in Table 1, the results of evaluating ten single crystals confirmed that all ten single crystals were defect-free crystals throughout the entire length.

[比較例1] 比較例1中,使用鏡像間隙的間隙組合方法來嘗試提拉無缺陷結晶。鏡像間隙係使用與檢測石英銷的亮度之CCD攝影機相同的CCD攝影機來檢測輻射屏蔽的實像與映照於矽融液面的鏡像之屏蔽的邊緣,從該差分計算間隙。 比較例1的結果與實施例1的結果一起顯示於表1。進行十根單晶提拉的結果,藉由Cu裝飾法所為的晶圓評價檢測出兩根單晶有遍及全長的晶格間缺陷(I-defect;Inter-Grid Type Defect)。此外,兩根結晶內的一部分觀察到DSOD(Direct Surface Oxide Defect;直接表面氧化物缺陷)或LPD等群集模式。 [Comparative Example 1] In Comparative Example 1, a gap combination method using a mirror gap was used to attempt to pull a defect-free crystal. The mirror gap uses the same CCD camera as the one that detects the brightness of the quartz pin to detect the edge of the shield of the real image of the radiation shield and the mirror image reflected on the silicon melt surface, and the gap is calculated from the difference. The results of Comparative Example 1 are shown in Table 1 together with the results of Example 1. As a result of pulling ten single crystals, two single crystals were detected to have inter-lattice defects (I-defect; Inter-Grid Type Defect) throughout the entire length by wafer evaluation using the Cu decoration method. In addition, cluster patterns such as DSOD (Direct Surface Oxide Defect; direct surface oxide defect) or LPD were observed in part of the two crystals.

[表1] 結晶根數 間隙不均(σ) 無缺陷結晶產率(平均) 實施例1 10 0.03 100% 比較例1 10 0.60 72% [Table 1] Number of crystal roots Gap Unevenness(σ) Defect-free crystal yield (average) Embodiment 1 10 0.03 100% Comparison Example 1 10 0.60 72%

實施例1的結果,根據本發明,確認到間隙不均變小,且無缺陷結晶產率較高。The results of Example 1 confirmed that the gap unevenness became smaller and the defect-free crystal yield was higher according to the present invention.

1:單晶提拉裝置 2:碳坩堝(石墨坩堝) 3:石英玻璃坩堝(坩堝) 4,52:加熱器 6:線 7,53:輻射屏蔽 7a:上部開口 7b:錐形部 7c:平台部 7c1:孔 7d:下部開口 8:石英銷 8a,C2:直筒部 8a1:前端 8b:頭部 9:提拉機構 9a:旋轉驅動控制部 10:爐體 10a:主腔 10a1,10a2:小窗 10b:提拉腔 11:控制器 11a:記憶裝置 11b:運算控制裝置 14:旋轉驅動部 14a:旋轉驅動控制部 15:升降驅動部 15a:升降驅動控制部 16:直徑測定感測器(直徑測定裝置) 17:亮度檢測計 50:腔 51:石英坩堝 53a:下端 60:銷 70:熔合環 C:單晶 C1:肩部 L:長度 M:矽融液 M1:矽融液面 P:種晶 S1~S15:步驟 1: Single crystal pulling device 2: Carbon crucible (graphite crucible) 3: Quartz glass crucible (crucible) 4,52: Heater 6: Wire 7,53: Radiation shield 7a: Upper opening 7b: Cone 7c: Platform 7c1: Hole 7d: Lower opening 8: Quartz pin 8a,C2: Straight tube 8a1: Front end 8b: Head 9: Pulling mechanism 9a: Rotation drive control unit 10: Furnace body 10a: Main chamber 10a1,10a2: Small window 10b: Pulling chamber 11: Controller 11a: Memory device 11b: Operation control device 14: Rotation drive unit 14a: Rotation drive control unit 15: Lifting drive unit 15a: Lifting drive control unit 16: Diameter measuring sensor (diameter measuring device) 17: Brightness detector 50: Cavity 51: Quartz crucible 53a: Lower end 60: Pin 70: Fusion ring C: Single crystal C1: Shoulder L: Length M: Silicon melt M1: Silicon melt surface P: Seed crystal S1~S15: Steps

[圖1]係顯示本發明的單晶提拉裝置的一例之剖視圖。 [圖2]係放大圖1的單晶提拉裝置的一部分之示意性剖視圖。 [圖3]係顯示本發明的單晶提拉方法的一例之流程圖。 [圖4]係顯示實施例的結果之圖表。 [圖5]係以往的單晶提拉裝置之剖視圖。 [圖6]中,(a)與(b)係圖5的局部放大圖,用以說明設於輻射屏蔽的下端之銷接觸於矽融液時產生的熔合環。 [FIG. 1] is a cross-sectional view showing an example of a single crystal pulling device of the present invention. [FIG. 2] is a schematic cross-sectional view showing a portion of the single crystal pulling device of FIG. 1 in an enlarged manner. [FIG. 3] is a flow chart showing an example of a single crystal pulling method of the present invention. [FIG. 4] is a graph showing the results of an embodiment. [FIG. 5] is a cross-sectional view of a conventional single crystal pulling device. [FIG. 6], (a) and (b) are partial enlarged views of FIG. 5, used to illustrate the fusion ring generated when the pin provided at the lower end of the radiation shield contacts the silicon melt.

1:單晶提拉裝置 1: Single crystal pulling device

2:碳坩堝(石墨坩堝) 2: Carbon crucible (graphite crucible)

3:石英玻璃坩堝(坩堝) 3: Quartz glass crucible (crucible)

4:加熱器 4: Heater

6:線 6: Line

7:輻射屏蔽 7: Radiation shielding

7b:錐形部 7b: Cone

7c:平台部 7c: Platform Department

8:石英銷 8: Quartz pins

9:提拉機構 9: Lifting mechanism

9a:旋轉驅動控制部 9a: Rotation drive control unit

10:爐體 10: Furnace body

10a:主腔 10a: Main cavity

10a1,10a2:小窗 10a1,10a2: small window

10b:提拉腔 10b: Pulling cavity

11:控制器 11: Controller

11a:記憶裝置 11a: Memory device

11b:運算控制裝置 11b: Computational control device

14:旋轉驅動部 14: Rotary drive unit

14a:旋轉驅動控制部 14a: Rotation drive control unit

15:升降驅動部 15: Lifting drive unit

15a:升降驅動控制部 15a: Lifting drive control unit

16:直徑測定感測器(直徑測定裝置) 16: Diameter measuring sensor (diameter measuring device)

17:亮度檢測計 17: Brightness tester

C:單晶 C: Single crystal

C1:肩部 C1: Shoulder

C2:直筒部 C2: Straight section

M:矽融液 M: Silicon melt

M1:矽融液面 M1: Silicon melt surface

P:種晶 P: Seed crystal

Claims (8)

一種單晶提拉裝置,係利用柴可拉斯基法從容納於腔內的坩堝之矽融液提拉單晶; 前述單晶提拉裝置係具備: 升降驅動部,係使前述坩堝升降; 加熱器,係加熱前述坩堝; 圓筒狀之輻射屏蔽,係配置於形成於前述坩堝內的前述矽融液的上方,且包圍提拉的單晶的周圍; 光透過性之銷構件,係貫穿前述輻射屏蔽而配置於位於前述輻射屏蔽的前端側之平台面,以使下部位於前述矽融液側且上部位於前述輻射屏蔽的內周側; 亮度檢測計,係檢測前述銷構件的亮度;以及 控制器,係控制前述升降驅動部; 前述控制器係藉由前述升降驅動部使前述坩堝上升並使前述亮度檢測計檢測前述銷構件的亮度,於所檢測的前述銷構件的亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止藉由前述升降驅動部所為的前述坩堝的上升。 A single crystal pulling device uses the Czochralski method to pull a single crystal from a silicon melt contained in a crucible in a chamber; The single crystal pulling device comprises: A lifting drive unit for lifting and lowering the crucible; A heater for heating the crucible; A cylindrical radiation shield is arranged above the silicon melt formed in the crucible and surrounds the pulled single crystal; A light-transmissive pin member is passed through the radiation shield and arranged on a platform surface located on the front end side of the radiation shield so that the lower part is located on the silicon melt side and the upper part is located on the inner circumference of the radiation shield; A brightness detector for detecting the brightness of the pin member; and A controller for controlling the lifting drive unit; The controller causes the crucible to rise by the lifting drive unit and causes the brightness detector to detect the brightness of the pin member. When the detected brightness of the pin member exceeds a predetermined threshold value, it is determined that the lower end of the pin member contacts the silicon melt and the lifting of the crucible by the lifting drive unit is stopped. 如請求項1所記載之單晶提拉裝置,其中前述控制器係在停止藉由前述升降驅動部所為的前述坩堝的上升之狀態下,藉由前述升降驅動部使前述坩堝下降達至下述距離:從自前述輻射屏蔽的下端至前述矽融液為止之間隙的期望值減去自前述銷構件中之前述輻射屏蔽的下端至前述銷構件的前端為止之已知的長度所得之距離。A single crystal pulling device as described in claim 1, wherein the controller, in a state where the lifting of the crucible by the lifting drive unit is stopped, causes the crucible to be lowered to the following distance by the lifting drive unit: a distance obtained by subtracting a known length from the lower end of the radiation shield in the pin member to the front end of the pin member from the expected value of the gap from the lower end of the radiation shield in the pin member. 如請求項1所記載之單晶提拉裝置,其中前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的25%以上的值所得之值。A single crystal pulling device as recited in claim 1, wherein the predetermined threshold value of the brightness is a value obtained by adding a value of 25% or more of the baseline brightness to a baseline brightness when the pin member is not in contact with the silicon melt. 如請求項1所記載之單晶提拉裝置,其中前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的50%以上的值所得之值。A single crystal pulling device as recited in claim 1, wherein the predetermined threshold value of the brightness is a value obtained by adding a value of 50% or more of the baseline brightness to a baseline brightness when the pin member is not in contact with the silicon melt. 一種單晶提拉方法,係利用柴可拉斯基法從容納於腔內的坩堝之矽融液提拉單晶; 前述單晶提拉方法係具備如下步驟: 於提拉單晶之前使前述坩堝上升並檢測光透過性之銷構件的亮度,前述銷構件係從圓筒狀之輻射屏蔽的下端向下方延伸,前述輻射屏蔽係配置於形成於前述坩堝內的前述矽融液的上方且包圍提拉的單晶的周圍;以及 於前述亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止前述坩堝的上升。 A single crystal pulling method is to pull a single crystal from a silicon melt contained in a crucible in a chamber by using the Czochralski method; The single crystal pulling method comprises the following steps: Before pulling the single crystal, the crucible is raised and the brightness of a light-transmitting pin member is detected, the pin member extends downward from the lower end of a cylindrical radiation shield, and the radiation shield is arranged above the silicon melt formed in the crucible and surrounds the pulled single crystal; and When the brightness exceeds a predetermined threshold value, it is determined that the lower end of the pin member contacts the silicon melt and the lifting of the crucible is stopped. 如請求項5所記載之單晶提拉方法,其中於前述亮度超過預定臨限值時判斷為前述銷構件的下端接觸於前述矽融液並停止前述坩堝的上升之步驟之後,具備如下步驟: 使前述坩堝下降達至下述距離:從自前述輻射屏蔽的下端至前述矽融液為止之間隙的期望值減去自前述銷構件的前述輻射屏蔽的下端至前述銷構件的前端為止之已知的長度所得之距離。 The single crystal pulling method described in claim 5, wherein after the step of judging that the lower end of the pin member contacts the silicon melt when the brightness exceeds a predetermined threshold value and stopping the ascent of the crucible, the following step is included: The crucible is lowered to the following distance: the distance obtained by subtracting the known length from the lower end of the radiation shield of the pin member to the front end of the pin member from the expected value of the gap from the lower end of the radiation shield to the silicon melt. 如請求項5所記載之單晶提拉方法,其中前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的25%以上的值所得之值。A single crystal pulling method as described in claim 5, wherein the predetermined threshold value of the brightness is a value obtained by adding a value of 25% or more of the baseline brightness to a value when the pin member is not in contact with the silicon melt. 如請求項5所記載之單晶提拉方法,其中前述亮度的預定臨限值為在前述銷構件未接觸於前述矽融液的狀態下之基準亮度加上前述基準亮度的50%以上的值所得之值。A single crystal pulling method as described in claim 5, wherein the predetermined threshold value of the brightness is a value obtained by adding a value of 50% or more of the baseline brightness to a value when the pin member is not in contact with the silicon melt.
TW112122510A 2022-10-13 2023-06-16 Single crystal pulling device and single crystal pulling method TW202415817A (en)

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