TW202140869A - Method for producing silicon single crystal - Google Patents

Method for producing silicon single crystal Download PDF

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TW202140869A
TW202140869A TW110105354A TW110105354A TW202140869A TW 202140869 A TW202140869 A TW 202140869A TW 110105354 A TW110105354 A TW 110105354A TW 110105354 A TW110105354 A TW 110105354A TW 202140869 A TW202140869 A TW 202140869A
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single crystal
crystal
oxygen concentration
silicon
pulling
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TWI751028B (en
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森由行
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日商環球晶圓日本股份有限公司
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Abstract

The purpose of the present invention is to provide a method for producing a silicon single crystal, whereby it becomes possible to keep an oxygen concentration required for the improvement in slip resistance by a thermal stress in the crystal and to prevent the occurrence of internal rearrangement upon the pulling up of the silicon single crystal. In a step for growing a straight barrel portion of a silicon single crystal, the correlational formula between the oxygen concentration A (*10<SP>18</SP> atoms/cm3) in the single crystal and the single crystal pulling up speed B (mm/min) is the formula: B = -1/4A+0.75, and the oxygen concentration in the single crystal is adjusted to A or more and the single crystal pulling up speed is adjusted to B or more.

Description

單晶矽的製造方法Method for manufacturing single crystal silicon

本發明係關於一種藉由柴可拉斯基(Czochralski)法(CZ法)提拉單晶矽之單晶矽的製造方法,特別是關於一種能夠將在單晶矽之提拉中的內部差排(dislocation)(有差排化)予以抑制之單晶矽的製造方法。The present invention relates to a method for manufacturing single crystal silicon by pulling single crystal silicon by the Czochralski method (CZ method), and particularly relates to a method that can reduce the internal difference in the pulling of single crystal silicon A method of manufacturing single crystal silicon that suppresses dislocation (dislocation).

由CZ法所為的單晶矽之育成係藉由如下進行:對如圖9所示般的設置於腔室50內之石英坩堝51填充作為原料的多晶矽(polysilicon),藉由被設置於石英坩堝51之周圍的加熱器52將多晶矽加熱熔融,做成矽熔液M之後,將被安裝於晶種夾具(seed chuck)的種晶(晶種)P浸漬於該矽熔液,一邊使晶種夾具以及石英坩堝51於同方向或反方向旋轉一邊提拉晶種夾具。The breeding system of single crystal silicon by the CZ method is carried out by filling the quartz crucible 51 installed in the chamber 50 as shown in FIG. The heater 52 around 51 heats and melts the polysilicon to form a silicon melt M. Then, the seed crystal (seed crystal) P installed in the seed chuck is immersed in the silicon melt while making the seed crystal The clamp and the quartz crucible 51 rotate in the same direction or in the opposite direction while pulling the seed crystal clamp.

一般來說,在提拉開始之前,矽熔液M的溫度穩定後,進行使種晶P與矽熔液M接觸來熔解種晶P之前端部的頸縮(necking)。所謂的頸縮,是用以藉由因種晶P與矽熔液M接觸所產生之熱震(thermal shock)來去除產生於單晶矽的差排的不可欠或缺之工序。 藉由該頸縮而形成有頸部P1。又,該頸部P1一般來說需要是直徑為3 mm至4 mm,長度為30 mm至40 mm以上。Generally speaking, before the start of pulling, after the temperature of the silicon melt M is stabilized, the necking of the front end of the seed crystal P is performed by contacting the seed crystal P with the silicon melt M to melt the seed crystal P. The so-called necking is an indispensable process for removing the differential row caused by the single crystal silicon by thermal shock caused by the contact between the seed crystal P and the silicon melt M. The neck P1 is formed by this necking. In addition, the neck P1 generally needs to have a diameter of 3 mm to 4 mm and a length of 30 mm to 40 mm or more.

又,以作為提拉開始後的工序來說,進行有:肩部C1的形成工序,係在頸縮結束後使結晶擴展至直體部直徑為止;直體部C2的形成工序,係將作為製品之單晶予以育成;以及尾部(不圖示)的形成工序,係將直體部形成工序後的單晶直徑緩緩地縮小。In addition, as a step after the start of the pulling, the following steps are carried out: the step of forming the shoulder C1 is to expand the crystal to the diameter of the straight body after the necking is completed; the step of forming the straight body C2 is to be The single crystal of the product is grown; and the step of forming the tail (not shown) is to gradually reduce the diameter of the single crystal after the step of forming the straight body.

然而,若在前述單晶矽的提拉工序時結晶有差排化,則從有差排化的結晶所切出的晶圓係包含很多差排,因此無法使用於器件(device)之製造。 針對此種課題,於專利文獻1(日本特開2006-347853號)揭露有一種單晶矽的育成方法,係使育成單晶時的氛圍氣體(atmosphere gas)含有含氫原子物質之氣體,藉此將因熱應力而起的有差排化予以抑制。However, if the crystals are misaligned during the pulling process of the aforementioned single crystal silicon, the wafers cut from the misaligned crystals contain many misalignments, and therefore cannot be used in the manufacture of devices. In response to this problem, Patent Document 1 (Japanese Patent Application Laid-Open No. 2006-347853) discloses a method for growing single crystal silicon, in which the atmosphere gas during single crystal growing contains a gas containing hydrogen atoms. This will suppress the differential displacement due to thermal stress.

具體來說,將在前述氛圍氣體中的含氫原子物質之氣體的氫分子分壓設為40 Pa至400 Pa,並且在將前述含氫原子物質之氣體的氫分子換算之濃度設為α且氧氣體濃度設為β時,使在前述氛圍氣體中的氧氣體之濃度符合體積的比例為α-2β≧3%。Specifically, the partial pressure of hydrogen molecules of the gas containing hydrogen atoms in the aforementioned atmospheric gas is set to 40 Pa to 400 Pa, and the concentration of the hydrogen molecules of the gas containing hydrogen atoms is set to α and When the oxygen gas concentration is set to β, the ratio of the oxygen gas concentration in the aforementioned atmosphere to the volume is α-2β≧3%.

根據專利文獻1所揭露之方法,由於含氫原子物質之氣體中的氫元素進入晶矽之晶格間,因此等同於提高晶矽之晶格間原子的濃度,能夠使在矽凝固的過程中從矽熔液被取入至結晶內的晶格間原子之數量減低。 藉此,能夠抑制以由熱應力所產生之差排團簇(dislocation cluster)(作為過剩的晶格間矽之聚集體(aggregate)而形成的10 μm左右之缺陷)為起點的滑移差排(slip dislocation)。According to the method disclosed in Patent Document 1, since the hydrogen element in the gas containing hydrogen atoms enters the crystal lattice of crystalline silicon, it is equivalent to increasing the concentration of atoms between the crystal lattices of crystalline silicon, which can make the silicon solidify during the process of solidification. The number of inter-lattice atoms taken from the silicon melt into the crystal is reduced. As a result, it is possible to suppress slip dislocation clusters (dislocation clusters) (defects around 10 μm formed as aggregates of excess inter-lattice silicon) caused by thermal stress as the starting point. (slip dislocation).

另外,於專利文獻2(日本特開2002-187796號)揭露有一種方法,係在施加磁場提拉單晶時,於育成中的單晶有差排化之情形下,不施加磁場地將加熱器的輸出提高到比單晶製造條件還高來熔解前述有差排化的單晶,之後再度施加磁場並且將加熱器的輸出設為前述單晶製造條件來再度提拉前述單晶。In addition, Patent Document 2 (Japanese Patent Application Laid-Open No. 2002-187796) discloses a method of heating the single crystal without applying a magnetic field when the single crystal in the growing process is differentially displaced when a magnetic field is applied to pull the single crystal. The output of the heater is increased to be higher than the single crystal manufacturing conditions to melt the aforementioned differentially aligned single crystals, and then a magnetic field is applied again and the heater output is set to the aforementioned single crystal manufacturing conditions to pull the single crystals again.

根據此方法,在不施加磁場地進行過回熔(meltback)(再熔融化)後的單晶提拉時,熔液表面的異物被取入至單晶內的情形被抑制,變得能夠抑制在肩部形成工序中的有差排化,達成良率之大幅提升。 [先前技術文獻] [專利文獻]According to this method, when the single crystal is pulled after meltback (remelting) without applying a magnetic field, the foreign matter on the surface of the melt is prevented from being taken into the single crystal, and it becomes possible to suppress The difference in the shoulder formation process is eliminated, and the yield rate is greatly improved. [Prior Technical Literature] [Patent Literature]

[專利文獻1]日本特開2006-347853號。 [專利文獻2]日本特開2002-187796號。[Patent Document 1] Japanese Patent Laid-Open No. 2006-347853. [Patent Document 2] Japanese Patent Application Laid-Open No. 2002-187796.

[發明所欲解決之課題][The problem to be solved by the invention]

然而,一般來說晶格間原子導入量係伴隨著單晶之提拉速度低速化而變多,往結晶內的應變(strain)導入量有增加的傾向。另一方面,滑移抗性(slip resistance)係伴隨著往結晶內的氧導入量變多而有變高的傾向。 在此,當結晶中的應變量增加而應變與滑移抗性之間的均衡崩壞時,從應力大的結晶中央部導入有差排。由於此種差排是於結晶內部產生(稱作內部差排),故在結晶表面上作為有差排/無差排之指標的晶癖線(crystal habit line)不會消失,要確認差排的話,切片成晶圓狀後的檢査是需要的。 然而,在專利文獻1、2所揭露之發明中,是以能夠藉由有無前述晶癖線來判定的差排為基準,並沒有考慮前述內部差排。However, generally speaking, the amount of inter-lattice atoms introduced increases as the pulling rate of the single crystal decreases, and the amount of strain introduced into the crystal tends to increase. On the other hand, slip resistance tends to increase as the amount of oxygen introduced into the crystal increases. Here, when the amount of strain in the crystal increases and the balance between the strain and the slip resistance collapses, a difference is introduced from the center of the crystal where the stress is large. Since this kind of row is generated inside the crystal (called internal row), the crystal habit line (crystal habit line) on the crystal surface as an indicator of poor row/no row will not disappear. If you want to confirm the row , Inspection after slicing into wafer shape is required. However, the inventions disclosed in Patent Documents 1 and 2 are based on the margin that can be determined by the presence or absence of the aforementioned crystal wobble line, and the aforementioned internal margin is not taken into consideration.

本案發明人係著眼於結晶提拉速度與結晶氧濃度之間的關係,該結晶提拉速度係影響應變量,該結晶氧濃度係影響應變與用以保持均衡的滑移抗性,苦心研究結果,找出在由CZ法所為的單晶矽之育成時,能夠藉由控制結晶氧濃度與提拉速度來抑制結晶的內部差排,以至完成本發明。The inventor of this case focused on the relationship between the crystal pulling speed and the crystal oxygen concentration. The crystal pulling speed affects the amount of strain, and the crystal oxygen concentration affects the strain and the slip resistance to maintain a balance. The results of painstaking research , To find out that during the incubation of single crystal silicon by the CZ method, it is possible to control the crystal oxygen concentration and the pulling speed to suppress the internal difference of crystals, and complete the present invention.

本發明係在如前述的事情之下所完成,目的為提供一種單晶矽的製造方法,係能夠在結晶中確保用以提升滑移抗性的氧濃度,並且能夠防止在提拉單晶矽時產生內部差排。 [用以解決課題之手段]The present invention is completed under the aforementioned matters, and its purpose is to provide a method for manufacturing single crystal silicon, which can ensure the oxygen concentration in the crystallization for improving the slip resistance, and can prevent the pulling of the single crystal silicon. When generating internal differences. [Means to solve the problem]

為了解決前述課題所完成的本發明之單晶矽的製造方法係藉由柴可拉斯基法提拉單晶矽,在前述單晶矽的直體部育成工序中,將前述單晶矽中的氧濃度之值A(×1018 atoms/cm3 )與單晶提拉速度之值B(mm/min)之相關式設為B=-1/4A+0.75,以前述單晶矽中的氧濃度與前述單晶提拉速度分別成為滿足前述相關式之A與B以上的值之方式進行控制。In order to solve the aforementioned problems, the manufacturing method of the single crystal silicon of the present invention is accomplished by pulling the single crystal silicon by the Tchaikrasky method. The correlation formula between the oxygen concentration value A (×10 18 atoms/cm 3 ) and the single crystal pulling speed B (mm/min) is set as B=-1/4A+0.75, and the value of the single crystal silicon The oxygen concentration and the aforementioned single crystal pulling speed are controlled so that they meet the values of A and B or more in the aforementioned correlation equation, respectively.

根據這樣的本案發明,以結晶直體部之育成中的結晶中的氧濃度與提拉速度成為基於它們的相關式決定的各自之臨限值(threshold value)以上的方式對它們進行控制,育成了單晶矽。 藉此,能夠在結晶中確保滑移抗性提升的氧濃度,又,因為得以確保由前述相關式決定的臨限值以上之提拉速度,故晶格間原子之導入量被抑制而應變變得難以在結晶內部累積,能夠抑制以結晶中之應變為原因而產生的內部差排產生。According to the invention of this case, the oxygen concentration and the pulling speed in the crystals during the growth of the straight body part of the crystals are controlled so that they are above their respective threshold values determined based on their correlation equations. Single crystal silicon. Thereby, it is possible to ensure the oxygen concentration for improving the slip resistance in the crystal, and since the pulling speed above the threshold determined by the aforementioned correlation equation is ensured, the amount of introduction of atoms between the lattices is suppressed and the strain is changed. It is difficult to accumulate inside the crystal and can suppress the generation of internal dislocations caused by the strain in the crystal.

另外,前述單晶矽中的氧濃度之下限值較期望為0.4×1018 atoms/cm3 ,上限值較期望為1.8×1018 atoms/cm3 。 又,較期望為將前述直體部之結晶軸部中的熱應力設為米賽斯應力(von Mises stress)18 MPa以下。在前述氧濃度與提拉速度被控制成成為基於相關式決定的各自之臨限值以上的情形下,能夠將結晶軸部的熱應力設為米賽斯應力18 MPa以下之小的熱應力。 [發明功效]In addition, the lower limit of the oxygen concentration in the aforementioned single crystal silicon is more desirably 0.4×10 18 atoms/cm 3 , and the upper limit is more desirably 1.8×10 18 atoms/cm 3 . In addition, it is more desirable to set the thermal stress in the crystal axis portion of the straight body portion to be less than or equal to 18 MPa von Mises stress. In the case where the aforementioned oxygen concentration and the pulling rate are controlled to be equal to or higher than their respective threshold values determined based on the correlation equation, the thermal stress of the crystal shaft can be made as small as the Mises stress of 18 MPa or less. [Efficacy of invention]

根據本發明,能夠提供一種單晶矽的製造方法,係能夠將用以提升由熱應力所致的滑移抗性之氧濃度在結晶中予以確保,並且能夠防止在提拉單晶矽時產生內部差排。According to the present invention, it is possible to provide a method for manufacturing single crystal silicon, which can ensure the oxygen concentration for improving the slip resistance caused by thermal stress in the crystal, and can prevent the generation of single crystal silicon during pulling. Internally poorly arranged.

以下,使用圖式說明本發明之單晶矽的製造方法。圖1是實施有本發明之單晶矽的製造方法之單晶提拉裝置的剖視圖。圖2是表示由圖1的單晶提拉裝置所為之單晶矽的製造方法之流程的流程圖。Hereinafter, the method of manufacturing the single crystal silicon of the present invention will be explained using drawings. FIG. 1 is a cross-sectional view of a single crystal pulling device implemented with a method of manufacturing a single crystal silicon of the present invention. FIG. 2 is a flowchart showing the flow of a single crystal silicon manufacturing method by the single crystal pulling device of FIG. 1.

該單晶提拉裝置1係具備在圓筒形狀的主腔室10a之上重疊提拉腔室(pull chamber)10b而形成的爐體10,且具備:碳基座(carbon susceptor)(或石墨基座)2,係被設置成能夠在該爐體10內繞鉛直軸旋轉且能夠升降;以及石英玻璃坩堝3(以下單以坩堝3稱之),係由前述碳基座2所保持。The single crystal pulling device 1 is provided with a furnace body 10 formed by overlapping a pull chamber 10b on a cylindrical main chamber 10a, and is provided with a carbon susceptor (or graphite The base) 2 is set to be able to rotate around a vertical axis in the furnace body 10 and can be raised and lowered; and the quartz glass crucible 3 (hereinafter simply referred to as the crucible 3) is held by the aforementioned carbon base 2.

前述坩堝3係具有直體部3a以及形成於直體部3a之下的底部3b,且被設為能夠與碳基座2之旋轉一起繞鉛直軸旋轉。 又,於碳基座2之下方係設置有:旋轉馬達等的旋轉驅動部14,係使該碳基座2繞鉛直軸旋轉;以及升降驅動部15,係使碳基座2升降移動。 另外,於旋轉驅動部14係連接有旋轉驅動控制部14a,於升降驅動部15係連接有升降驅動控制部15a。The aforementioned crucible 3 has a straight body portion 3a and a bottom portion 3b formed under the straight body portion 3a, and is configured to be able to rotate around a vertical axis together with the rotation of the carbon base 2. In addition, under the carbon base 2 are provided: a rotation drive unit 14 such as a rotary motor to rotate the carbon base 2 around a vertical axis; and an up-and-down drive unit 15 to move the carbon base 2 up and down. Moreover, the rotation drive control part 14a is connected to the rotation drive part 14, and the raising/lowering drive control part 15a is connected to the raising/lowering drive part 15. As shown in FIG.

又,單晶提拉裝置1係具備:電阻加熱的側部加熱器(side heater)4,係將被裝填於坩堝3的半導體原料(原料多晶矽)予以熔融而做成矽熔液M(以下單以熔液M稱之);以及提拉機構9,係捲起纜索(wire)6,將育成的矽單晶C提拉。於前述提拉機構9所具有的纜索6之前端係安裝有種晶P。In addition, the single crystal pulling device 1 is equipped with a resistance-heated side heater 4, which melts the semiconductor raw material (raw polysilicon) filled in the crucible 3 to form a silicon melt M (the following single It is called melt M); and the pulling mechanism 9 is a wire 6 which pulls the bred silicon single crystal C. A seed crystal P is installed at the front end of the cable 6 of the aforementioned pulling mechanism 9.

另外,於側部加熱器4係連接有將供給電力量予以控制的加熱器驅動控制部4a,於提拉機構9係連接有進行提拉機構9的旋轉驅動之控制的旋轉驅動控制部9a。 又,在該單晶提拉裝置1中,於爐體2之外側設置有磁場施加用電磁線圈8。當於該磁場施加用電磁線圈8施加有預定的電流時,對坩堝3內的矽熔液M施加有預定強度的水平磁場。於磁場施加用電磁線圈8係連接有進行磁場施加用電磁線圈8之動作控制的電磁線圈控制部8a。In addition, the side heater 4 is connected to a heater drive control unit 4a that controls the amount of supplied electric power, and the lifting mechanism 9 is connected to a rotation drive control unit 9a that controls the rotation drive of the lifting mechanism 9. In addition, in the single crystal pulling device 1, an electromagnetic coil 8 for applying a magnetic field is provided on the outer side of the furnace body 2. When a predetermined current is applied to the electromagnetic coil 8 for applying a magnetic field, a horizontal magnetic field of predetermined strength is applied to the silicon melt M in the crucible 3. The electromagnetic coil 8 for magnetic field application is connected with the electromagnetic coil control part 8a which performs operation control of the electromagnetic coil 8 for magnetic field application.

亦即,在本實施形態中係實施有對熔液M內施加磁場來育成單晶的MCZ(Magnetic field applied CZ;磁場施加柴可拉斯基)法,藉此控制矽熔液M之對流,謀求單晶化的穩定。That is, in this embodiment, a magnetic field applied CZ (Magnetic field applied CZ; magnetic field applied Czochralski) method is implemented to grow a single crystal by applying a magnetic field to the melt M, thereby controlling the convection of the silicon melt M. Seek the stability of single crystalization.

又,在形成於坩堝3內的熔液M之上方係配置有包圍矽單晶C的周圍的輻射護罩(radiation shield)7。該輻射護罩7係上部與下部形成有開口,針對育成中的矽單晶C將來自側部加熱器4、熔液M等的多餘輻射熱遮蔽,並且將爐內的氣體流予以整流。 另外,輻射護罩7的下端與熔液面之間的間隔係以因應育成的單晶之所期望之特性來維持預定的距離之方式進行控制。In addition, a radiation shield 7 surrounding the silicon single crystal C is arranged above the melt M formed in the crucible 3. The radiation shield 7 has openings formed on the upper and lower portions to shield the excess radiant heat from the side heater 4, the melt M, etc. from the growing silicon single crystal C, and to rectify the gas flow in the furnace. In addition, the interval between the lower end of the radiation shield 7 and the molten surface is controlled in such a way as to maintain a predetermined distance in accordance with the desired characteristics of the grown single crystal.

又,於輻射護罩7之內側係配置有圓筒狀的水冷體12。於該水冷體12係藉由冷卻水供給機構12a而供給有冷卻水,且構成為藉由循環來維持預定溫度。In addition, a cylindrical water cooling body 12 is arranged inside the radiation shield 7. The water cooling body 12 is supplied with cooling water by a cooling water supply mechanism 12a, and is configured to maintain a predetermined temperature through circulation.

又,該單晶提拉裝置1係具備具有儲存裝置11a與運算控制裝置11b的電腦11,且旋轉驅動控制部14a、升降驅動控制部15a、電磁線圈控制部8a、旋轉驅動控制部9a及冷卻水供給機構12a係分別與運算控制裝置11b連接。In addition, the single crystal pulling device 1 includes a computer 11 having a storage device 11a and an arithmetic control device 11b, and a rotation drive control unit 14a, an elevation drive control unit 15a, an electromagnetic coil control unit 8a, a rotation drive control unit 9a, and cooling The water supply mechanism 12a is connected to the arithmetic control device 11b, respectively.

在如此地構成的單晶提拉裝置1中,在育成例如直徑300 mm的矽單晶C之情形下,如接下來般地進行提拉。亦即,最初對坩堝3裝填原料多晶矽(例如350 kg),基於儲存在電腦11之儲存裝置11a的程式,開始結晶育成工序。In the single crystal pulling device 1 configured in this way, in the case of growing a silicon single crystal C having a diameter of, for example, 300 mm, pulling is performed as follows. That is, the crucible 3 is initially filled with raw material polysilicon (for example, 350 kg), and based on the program stored in the storage device 11a of the computer 11, the crystal incubation process is started.

首先,爐體10內設為預定的氛圍(氬氣等的惰性氣體為主),藉由側部加熱器4所進行的加熱將被裝填於坩堝3內的原料多晶矽熔融,做成熔液M(圖2的步驟S1)。進一步地,坩堝3在預定的高度位置以預定的旋轉速度(rpm)進行旋轉動作(圖2的步驟S2)。First, the furnace body 10 is set in a predetermined atmosphere (mainly inert gas such as argon), and the raw material polycrystalline silicon charged in the crucible 3 is melted by heating by the side heater 4 to form a melt M (Step S1 in Fig. 2). Further, the crucible 3 performs a rotation operation at a predetermined height position and a predetermined rotation speed (rpm) (step S2 in FIG. 2).

接下來,開始對磁場施加用電磁線圈8流動預定的電流,以設定在1000高斯(Gauss)至4000高斯之範圍內的磁通密度(例如2500高斯)開始對熔液M內施加有水平磁場(圖2的步驟S3)。 又,纜索6降下而種晶P與熔液M接觸,進行熔解種晶P之前端部的頸縮,頸部P1形成開始(圖2的步驟S4)。 當頸部P1形成時,將針對側部加熱器4的供給電力、提拉速度、磁場施加強度等作為參數來調整提拉條件,種晶P於坩堝3之旋轉方向的反方向以預定的旋轉速度開始旋轉。Next, start to flow a predetermined current to the electromagnetic coil 8 for magnetic field application, and start to apply a horizontal magnetic field ( Step S3 of Fig. 2). In addition, the cable 6 is lowered and the seed crystal P is in contact with the melt M, and the end of the melted seed crystal P is necked, and the formation of the neck P1 starts (step S4 in FIG. 2). When the neck P1 is formed, the power supply for the side heater 4, the pulling speed, the strength of the magnetic field, etc. are used as parameters to adjust the pulling conditions, and the seed crystal P rotates in a predetermined direction opposite to the direction of rotation of the crucible 3 The speed starts to spin.

然後,結晶徑緩緩地擴徑而形成有肩部C1(圖2的步驟S5),移行到形成作為製品部分之直體部C2的工序(圖2的步驟S6)。 在此,電腦11在直體部C2的育成中,在如圖3所示般將橫軸x設為結晶氧濃度之值A(×1018 atoms/cm3 )且將縱軸y設為提拉速度之值B(mm/min)時,將由一次函數之相關式B=-1/4A+0.75決定的A、B之值作為臨限值來控制提拉速度與結晶氧濃度,以使提拉速度與結晶氧濃度分別成為該臨限值以上的值。Then, the crystal diameter is gradually expanded to form a shoulder portion C1 (step S5 in FIG. 2), and it proceeds to the step of forming a straight body portion C2 as a product part (step S6 in FIG. 2). Here, in the cultivation of the straight body portion C2 by the computer 11, as shown in FIG. 3, the horizontal axis x is set to the value of crystal oxygen concentration A (×10 18 atoms/cm 3 ) and the vertical axis y is set to increase When the pulling speed value B (mm/min), the values of A and B determined by the correlation equation of the linear function B=-1/4A+0.75 are used as the threshold to control the pulling speed and the crystal oxygen concentration, so as to increase The pulling speed and the crystalline oxygen concentration are respectively above the threshold value.

具體來說,當將結晶氧濃度之值以成為例如作為製品之晶圓的目標氧濃度之值的方式設定,將A設為氧濃度之目標值時,將氧濃度之值A(×1018 atoms/cm3 )代入前述相關式得到的提拉速度之值B=-1/4A+0.75(mm/min)就設為提拉速度的臨限值。亦即,電腦11係以氧濃度成為目標值A以上之方式進行提拉控制,並且以目標值B以上的提拉速度進行提拉控制。Specifically, when the value of the crystal oxygen concentration is set to be the value of the target oxygen concentration of the wafer as a product, and A is set as the target value of the oxygen concentration, the oxygen concentration value A (×10 18 Atoms/cm 3 ) is substituted into the aforementioned correlation equation to obtain the value of the pulling speed B=-1/4A+0.75 (mm/min), which is set as the threshold of the pulling speed. That is, the computer 11 performs the pulling control so that the oxygen concentration becomes the target value A or more, and performs the pulling control at the pulling speed of the target value B or more.

在如此地育成前述結晶氧濃度之值為A之矽單晶C時,將提拉速度控制在B以上,藉此晶格間原子之導入量被抑制而應變變得難以在結晶內部累積,以結晶中之應變為原因而產生的內部差排之產生得以抑制。 另外,結晶氧濃度之值A之範圍較期望為0.4(×1018 atoms/cm3 )以上不滿1.8(×1018 atoms/cm3 )。這是因為對結晶氧濃度來說低氧濃度的界限是0.4(×1018 atoms/cm3 ),若為1.8(×1018 atoms/cm3 )以上則在結晶提拉中存在有差排化之疑慮。 又,提拉速度之值B之範圍較期望為0.3(mm/min)以上不滿1.1(mm/min)。這是因為對提拉速度來說,不滿0.3(mm/min)則在結晶提拉中有差排化的比例會增加,若為1.1(mm/min)以上則有結晶會變形之疑慮。When the silicon single crystal C whose crystal oxygen concentration value is A is grown in this way, the pulling rate is controlled to be higher than B, whereby the introduction of atoms between the lattices is suppressed and strain becomes difficult to accumulate in the crystal. The internal displacement caused by the strain in the crystal is suppressed. In addition, the range of the value A of the crystal oxygen concentration is more than expected to be 0.4 (×10 18 atoms/cm 3 ) or more and less than 1.8 (×10 18 atoms/cm 3 ). This is because the low oxygen concentration limit for crystal oxygen concentration is 0.4 (×10 18 atoms/cm 3 ), and if it is 1.8 (×10 18 atoms/cm 3 ) or more, there is a difference in crystal pulling. The doubts. Moreover, the range of the value B of the pulling speed is more than 0.3 (mm/min) and less than 1.1 (mm/min) than expected. This is because if the pulling speed is less than 0.3 (mm/min), the ratio of dislocation in the crystal pulling will increase, and if it is 1.1 (mm/min) or more, there is a concern that the crystal will be deformed.

另外,如接下來般地導入單晶中的氧。在矽熔液M貼著(沿著)坩堝3之側壁流動時,由於熔點中的矽為化學上活性,故矽熔液M係與坩堝3的石英成分反應,將坩堝3的側壁熔解,O(氧)被取入至矽熔液M中。In addition, oxygen in the single crystal was introduced as follows. When the silicon melt M flows against (along) the side wall of the crucible 3, since the silicon in the melting point is chemically active, the silicon melt M reacts with the quartz component of the crucible 3 to melt the side wall of the crucible 3, and O (Oxygen) is taken into the silicon melt M.

要控制從如此地導入O(氧)之矽熔液M所育成的單晶中之氧濃度,較佳為調整爐內壓(提高爐內壓則結晶氧濃度下降),藉此能夠控制矽熔液M的流動(對流)來進行。To control the oxygen concentration in the single crystal grown from the silicon melt M into which O (oxygen) is introduced, it is better to adjust the furnace pressure (increase the furnace pressure, the crystal oxygen concentration will decrease), thereby controlling the silicon melting The flow (convection) of the liquid M is performed.

又,藉由調整水冷體12之溫度,所育成的直體部C2之溫度被冷卻到例如1412℃至800℃,結晶軸部的熱應力被抑制在米賽斯應力例如18 MPa以下。 如此地將結晶內部的熱應力抑制得低,在直體部C2之育成中,結晶氧濃度被控制在目標值A以上,藉此確保結晶氧導入量而提升滑移抗性。Furthermore, by adjusting the temperature of the water cooling body 12, the temperature of the cultivated straight body part C2 is cooled to, for example, 1412°C to 800°C, and the thermal stress of the crystal shaft part is suppressed to the Mises stress, for example, 18 MPa or less. In this way, the thermal stress inside the crystal is suppressed to be low, and the crystal oxygen concentration is controlled above the target value A during the growth of the straight body portion C2, thereby ensuring the amount of crystal oxygen introduced and improving the slip resistance.

隨著單晶矽C的直體部C2之形成的進行,收容坩堝3的碳基座2係上升移動,維持住熔液面M1相對於位置固定之輻射護罩7以及側部加熱器4的位置。 又,施加有以例如1000高斯至4000高斯之範圍,更佳為2000高斯至3000高斯所設定的磁通密度之磁場,藉此熔液M的自然對流得以抑制。另外,若於800高斯至1000高斯之範圍將水平磁場的磁通密度設定得低,則熔液M會變得不穩定,結晶變形容易產生。As the formation of the straight body C2 of the single crystal silicon C progresses, the carbon susceptor 2 containing the crucible 3 moves up and moves to maintain the melt level M1 relative to the fixed position of the radiation shield 7 and the side heater 4 Location. In addition, a magnetic field with a magnetic flux density set in the range of, for example, 1000 Gauss to 4000 Gauss, and more preferably 2000 Gauss to 3000 Gauss is applied, whereby the natural convection of the melt M is suppressed. In addition, if the magnetic flux density of the horizontal magnetic field is set to be low in the range of 800 Gauss to 1000 Gauss, the melt M becomes unstable and crystal deformation is likely to occur.

然後,當形成有直體部C2直至預定的長度時,移行到最後的尾部工序(圖2的步驟S7)。在該尾部工序中,結晶下端與熔液M之接觸面積會緩緩地變小,將矽單晶C與熔液M切離,單晶矽被製造出來。Then, when the straight body portion C2 is formed to a predetermined length, it proceeds to the final tail portion step (step S7 in FIG. 2). In this tail process, the contact area between the lower end of the crystal and the melt M will gradually decrease, and the silicon single crystal C and the melt M are cut away, and the single crystal silicon is manufactured.

如以上般,根據本實施形態,以結晶直體部之育成中的結晶中的氧濃度與提拉速度成為基於它們的相關式決定的各自之臨限值以上的方式對它們進行控制,育成了單晶矽。又,在直體部育成中,結晶軸部的熱應力被抑制在米賽斯應力18 MPa以下。 藉此,能夠在結晶中確保用以提升滑移抗性的氧濃度,又,因為得以確保由前述相關式決定的臨限值以上之提拉速度,故晶格間原子之導入量被抑制而應變變得難以在結晶內部累積,能夠抑制以結晶中之應變為原因而產生的內部差排產生。 [實施例]As described above, according to the present embodiment, the oxygen concentration and the pulling speed in the crystal during the growth of the straight body part of the crystal are controlled so that they are equal to or higher than their respective threshold values determined based on their correlation equations, and the growth is Single crystal silicon. In addition, in the straight body part growing, the thermal stress of the crystal shaft part is suppressed to less than 18 MPa Mises stress. Thereby, the oxygen concentration for improving the slip resistance can be ensured in the crystal, and since the pulling speed above the threshold determined by the aforementioned correlation equation can be ensured, the introduction amount of atoms between the lattices is suppressed. It becomes difficult for strain to accumulate inside the crystal, and it is possible to suppress the generation of internal displacement caused by the strain in the crystal. [Example]

基於實施例,進一步地說明本發明之單晶矽的製造方法。 (實驗1) 在實驗1中,在上述之實施形態所示的構成之單晶提拉裝置中,對坩堝投入360 kg的原料多晶矽,進行了直徑307 mm之單晶矽的提拉。為了抑制矽熔液的自然對流,在提拉中施加的水平磁場之磁通密度係設定為2500高斯。Based on the embodiment, the method of manufacturing the single crystal silicon of the present invention is further explained. (Experiment 1) In Experiment 1, in the single crystal pulling device of the configuration shown in the above embodiment, 360 kg of raw polycrystalline silicon was put into the crucible, and the single crystal silicon with a diameter of 307 mm was pulled. In order to suppress the natural convection of the silicon melt, the magnetic flux density of the horizontal magnetic field applied during the pulling is set to 2500 Gauss.

又,將包圍單晶之水冷體的溫度予以調整,將從單晶表面至水冷體表面之距離設為55 mm,將米賽斯應力調整至18 MPa以下。磁場強度係設為3000高斯。 又,使用氬氣體作為惰性氣體,惰性氣體之流量係設為130 l/min。又,將爐內壓設為15 Torr至80 Torr。進一步地,將坩堝的轉速設為0.5 rpm,單晶的轉速設為9.5 rpm(旋轉方向係設成互為反方向)。In addition, the temperature of the water cooling body surrounding the single crystal was adjusted, and the distance from the surface of the single crystal to the surface of the water cooling body was set to 55 mm, and the Mises stress was adjusted to 18 MPa or less. The magnetic field intensity is set to 3000 Gauss. In addition, argon gas was used as the inert gas, and the flow rate of the inert gas was set to 130 l/min. In addition, the furnace internal pressure is set to 15 Torr to 80 Torr. Furthermore, the rotation speed of the crucible was set to 0.5 rpm, and the rotation speed of the single crystal was set to 9.5 rpm (the rotation directions were set to be opposite to each other).

又,在實驗1中,實施了110次的提拉試驗。 然後,針對每個試驗設定作為目標之結晶氧濃度,將提拉速度做各種更換而進行了提拉。將實驗1中的各試驗之結果表示於圖4的圖表。 圖4的圖表是將縱軸y設為平均提拉速度(mm/min),將橫軸x設為結晶中央的氧濃度(1018 atoms/cm3 ),繪出各試驗中的平均提拉速度與結晶中央的氧濃度。 又,在各試驗中,將得到的單晶加工成已蝕刻晶圓(etched wafer),照射斜光來確認有無由面透射所造成的內部差排。然後,如圖4所示,在各試驗中將沒有內部差排的部分以◇表示,有內部差排的部分以×表示。In addition, in Experiment 1, 110 pull tests were carried out. Then, the target crystalline oxygen concentration was set for each test, and the pulling speed was changed variously to perform the pulling. The results of each test in Experiment 1 are shown in the graph of FIG. 4. The graph in Fig. 4 shows the average pulling rate (mm/min) on the vertical axis y and the oxygen concentration (10 18 atoms/cm 3 ) in the center of the crystal on the horizontal axis x. The average pulling rate in each test is plotted. The speed is related to the oxygen concentration in the center of the crystal. In addition, in each test, the obtained single crystal was processed into an etched wafer, and oblique light was irradiated to confirm the presence or absence of internal dislocations caused by surface transmission. Then, as shown in Figure 4, in each test, the parts without internal deviations are represented by ◇, and the parts with internal deviations are represented by ×.

根據該圖4的圖表,在相關式y=-1/4x+0.75(y是平均提拉速度(mm/min)且x是結晶中央的氧濃度(1018 atoms/cm3 ))中,將x=B時的y的值A設為平均提拉速度之臨限值,當結晶氧濃度成為B以上且提拉速度成為A以上時,判明了沒有內部差排。According to the graph in Figure 4, in the correlation equation y=-1/4x+0.75 (y is the average pulling speed (mm/min) and x is the oxygen concentration in the center of the crystal (10 18 atoms/cm 3 )), the The value A of y when x=B is set as the threshold value of the average pulling speed. When the crystal oxygen concentration becomes B or higher and the pulling speed becomes A or higher, it is determined that there is no internal displacement.

另外,將檢査有無內部差排時沒有內部差排之情形的照片表示於圖5中的(a),將有內部差排之情形的照片表示於圖5中的(b)。在圖5中的(b)所示的結果之例中,看得到數處5 mm至20 mm左右的大小之十字狀的反射,由於晶癖線沒有消失,因此可確認這些是內部差排。In addition, a photo of the situation where there is no internal runout when checking for internal runout is shown in (a) in FIG. 5, and a photo of the situation where there is an internal runout is shown in (b) in FIG. 5. In the example of the result shown in Fig. 5(b), several cross-shaped reflections with a size of about 5 mm to 20 mm are seen. Since the crystal habit lines have not disappeared, it can be confirmed that these are internal differences.

如該實驗1的結果及圖4的圖表所示,在用相關式y=-1/4x+0.75的x以目標氧濃度代入時的y的值以上提拉單晶之情形下,確認到內部差排不會產生。As shown in the results of this experiment 1 and the graph in Fig. 4, when the single crystal is pulled up to the value of y when the target oxygen concentration is substituted for x with the correlation equation y=-1/4x+0.75, it is confirmed that the inside Poor row will not occur.

(實驗2) 在實驗2中,將上述實驗1的條件之中影響到矽熔液之流動(對流)的磁通密度、惰性氣體之流量、爐內壓、坩堝以及單晶之轉速的條件予以變更。其他的條件係與實驗1的條件相同。 具體來說,磁通密度係設為2000高斯,惰性氣體之流量係設為130 l/min。又,將爐內壓設為15 Torr至80 Torr。進一步地,將坩堝之轉速設為0.5 rpm,單晶之轉速設為9.5 rpm(旋轉方向係設成互為反方向)。(Experiment 2) In experiment 2, among the conditions of experiment 1 above, the conditions that affect the flow (convection) of the silicon melt, the magnetic flux density, the flow rate of the inert gas, the furnace pressure, the crucible, and the rotation speed of the single crystal were changed. The other conditions are the same as those of Experiment 1. Specifically, the magnetic flux density is set to 2000 Gauss, and the flow rate of the inert gas is set to 130 l/min. In addition, the furnace internal pressure is set to 15 Torr to 80 Torr. Further, the rotation speed of the crucible was set to 0.5 rpm, and the rotation speed of the single crystal was set to 9.5 rpm (the rotation directions were set to be opposite to each other).

將實驗2中的各試驗之結果表示於圖6的圖表。圖6的圖表是將縱軸y設為平均提拉速度(mm/min),將橫軸x設為結晶中央的氧濃度(1018 atoms/cm3 ),繪出各試驗中的平均提拉速度與結晶中央的氧濃度。在各試驗中將沒有內部差排的部分以◇表示,有內部差排的部分以×表示。 如實驗2的結果及圖6的圖表所示,在用相關式y=-1/4x+0.75的x以目標氧濃度代入時的y的值以上提拉單晶之情形下,內部差排不會產生。The results of each test in Experiment 2 are shown in the graph of FIG. 6. The graph in Fig. 6 shows the average pulling speed (mm/min) on the vertical axis y and the oxygen concentration (10 18 atoms/cm 3 ) in the center of the crystal on the horizontal axis x. The average pulling rate in each test is plotted. The speed is related to the oxygen concentration in the center of the crystal. In each test, the parts without internal deviations are represented by ◇, and the parts with internal deviations are represented by ×. As shown in the results of Experiment 2 and the graph in Fig. 6, when the single crystal is pulled up to the value of y when the target oxygen concentration is substituted for x with the correlation formula y=-1/4x+0.75, the internal difference is not Will produce.

(實驗3) 在實驗3中,將上述實驗1、2的條件之中影響到矽熔液之流動(對流)的磁通密度、惰性氣體之流量、爐內壓、坩堝以及單晶之轉速的條件予以變更。其他的條件係與實驗1、2的條件相同。 具體來說,磁通密度係設為3000高斯,惰性氣體之流量係設為130 l/min。又,將爐內壓設為15 Torr至80 Torr。進一步地,將坩堝之轉速設為2.0 rpm,單晶之轉速設為9.5 rpm(旋轉方向係設成互為反方向)。(Experiment 3) In Experiment 3, among the conditions of Experiments 1 and 2 above, the conditions affecting the flow (convection) of the silicon melt, the magnetic flux density, the flow rate of the inert gas, the furnace pressure, the crucible, and the rotation speed of the single crystal were changed. The other conditions are the same as those of experiments 1 and 2. Specifically, the magnetic flux density is set to 3000 Gauss, and the flow rate of the inert gas is set to 130 l/min. In addition, the furnace internal pressure is set to 15 Torr to 80 Torr. Further, the rotation speed of the crucible was set to 2.0 rpm, and the rotation speed of the single crystal was set to 9.5 rpm (the rotation directions were set to be opposite to each other).

將實驗3中的各試驗之結果表示於圖7的圖表。圖7的圖表是將縱軸y設為平均提拉速度(mm/min),將橫軸x設為結晶中央的氧濃度(1018 atoms/cm3 ),繪出各試驗中的平均提拉速度與結晶中央的氧濃度。在各試驗中將沒有內部差排的部分以◇表示,有內部差排的部分以×表示。 如實驗3的結果及圖7的圖表所示,在用相關式y=-1/4x+0.75的x以目標氧濃度代入時的y的值以上提拉單晶之情形下,內部差排不會產生。The results of each test in Experiment 3 are shown in the graph of FIG. 7. The graph in Fig. 7 shows the average pulling speed (mm/min) on the vertical axis y and the oxygen concentration in the center of the crystal (10 18 atoms/cm 3 ) on the horizontal axis x. The average pulling rate in each test is plotted. The speed is related to the oxygen concentration in the center of the crystal. In each test, the part without internal deviation is indicated by ◇, and the part with internal deviation is indicated by ×. As shown in the results of Experiment 3 and the graph in Fig. 7, when the single crystal is pulled up to the value of y when the target oxygen concentration is substituted for x with the correlation equation y=-1/4x+0.75, the internal difference is not Will produce.

根據以上實驗1至3的結果,為了抑制內部差排產生,能夠定義平均提拉速度(mm/min)與結晶中央的氧濃度(1018 atoms/cm3 )之相關式y=-1/4x+0.75,在相關式y=-1/4x+0.75的x以目標氧濃度代入且用y的值以上提拉單晶之情形下,確認到內部差排不會產生。According to the results of the above experiments 1 to 3, in order to suppress the generation of internal dislocations, the correlation between the average pulling speed (mm/min) and the oxygen concentration in the center of the crystal (10 18 atoms/cm 3 ) can be defined as y=-1/4x +0.75, in the case where x in the correlation equation y=-1/4x+0.75 is substituted with the target oxygen concentration and the single crystal is pulled above the value of y, it is confirmed that no internal displacement will occur.

(實驗4) 在實驗4中,於上述實驗1的試驗之中,在提拉速度設為0.55 mm/min且結晶氧濃度設為1.1E18 atoms/cm3 之條件下,藉由模擬確認到於結晶內部產生的熱應力。 在該模擬中係使用STR(Semiconductor Technology Research)公司製作的綜合導熱解析軟體CGSim_Basic,作為參數設定了熱膨脹率2.6×10-6 K-1 、楊氏模數(Young's modulus)185 GPa、帕松比(Poisson’s ratio)0.28、密度2330 kg/m3 。 將該模擬結果表示於圖8。在圖8中,於固液界面上方150 mm附近的結晶軸部處確認到熱應力小到18 MPa,能夠使滑移抗性提升。(Experiment 4) In Experiment 4, in the experiment of the above experiment 1, under the condition that the pulling speed was set to 0.55 mm/min and the crystal oxygen concentration was set to 1.1E18 atoms/cm 3, it was confirmed by simulation that Thermal stress generated inside the crystal. In this simulation, the comprehensive thermal analysis software CGSim_Basic produced by STR (Semiconductor Technology Research) is used, and the thermal expansion coefficient is set as 2.6×10 -6 K -1 , Young's modulus 185 GPa, and Passon’s ratio. (Poisson's ratio) 0.28, density 2330 kg/m 3 . The simulation results are shown in FIG. 8. In Figure 8, it was confirmed that the thermal stress was as small as 18 MPa at the crystal axis near 150 mm above the solid-liquid interface, which improved the slip resistance.

從以上的實驗1至4之結果確認到:根據本發明,能夠防止在單晶的直體部育成中之應變為原因而產生的內部差排產生。From the results of the above experiments 1 to 4, it was confirmed that according to the present invention, it is possible to prevent the occurrence of internal dislocations caused by strain in the growth of the straight body portion of the single crystal.

1:單晶提拉裝置 2:碳基座 3:石英玻璃坩堝(坩堝) 3a:直體部 3b:底部 4:側部加熱器 4a:加熱器驅動控制部 6:纜索 7:輻射護罩 8:磁場施加用電磁線圈 8a:電磁線圈控制部 9:提拉機構 9a,14a:旋轉驅動控制部 10:爐體 10a:主腔室 10b:提拉腔室 11:電腦 11a:儲存裝置 11b:運算控制裝置 12:水冷體 12a:冷卻水供給機構 14:旋轉驅動部 15:升降驅動部 15a:升降驅動控制部 50:腔室 51:石英坩堝 52:加熱器 C:單晶矽 C1:肩部 C2:直體部 M:矽熔液(熔液) M1:熔液面 P:種晶 P1:頸部 S1~S7:步驟1: Single crystal pulling device 2: Carbon base 3: Quartz glass crucible (crucible) 3a: Straight body 3b: bottom 4: side heater 4a: Heater drive control unit 6: Cable 7: Radiation shield 8: Electromagnetic coil for magnetic field application 8a: Solenoid coil control unit 9: Lifting mechanism 9a, 14a: Rotation drive control unit 10: Furnace 10a: Main chamber 10b: Lifting chamber 11: Computer 11a: storage device 11b: Operational control device 12: Water cooling body 12a: Cooling water supply mechanism 14: Rotary drive part 15: Lifting drive 15a: Lifting drive control unit 50: Chamber 51: Quartz Crucible 52: heater C: Monocrystalline silicon C1: Shoulder C2: Straight body M: Silicon melt (melt) M1: Melt level P: seed crystal P1: neck S1~S7: steps

[圖1]是實施有本發明之單晶矽的製造方法之單晶提拉裝置的剖視圖。 [圖2]是表示由圖1的單晶提拉裝置所為之單晶矽的製造方法之流程的流程圖。 [圖3]是用以說明本發明之單晶矽的製造方法的圖表(graph)。 [圖4]是表示本發明的實驗1之結果的圖表。 [圖5]是表示本發明的實施例以及比較例之結果的照片。 [圖6]是表示本發明的實驗2之結果的圖表。 [圖7]是表示本發明的實驗3之結果的圖表。 [圖8]是表示本發明的實施例之結果的模擬影像。 [圖9]是用以說明藉由柴可拉斯基法提拉單晶矽之工序的剖視圖。[Fig. 1] is a cross-sectional view of a single crystal pulling device in which the method of manufacturing a single crystal silicon of the present invention is implemented. [FIG. 2] is a flowchart showing the flow of a method of manufacturing single crystal silicon by the single crystal pulling device of FIG. 1. [FIG. 3] is a graph for explaining the manufacturing method of the single crystal silicon of the present invention. Fig. 4 is a graph showing the results of Experiment 1 of the present invention. [Fig. 5] is a photograph showing the results of the Examples and Comparative Examples of the present invention. Fig. 6 is a graph showing the results of Experiment 2 of the present invention. Fig. 7 is a graph showing the results of Experiment 3 of the present invention. [Fig. 8] is a simulated video showing the result of the embodiment of the present invention. [Fig. 9] is a cross-sectional view for explaining the process of pulling single crystal silicon by the Tchaikrasky method.

S1~S7:步驟 S1~S7: steps

Claims (3)

一種單晶矽的製造方法,係藉由柴可拉斯基法提拉單晶矽; 在前述單晶矽的直體部育成工序中,將前述單晶矽中的氧濃度之值A×1018 atoms/cm3 與單晶提拉速度之值B mm/min之相關式設為B=-1/4A+0.75; 以前述單晶矽中的氧濃度與前述單晶提拉速度分別成為滿足前述相關式之A與B以上的值之方式進行控制。A method for manufacturing single crystal silicon is to pull the single crystal silicon by the Tchaikrasky method; in the step of growing the straight body of the single crystal silicon, the value of the oxygen concentration in the single crystal silicon is A×10 The correlation between 18 atoms/cm 3 and the single crystal pulling speed B mm/min is set as B=-1/4A+0.75; the oxygen concentration in the aforementioned single crystal silicon and the aforementioned single crystal pulling speed are satisfied respectively The above-mentioned correlation formula A and B above the value of the way to control. 如請求項1所記載之單晶矽的製造方法,其中前述單晶矽中的氧濃度之下限值為0.4×1018 atoms/cm3 ,上限值為1.8×1018 atoms/cm3The method for manufacturing single crystal silicon described in claim 1, wherein the lower limit value of the oxygen concentration in the single crystal silicon is 0.4×10 18 atoms/cm 3 , and the upper limit value is 1.8×10 18 atoms/cm 3 . 如請求項1或2所記載之單晶矽的製造方法,其中將前述直體部之結晶軸部中的熱應力設為米賽斯應力18 MPa以下。The method for manufacturing single crystal silicon as described in claim 1 or 2, wherein the thermal stress in the crystal axis portion of the straight body portion is set to 18 MPa or less of Mises stress.
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