WO2020100512A1 - 単結晶の製造方法 - Google Patents

単結晶の製造方法 Download PDF

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Publication number
WO2020100512A1
WO2020100512A1 PCT/JP2019/040814 JP2019040814W WO2020100512A1 WO 2020100512 A1 WO2020100512 A1 WO 2020100512A1 JP 2019040814 W JP2019040814 W JP 2019040814W WO 2020100512 A1 WO2020100512 A1 WO 2020100512A1
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WIPO (PCT)
Prior art keywords
single crystal
diameter
raw material
crystal
yield
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Application number
PCT/JP2019/040814
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English (en)
French (fr)
Japanese (ja)
Inventor
直樹 永井
一徳 渡邉
鈴木　聡
義博 児玉
Original Assignee
信越半導体株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 信越半導体株式会社 filed Critical 信越半導体株式会社
Priority to CN201980072061.XA priority Critical patent/CN112996954B/zh
Priority to DE112019005137.7T priority patent/DE112019005137T5/de
Publication of WO2020100512A1 publication Critical patent/WO2020100512A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

Definitions

  • the present invention relates to a method for producing a single crystal by the FZ method, and more specifically, a method for producing a single crystal in which the remaining raw material crystal rods are reasonably utilized when the growth is stopped during the growth of the single crystal by the FZ method. Regarding the method.
  • high-purity silicon wafers manufactured by the FZ method have been used for manufacturing power devices such as high breakdown voltage power devices and thyristors.
  • caliber 8 inch (diameter 200 mm), 6 inch (diameter 150 mm), 5 inch (diameter 125 mm), 4 inch (diameter 100 mm) and smaller are manufactured. ..
  • a raw material crystal rod is heated and melted by an induction heating coil to form a floating zone, and an upper raw material crystal rod and a lower single crystal rod are relatively lowered with respect to the induction heating coil to form a floating zone.
  • the single crystal ingot is grown by moving it (see, for example, Patent Document 1).
  • FIG. 3 shows a generally used FZ single crystal production apparatus 30. A method of manufacturing a silicon single crystal using this FZ single crystal manufacturing apparatus 30 will be described.
  • a silicon raw material crystal rod 1 a silicon polycrystal rod manufactured by the Siemens method or a silicon single crystal rod manufactured by the CZ method is used.
  • the upper shaft 3 of the upper shaft 3 is previously attached to the upper side of the silicon raw material crystal rod 1 (the tail side when becoming a single crystal). A part of it is machined to hold it in the upper holding jig 4, the tip side is machined on the lower side (cone side when it becomes a single crystal) to facilitate seeding, and the straight body part is Machining or the like to obtain a desired diameter may be performed.
  • impurities are attached to the surface as it is, and therefore etching or cleaning is generally performed in order to manufacture a high-purity single crystal.
  • the silicon raw material crystal rod 1 is held by the upper holding jig 4 of the upper shaft 3 installed in the chamber 20. Then, a single crystal seed (seed crystal) 8 having a small diameter is held by the lower holding jig 6 of the lower shaft 5 located below the silicon raw material crystal rod 1.
  • the silicon raw material crystal rod 1 is melted by the induction heating coil 7 and fused to the seed crystal 8. After that, the narrowed portion 9 is formed by the seed narrowing to eliminate dislocation. Then, by lowering the silicon raw material crystal rod 1 and the silicon single crystal 2 while rotating the upper shaft 3 and the lower shaft 5, a floating zone 10 (also referred to as a melting zone or a melt) is formed in the silicon raw material crystal rod 1 and the silicon single crystal 2.
  • the silicon single crystal 2 is grown by moving the floating zone 10 to the upper end of the silicon raw material crystal rod 1 and zoning. This growth is performed in an atmosphere in which a small amount of nitrogen gas is mixed with Ar gas.
  • an induction heating coil made of copper or silver in which single or multiple winding water for cooling is circulated is used.
  • the silicon single crystal may become dislocations on the way before reaching the target weight.
  • the weight of the remaining silicon raw material crystal rod becomes larger than expected, and the weight of the remaining silicon raw material crystal rod measured is the minimum product according to the conventional flow of reusing the silicon raw material crystal rod shown in FIG. If the weight is large enough to be acquired, it can be used again for the FZ method.
  • a silicon single crystal (hereinafter, simply referred to as a single crystal) having a weight as large as possible from one silicon raw material crystal rod (hereinafter also simply referred to as a raw material crystal rod). It is preferable because it leads to yield improvement and cost improvement. The reason for this is that the silicon raw material crystal rod for producing a single crystal by the FZ method is expensive and occupies a large ratio to the cost of the produced single crystal.
  • crystal growth may be stopped midway due to unavoidable dislocations, earthquakes, and stoppages due to momentary blackouts.
  • the products of the FZ method are high-mix low-volume production, the required product quantity is very small, and the growth may be stopped midway. In these cases, the remaining weight of the silicon raw material crystal rod becomes large.
  • the present invention has been made in view of such a problem, and provides a method for producing a single crystal in which the yield reduction is suppressed by effectively utilizing the remaining raw material crystal rods when the crystal growth is stopped midway.
  • the purpose is to
  • the present invention forms a floating zone by heating and melting a raw material crystal rod with an induction heating coil, and the raw material crystal rod on the upper side and the single crystal rod on the lower side with respect to the induction heating coil.
  • a method for producing a single crystal by the FZ method in which the single crystal ingot is grown by relatively lowering while rotating, and moving the floating zone, When the growth is stopped during the crystal growth and the production of the single crystal by the FZ method is finished, a measurement step of measuring the weight of the remaining raw material crystal rods, The theoretical yield of the single crystal straight body part excluding the cone part and the tail part with respect to the remaining raw material crystal rod of the single crystal rod that can be theoretically produced from the remaining raw material crystal rod is calculated from the measured weight, and the crystal is obtained.
  • the diameter of the first single crystal before the growth is stopped in the middle of the growth is less than or equal to the predetermined reference yield, the maximum diameter of the single crystal that can be produced again using the remaining raw material crystal rods is determined, or If the predetermined reference yield is not satisfied, a determination step of determining not to manufacture a single crystal with the remaining raw material crystal rods, When the maximum diameter of the re-manufacturable single crystal is determined, it has a re-manufacturing step of manufacturing a single crystal with the maximum diameter of the re-manufacturable single crystal determined using the remaining raw material crystal rods.
  • a method for producing a characteristic single crystal is provided.
  • the manufacturing cost can be reduced as compared with the conventional case by not manufacturing the single crystal.
  • the diameter of the manufacturable single crystal, and the minimum yield for each diameter of the manufacturable single crystal as the reference yield is predetermined, Can be manufactured from the remaining raw material crystal rods, perform the first calculation process to calculate the theoretical yield of the diameter of the first manufactured single crystal, If the theoretical yield of the diameter of the initially produced single crystal is greater than or equal to the minimum yield determined for each diameter, the same diameter is used as the maximum diameter of the single crystal that can be produced again, and if it is less than the minimum yield determined for each diameter.
  • Performing a first determination process of setting a provisional maximum diameter of the single crystal to be one size smaller than the predetermined diameter of the manufacturable single crystal Again, it can be produced from the remaining raw material crystal rods, perform a calculation process to calculate the theoretical yield of the temporary maximum diameter of the single crystal, If the theoretical yield of the provisional maximum diameter of the single crystal is equal to or more than the minimum yield determined for each diameter, the diameter is the maximum diameter of the single crystal that can be manufactured again, and if the minimum yield is less than the minimum yield determined for each diameter, A determination process is performed to reset the provisional maximum diameter of the single crystal to a diameter smaller by one size among the predetermined diameters of the manufacturable single crystals, and the provisional maximum diameter of the reset single crystal is used. Repeating the calculation process and the determination process, if the theoretical yield calculated at the predetermined minimum diameter of the diameter of the manufacturable single crystal is smaller than the minimum yield determined for each diameter, the single crystal should not be manufactured. It is preferable to determine.
  • the product yield can be improved more easily and reliably than before, and the manufacturing cost can be reduced.
  • the weight of the remaining raw material crystal rod is measured, and from the raw material crystal rod of that weight, the diameter of the first produced single crystal or less, the maximum diameter of the single crystal satisfying the reference yield Since it becomes possible to manufacture a single crystal having an appropriate diameter, it is possible to effectively use the raw material crystal ingot, and it is possible to improve the product yield more than ever before. Further, when the predetermined reference yield is not satisfied, the manufacturing cost can be reduced as compared with the conventional case by not manufacturing the single crystal.
  • the inventors of the present invention can suppress the yield reduction by effectively utilizing the remaining raw material crystal rods when the crystal growth is stopped midway. Understood, the present invention was completed.
  • a raw material crystal rod is heated and melted by an induction heating coil to form a floating zone, and the upper raw material crystal rod and the lower single crystal rod are relatively rotated with respect to the induction heating coil.
  • the method for producing a single crystal by the FZ method in which the single crystal ingot is grown by moving the floating zone to a low temperature, the growth is stopped during the crystal growth, and the production of the single crystal by the FZ method is completed.
  • the theoretical yield of the straight body is calculated from the measured weight, the diameter of the first single crystal before the growth is stopped before the growth is stopped during the crystal growth, and the predetermined standard yield is satisfied, the remaining raw material crystals.
  • a determination step to determine that the remaining raw material crystal rod does not produce a single crystal is included.
  • a remanufacturing step of manufacturing a single crystal with the maximum diameter of the re-manufacturable single crystal determined using the remaining raw material crystal rods is included. And a method for producing a single crystal.
  • a judgment standard in the judgment step of the method for producing a single crystal of the present invention for example, a criterion used in the flow of reusing a silicon source crystal ingot as shown in FIG. 1 can be created.
  • the diameter of the single crystal that can be manufactured first before the growth is stopped in the middle of crystal growth, the diameter of the single crystal that can be manufactured, and the minimum yield for each diameter of the single crystal that can be manufactured as the reference yield are set in advance. Set (A in FIG. 1).
  • the first calculation process is performed to calculate the theoretical yield of the diameter of the first single crystal produced before the growth was stopped at (D in FIG. 1). If the theoretical yield is equal to or higher than the minimum yield preset for each diameter, it is the same.
  • the diameter of the single crystal is determined to be the maximum diameter of the single crystal that can be produced again (F in FIG. 1).
  • the first determination process for making the diameter smaller is performed (H in FIG. 1).
  • the calculation process of calculating the theoretical yield of the provisional maximum diameter of the single crystal is performed, and if the theoretical yield is more than the minimum yield previously determined for each diameter,
  • the diameter is defined as the maximum diameter of the single crystal that can be manufactured again, and when the yield is smaller than the minimum yield, the determination processing is performed to reset the temporary maximum diameter of the single crystal to a diameter that is one size smaller than the predetermined diameter (E in FIG. 1). ).
  • the calculation process and the determination process are repeated with the temporary maximum diameter of the single crystal reset. If the theoretical yield calculated at the predetermined minimum diameter is smaller than the minimum yield at the minimum diameter, the product is not manufactured (I in FIG. 1).
  • the theoretical yield means a single crystal rod that is theoretically manufactured from the remaining raw material crystal rods after the growth is stopped during the crystal growth, except for the cone portion and the tail portion for the remaining raw material crystal rods. It is the yield of the straight body of the crystal.
  • the product yield can be improved more easily and reliably than before, and the manufacturing cost can be reduced.
  • the weight of the remaining raw material crystal rod is light, for example, the weight of the cone portion and the tail portion is less than the weight, it is apparent that the minimum yield cannot be reached at the same diameter as the diameter of the initially prepared single crystal, A diameter smaller than the diameter of the initially manufactured product can be temporarily determined as the temporary maximum diameter of the single crystal, and the calculation processing and the determination processing can be started from the diameter.
  • the diameters of the single crystals that can be manufactured are 8 inches (diameter 200 mm), 6 inches (diameter 150 mm), 5 inches (diameter 125 mm), 4 inches (diameter 100 mm), 3 inches (diameter 75 mm), 60 mm, 2 Inches (diameter 50 mm) and the like can be selected, but the product diameter to be manufactured is not limited to this.
  • a single crystal is actually manufactured by the FZ method. Then, when the growth is stopped during the growth due to a power outage, an earthquake or the like (B in FIG. 1), a measurement step of measuring the weight of the remaining silicon raw material crystal ingot is performed (C in FIG. 1).
  • the theoretical yield of the single crystal straight body is calculated from the measured weight, and is less than or equal to the diameter of the first single crystal produced before stopping the growth in the course of crystal growth, and the predetermined reference yield is satisfied.
  • the temporarily determined diameter is used as the temporary maximum diameter of the single crystal, and the theoretical yield of the diameter is calculated (D in FIG. 1). Then, in comparison with the predetermined minimum yield of the diameter (E in FIG. 1), if the yield is more than the minimum yield, the diameter is set as the maximum diameter of the single crystal that can be manufactured again (F in FIG. 1), and the minimum yield is calculated. If it is smaller, a determination process for resetting the diameter one size smaller than the diameter to the temporary maximum diameter is performed (H in FIG. 1), the theoretical yield is calculated again, and the same comparison as above is performed.
  • the re-manufacturing step of manufacturing the single crystal with the determined maximum diameter of the re-manufacturable single crystal is performed using the remaining raw material crystal rods ( G in FIG. 1).
  • a general FZ method single crystal manufacturing method can be used as a method of performing a single crystal remanufacturing process using the remaining raw material crystal rods.
  • a single crystal is manufactured through a cone process of growing a single crystal rod while expanding it to a desired diameter, and a straight body process of growing the single crystal rod while controlling the diameter of the single crystal rod to a constant diameter after the cone is formed.
  • the diameter of the single crystal is expanded to the maximum diameter of the single crystal that can be remanufactured, which has been determined in the determination step, and the single crystal having this diameter is grown.
  • a single crystal having a diameter of 8 inches (200 mm) according to the FZ method is determined based on whether the theoretical yield of the single crystal is equal to or higher than the minimum yield determined for each diameter below or smaller than the minimum yield determined for each diameter.
  • the remaining raw material crystal rods are used to remanufacture the single crystal having the maximum diameter satisfying the minimum yield defined for each of the following diameters as the reference yield by the flow as shown in FIG. went.
  • the determination step of the example it was not determined that the single crystal was not produced.
  • the product yield of the example is higher than that of the comparative example, and by using the method for producing a single crystal of the present invention, when the growth is stopped during the crystal growth and the production of the single crystal by the FZ method is completed, The remaining raw material crystal rods can be effectively used, and the product yield can be improved more than ever before. In addition, the manufacturing cost could be reduced by manufacturing a single crystal having the largest possible weight from the remaining raw material crystal rods.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an exemplification, has substantially the same configuration as the technical idea described in the scope of the claims of the present invention, and has the same operational effect It is included in the technical scope of the invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
PCT/JP2019/040814 2018-11-13 2019-10-17 単結晶の製造方法 WO2020100512A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201980072061.XA CN112996954B (zh) 2018-11-13 2019-10-17 单晶的制造方法
DE112019005137.7T DE112019005137T5 (de) 2018-11-13 2019-10-17 Verfahren zur Herstellung eines Einkristalls

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JP2018-212846 2018-11-13
JP2018212846A JP6996477B2 (ja) 2018-11-13 2018-11-13 単結晶の製造方法

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07206573A (ja) * 1994-01-17 1995-08-08 Komatsu Electron Metals Co Ltd 浮遊帯域溶融法における晶出結晶径の制御方法
JPH11278981A (ja) * 1998-03-26 1999-10-12 Shin Etsu Handotai Co Ltd Ｆｚ法半導体単結晶製造の監視方法
JP2017193461A (ja) * 2016-04-20 2017-10-26 株式会社Sumco 単結晶の製造方法および装置

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5880415B2 (ja) * 2012-12-06 2016-03-09 信越半導体株式会社 単結晶の製造方法
JP6064675B2 (ja) * 2013-02-28 2017-01-25 信越半導体株式会社 半導体単結晶棒の製造方法
JP6318938B2 (ja) * 2014-07-17 2018-05-09 株式会社Sumco 単結晶の製造方法及び製造装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07206573A (ja) * 1994-01-17 1995-08-08 Komatsu Electron Metals Co Ltd 浮遊帯域溶融法における晶出結晶径の制御方法
JPH11278981A (ja) * 1998-03-26 1999-10-12 Shin Etsu Handotai Co Ltd Ｆｚ法半導体単結晶製造の監視方法
JP2017193461A (ja) * 2016-04-20 2017-10-26 株式会社Sumco 単結晶の製造方法および装置

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CN112996954A (zh) 2021-06-18
JP2020079181A (ja) 2020-05-28
CN112996954B (zh) 2023-09-01
JP6996477B2 (ja) 2022-01-17
DE112019005137T5 (de) 2021-07-01

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