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WO2005083160A1 - PROCÉDÉ DE FABRICATION D'UN MONOCRISTAL SEMI-CONDUCTEUR COMPOSÉ ET MONOCRISTAL ZnTe - Google Patents

PROCÉDÉ DE FABRICATION D'UN MONOCRISTAL SEMI-CONDUCTEUR COMPOSÉ ET MONOCRISTAL ZnTe Download PDF

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Publication number
WO2005083160A1
WO2005083160A1 PCT/JP2005/003348 JP2005003348W WO2005083160A1 WO 2005083160 A1 WO2005083160 A1 WO 2005083160A1 JP 2005003348 W JP2005003348 W JP 2005003348W WO 2005083160 A1 WO2005083160 A1 WO 2005083160A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
crystal
single crystal
raw material
compound semiconductor
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2005/003348
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English (en)
Japanese (ja)
Inventor
Toshiaki Asahi
Kenji Sato
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Mining Holdings Inc
Original Assignee
Nippon Mining and Metals Co Ltd
Nikko Materials Co Ltd
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.)
Filing date
Publication date
Application filed by Nippon Mining and Metals Co Ltd, Nikko Materials Co Ltd filed Critical Nippon Mining and Metals Co Ltd
Publication of WO2005083160A1 publication Critical patent/WO2005083160A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C30B15/12—Double crucible methods
    • 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
    • C30B27/00—Single-crystal growth under a protective fluid
    • C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
    • 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
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te

Definitions

  • the present invention relates to a method for producing a compound semiconductor single crystal by a liquid-sealed Czochralski (LEC) method and a technique useful for being applied to a ZnTe single crystal.
  • LOC liquid-sealed Czochralski
  • a ZnTe-based compound semiconductor single crystal is expected to be a crystal that can be used for a pure green light emitting device.
  • the present applicant has proposed a method of manufacturing a compound semiconductor single crystal by a liquid-sealed Czochralski method (LEC method) using a double crucible (Japanese Patent Application No. 2002-249963).
  • LOC method liquid-sealed Czochralski method
  • the above-mentioned prior application is characterized in that the crystal is grown so as to be substantially the same as the inner diameter of the inner crucible while maintaining the surface of the grown crystal covered with the liquid sealant until the crystal growth is completed.
  • one communication hole having an inner diameter of 1Z5 or less is provided on the bottom surface of the inner crucible to provide an introduction path for the raw material melt accommodated in the outer crucible, so that the temperature fluctuation of the raw material melt in the inner crucible is small.
  • Patent Documents 14 and 14 propose a technique for manufacturing a compound semiconductor single crystal by a LEC method using a double crucible.
  • Patent Documents 1 and 2 disclose multiple techniques near the bottom surface of an inner crucible.
  • a crystal growth apparatus provided with a communication hole is exemplified.
  • Patent Document 1 JP-A-61-26590
  • Patent Document 2 JP-A-63-195188
  • Patent Document 3 JP-A-62-288193
  • Patent Document 4 JP-A-60-27693
  • the inventors of the present invention utilized the above-mentioned prior application technique to grow a ZnTe single crystal by pulling it up in the ⁇ 110> direction by the LEC method. found. In addition, the obtained ZnTe single crystal did not grow at a uniform rate in the ⁇ 110> direction. It was a crystal with large distortion.
  • Patent Literature 2 exemplifies a method of growing an InAs single crystal in the ⁇ 100> direction
  • Patent Literature 4 discloses a method of growing a GaAs single crystal in the ⁇ 100> direction. Is illustrated.
  • Japanese Patent Application No. 2002-249963 exemplifies a method of growing a ZnTe-based compound semiconductor single crystal by pulling it in the ⁇ 100> direction.
  • Patent Documents 1 and 3 do not specifically describe the crystal orientation of the grown crystal!
  • the above-mentioned prior art is suitable for growing a compound semiconductor single crystal having a relatively good symmetry in a (100) orientation, but has a poor symmetry and a compound in a (110) orientation. It cannot be used as it is when growing a semiconductor single crystal.
  • An object of the present invention is to provide a method for producing a compound semiconductor single crystal capable of growing a compound semiconductor single crystal having a (110) orientation with excellent crystal quality.
  • the present invention has been completed based on the above findings, and has a first crucible having a bottomed cylindrical shape and a communication hole provided inside the first crucible and communicating with the first crucible.
  • a semiconductor material and a sealant are accommodated in a material melt accommodating portion composed of a crucible, and the material accommodating portion is heated to melt the material, and the material melt is covered with the sealant.
  • a method for producing a compound semiconductor single crystal by a liquid-sealed Czochralski method in which a seed crystal is brought into contact with a surface to grow the seed crystal while pulling the seed crystal, wherein the second crucible has a plurality of communication holes. And grow the crystal while pulling the seed crystal in the ⁇ 110> direction. It is characterized by that.
  • a plurality of communication holes are formed along the outer periphery of the bottom surface of the second crucible off the center, and the total area of the plurality of communication holes is 1Z10 or less of the bottom area of the second crucible.
  • the plurality of communication holes are provided at equal intervals along a circumference at a fixed distance from the center of the bottom surface of the second crucible.
  • the temperature fluctuation in the raw material melt in the second crucible can be reduced, and the crystal can be grown at a uniform rate in the ⁇ 110> direction.
  • the single crystallization ratio of the crystal can be improved.
  • a ZnTe single crystal having a plane orientation of (110) and a light transmittance of 20% or less can be obtained by the above-described manufacturing method.
  • the light transmittance here means that the first polarizing plate 22, the ZnTe single crystal substrate 23, and the second polarizing plate 24 are respectively placed on the optical path connecting the light source 21 and the photodiode 25.
  • the light receiving surface is arranged perpendicular to the optical path and the polarization directions A and B of the two polarizers 22 and 24 are adjusted to be perpendicular, based on the amount of transmitted light measured by the photodiode 25, It is calculated.
  • the amount of light received by the photodiode 25 is reduced by 100%. Is calculated as the light transmittance.
  • the crystal distortion of the ZnTe single crystal substrate 23 disposed between the two polarizing plates 22 and 24 is specified by a numerical value. In other words, it can be said that the smaller the light transmittance, the smaller the crystal distortion and the better the crystal quality.
  • a raw material melt comprising a bottomed cylindrical first crucible and a second crucible disposed inside the first crucible and provided with a communication hole with the first crucible.
  • a semiconductor material and a sealing material are housed in a housing part, the material housing part is heated to melt the raw material, and a seed crystal is brought into contact with the surface of the raw material melt in a state of being covered with the sealing material.
  • the crystal Since the crystal is grown while pulling the seed crystal in the direction, the temperature fluctuation in the raw material melt contained in the second crucible can be suppressed. As a result, it is possible to prevent the generation of twin crystal and polycrystal and to increase the single crystallization ratio, and to produce an effect of producing a semiconductor compound single crystal with a high yield.
  • a ZnTe single crystal having a plane orientation of (110) and a light transmittance of 20% or less obtained by the above-described manufacturing method has extremely small distortion and excellent crystallinity, and thus is suitable as a semiconductor device such as a light emitting element. It is.
  • FIG. 1 is a schematic configuration diagram of a crystal growth apparatus used in an embodiment of the present invention.
  • FIG. 2 is an enlarged view of a raw material accommodating portion of the crystal growth apparatus of FIG. 1, wherein (a) is a cross-sectional view and (b) is a top view.
  • FIG. 3 is a schematic view of a measuring device for measuring a light reception amount for calculating a light transmittance of a ZnTe single crystal wafer.
  • FIG. 1 is a schematic configuration diagram of a crystal growth apparatus according to the present embodiment.
  • the crystal growth apparatus 100 of the present embodiment includes a high-pressure vessel 1, a heat insulating material 2 and a heater 3 arranged concentrically with the high-pressure vessel, and a rotating shaft vertically arranged at the center of the high-pressure vessel 1. 4, a susceptor 13 arranged at the upper end of the rotating shaft 4, an outer crucible (first crucible) 5 made of pBN having a bottomed cylindrical shape fitted to the susceptor, and an inner crucible 5.
  • the inner crucible 6 has a communication hole 6 a on the bottom surface communicating with the outer crucible 5, and the raw material melt 12 can be moved from the outer crucible 5 to the inner crucible 6 via this communication hole. .
  • four communication holes 6a are provided on the bottom surface of the inner crucible 6 at equal intervals along a circumference at a fixed distance from the center of the bottom surface.
  • the inner crucible 6 is fixed to the outer crucible 5 or another jig by a suitable holder (not shown).
  • the inner crucible 6 has a tapered structure in which the inner diameter at the bottom is smaller than the inner diameter at the top, the diameter of the grown crystal that has been pulled up is smaller than the inner diameter at the corresponding position of the second crucible. And the grown crystal no longer contacts the crucible wall except at the growth interface
  • the rotary pulling shaft 7 is connected to a driving unit (not shown) arranged outside the high-pressure vessel to constitute a rotary pulling mechanism.
  • the rotating shaft 4 is connected to a driving unit (not shown) arranged outside the high-pressure vessel to constitute a crucible rotating mechanism and constitute a susceptor elevating mechanism.
  • the movements of the rotation and lifting shaft 7 and the crucible rotation shaft 4 and the movement of the elevating movement are set and controlled independently of each other.
  • the plurality of communication holes 6a are provided at positions off the center of the bottom surface of the inner crucible 6, temperature fluctuation in the raw material melt accommodated in the inner crucible 6 is suppressed.
  • the crystal can be grown at a uniform speed in the ⁇ 110> direction. That As a result, it is possible to prevent twins and polycrystals from being generated, to increase the single crystallization ratio, and to produce a single crystal with a high yield.
  • a (110) oriented ZnTe single crystal was produced as an example of a compound semiconductor.
  • a crucible made of ⁇ having an inner diameter of 100 mm ⁇ ⁇ 100 mm height ⁇ lmm thickness is used as the outer crucible 5, and a taper structure having an inner diameter of 54 mm ⁇ —56 mm ⁇ ⁇ 100 mm height ⁇ lmm thickness lmm is used as the inner knurling 6.
  • a crucible made of pBN was used.
  • the bottom surface of the inner crucible 6 is provided with four communication holes 6a at positions that are rotated by 90 ° from each other on a circle having a diameter of 50 mm and concentric with the bottom surface.
  • the diameter of the communication hole 6a was 4 mm.
  • the size of the communication hole 6a is not limited to 4 mm, and it is sufficient that the total area of the communication hole 6a is not more than 1Z10 of the bottom area of the inner crucible 6.
  • the inner crucible 6 was fixed with a holder so that the raw material was melted by the heating heater 2 and then immersed at a depth of 20 mm from the liquid surface of the raw material melt. Although the raw material melt gradually decreases with the crystal growth, the immersion state of the inner crucible 6 was controlled by raising and lowering the susceptor 13 (the outer crucible 5) by driving the rotating shaft 4 up and down. For example, the inner crucible 6 was kept immersed in a range of 10 mm to 40 mm from the liquid level of the raw material melt.
  • the outer crucible 5 and the inner crucible 6 were arranged on the susceptor 13, and the inside of the high-pressure vessel 1 was filled with an inert gas (for example, Ar) and adjusted to a predetermined pressure. Then, heating was performed at a predetermined temperature using a heater 2 while suppressing the surface of the raw material with a sealing agent, and Zn and Te were melted and directly synthesized.
  • an inert gas for example, Ar
  • the seed crystal 9 was brought into contact with the surface of the raw material melt.
  • a seed crystal having a crystal orientation of (110) was used as the seed crystal.
  • the seed crystal was covered with a cover (not shown) made of molybdenum.
  • the pulling rotation shaft 7 was rotated at a rotation speed of 11 to 12 rpm, and a shoulder portion of a crystal was formed while pulling at a speed of 2.5 mmZh.
  • the crucible rotation shaft was rotated at 115 rpm, and the body was formed while pulling up at a speed of 2.5 mmZh.
  • the gap between the growing crystal 11 and the inner crucible 6 is small, the amount of the sealant 11 on the upper part of the crystal wrapping around the gap is small, and the crystal surface is always kept covered with the sealant 11.
  • the constituent elements of the grown crystal 10 were prevented from evaporating, and the temperature gradient in the sealant could be made very small.
  • the temperature fluctuation in the raw material melt in the inner crucible 6 was about 0.5 ° C, and the temperature fluctuation in the raw material melt between the inner crucible 6 and the outer crucible 5 was 1 ° C.
  • the crystal was grown by the LEC method, and after the crystal growth, the grown crystal 10 was separated from the encapsulant 11 to obtain a crack-free ZnTe single crystal.
  • the obtained crystal was a very good single crystal having a (110) orientation without polycrystals or twins.
  • the size of the grown crystal was 54 mm in diameter and 40 mm in length of the straight body.
  • a ZnTe single crystal was repeatedly grown, seven out of ten single crystals became single crystals, and the single crystallization ratio was 70% .o
  • a single-crystal wafer was prepared by slicing the obtained (110) -oriented ZnTe single crystal to a thickness of 1000 m, and the light transmittance of the single-crystal wafer was measured by a measuring apparatus shown in FIG. Specifically, first, the polarization directions A and B of the two polarizing plates 22 and 24 were adjusted so as to be parallel, and the amount of received light at this time was measured by the photodiode 25. Next, the polarization directions A and B of the two polarizing plates 22 and 24 were adjusted to be vertical, and it was confirmed that the amount of received light was 0 at this time.
  • the two polarizers 22, 24 are held in this state, and the ZnTe single crystal wafer 23 produced between them is moved so that the (110) planes of the polarizers 22, 24 and the ZnTe single crystal wafer 23 are parallel.
  • the light receiving amount (transmitted light amount) at this time was measured.
  • the amount of received light when the polarization directions A and B of the two polarizing plates 22 and 24 are adjusted to be parallel is 100, and the amount of received light when the ZnTe single crystal wafer 23 is disposed is also the light transmittance ( %) was calculated.
  • the light source used was 800 nm laser light. As a result, the light transmittance is 6% or less, and It helped to be a crystal.
  • the (110) oriented ZnTe single crystal obtained by the above-described manufacturing method has a light transmittance of 20% or less, extremely small crystal distortion, and excellent crystallinity. It is suitable as.
  • Comparative Example 1 a (110) oriented ZnTe single crystal was manufactured using the crystal growth apparatus proposed by the present applicant in Japanese Patent Application No. 2002-249963.
  • the crystal growth apparatus according to the prior application differs from the crystal growth apparatus according to the above embodiment in that only one communication hole is provided at the center of the bottom surface of the inner crucible. The crystal growth was performed in exactly the same manner as the other conditions.
  • the same crystal growth apparatus was used to increase the temperature gradient during crystal growth and grow the crystal at 30 ° CZcm, a single crystal could be grown.
  • the light transmittance of the obtained ZnTe single crystal wafer was about 25%, which was a component of the fact that it was a single crystal with large crystal distortion. In other words, it is considered that if the temperature gradient is too large, the thermal stress applied to the grown crystal increases, and the crystal distortion increases.
  • the formation pattern and the number of the force communication holes in which the four communication holes 6a are provided on the bottom surface of the inner crucible along the circumference at a fixed distance from the center of the bottom surface are not limited to this.
  • the present invention can be applied not only to the growth of the (110) orientation but also to the growth of the (100) and (111) orientations. By applying the present invention also to the production of a compound semiconductor single crystal, a large and high-quality compound semiconductor single crystal can be obtained.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Un procédé de fabrication d’un monocristal semi-conducteur composé est proposé de façon à cultiver un (110) monocristal semi-conducteur composé orienté ayant une excellente qualité cristalline. Dans un procédé de fabrication d’un monocristal semi-conducteur composé utilisant un procédé Czochralski d‘encapsulation de liquide, un conteneur de matériau fondu constitué d’un premier creuset en forme de cylindre à fond plat et d’un deuxième creuset, qui est disposé sur le côté interne du premier creuset et présente des trous permettant de communiquer avec le premier creuset, contient un matériau semi-conducteur et un matériau d’étanchéité, le conteneur est chauffé pour fondre un matériau, un germe cristallin est mis en contact avec la surface du matériau fondu dans la condition où le matériau est recouvert du matériau d’étanchéité, et le cristal est cultivé en tirant le germe cristallin. En tant que deuxième creuset, un creuset ayant une pluralité de trous de communication est utilisé, et le cristal est cultivé en tirant le germe cristallin dans la direction <110>.
PCT/JP2005/003348 2004-03-02 2005-03-01 PROCÉDÉ DE FABRICATION D'UN MONOCRISTAL SEMI-CONDUCTEUR COMPOSÉ ET MONOCRISTAL ZnTe Ceased WO2005083160A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004056972A JP2007223815A (ja) 2004-03-02 2004-03-02 化合物半導体単結晶の製造方法及びＺｎＴｅ単結晶
JP2004-056972 2004-03-02

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WO2005083160A1 true WO2005083160A1 (fr) 2005-09-09

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WO (1) WO2005083160A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5614857B2 (ja) * 2012-10-31 2014-10-29 株式会社Sumco シリカガラスルツボの評価方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6126590A (ja) * 1984-07-17 1986-02-05 Sumitomo Electric Ind Ltd 化合物半導体単結晶の引上方法及び装置
JPS63195188A (ja) * 1987-02-06 1988-08-12 Sumitomo Electric Ind Ltd 化合物半導体単結晶の製造方法および製造装置
JPS63195189A (ja) * 1987-02-10 1988-08-12 Sumitomo Electric Ind Ltd 単結晶の製造装置
JPH01203287A (ja) * 1988-02-08 1989-08-16 Nec Corp 単結晶引き上げ方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6126590A (ja) * 1984-07-17 1986-02-05 Sumitomo Electric Ind Ltd 化合物半導体単結晶の引上方法及び装置
JPS63195188A (ja) * 1987-02-06 1988-08-12 Sumitomo Electric Ind Ltd 化合物半導体単結晶の製造方法および製造装置
JPS63195189A (ja) * 1987-02-10 1988-08-12 Sumitomo Electric Ind Ltd 単結晶の製造装置
JPH01203287A (ja) * 1988-02-08 1989-08-16 Nec Corp 単結晶引き上げ方法

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