WO2000052233A1 - Appareil de croissance de monocristaux - Google Patents

Appareil de croissance de monocristaux Download PDF

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Publication number
WO2000052233A1
WO2000052233A1 PCT/IL2000/000120 IL0000120W WO0052233A1 WO 2000052233 A1 WO2000052233 A1 WO 2000052233A1 IL 0000120 W IL0000120 W IL 0000120W WO 0052233 A1 WO0052233 A1 WO 0052233A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
heater
annular
zone
bottom wall
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/IL2000/000120
Other languages
English (en)
Inventor
Yuri Gelfgat
Herman Branover
Shaul Lesin
Mark Tsirlin
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.)
Solmecs Israel Ltd
Original Assignee
Solmecs Israel 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 Solmecs Israel Ltd filed Critical Solmecs Israel Ltd
Priority to KR1020017011261A priority Critical patent/KR20010113724A/ko
Priority to AU29367/00A priority patent/AU2936700A/en
Publication of WO2000052233A1 publication Critical patent/WO2000052233A1/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
    • C30B15/14—Heating of the melt or the crystallised materials
    • 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

Definitions

  • the present invention relates to apparatus for the production of large single crystals by the Czochralski method. More particularly, the present invention is concerned with the production of high-quality, single crystals of silicon, gallium arsenide and other semiconductor materials.
  • Conventional apparatus for single crystal growth by the Czochralski method comprises an air-tight chamber with a crucible, which as a rule is made of quartz, mounted along its axis and surrounded by coaxial heaters and heat screens.
  • the crucible is symmetrically arranged on a special support, commonly made of graphite, fixed on a shaft capable of rotating and moving in a vertical direction.
  • a rod with a mono-crystalline seed, fixed at its lower end and fitted with means for its rotation and vertical displacement, is located above the crucible along the common vertical symmetrical axis.
  • Devices of such a type operate as follows: Starting material, for instance, silicon in the solid state, is placed into a crucible and then melted by heaters and heated to a temperature somewhat exceeding the silicon melting point. A seed crystal is immersed into the melt and then pulled upwards, the single crystal formed is grown to the required size, and a cylindrical single crystal is grown at the subsequent upward displacement of the rod. The crystal and the crucible are conventionally rotated in opposite directions, and the top surface of the melt in the crucible is maintained at a constant level.
  • An increase in the temperature of the crucible walls causes their enhanced dissolution in the melt, resulting in the incorporation of an elevated amount of oxygen and unfavorable background impurities from the crucible wall material into the melt and further into the single crystal.
  • Such a gradient causes the appearance of intense, uncontrollable, thermo- convective flows in the melt, leading to local fluctuations of temperature and a concentration of doping and background impurities, and resulting in an inhomogeneous distribution of said impurities, particularly, oxygen, in a single crystal grown.
  • crucible with the melt is located within the zone of an axial (aligned with growth axis), transverse (normal to growth axis) or axial-radial (cusp-type) steady magnetic field, produced by magnetic systems fixed either outside or inside the growth apparatus chamber.
  • Steady magnetic fields suppress velocity and temperature fluctuations in the melt and reduce the intensity of convective flows, thus reducing crucible wall erosion and the extent of oxygen incorporation into the melt.
  • Apparatus for single crystal growth by the Czochralski method equipped with systems of a rotating magnetic field, are also known.
  • an inductor of a rotating magnetic field mounted around a crucible with the melt affects the melt and sets it in rotation around the crucible axis.
  • Melt rotation stabilizes convective flows in a crucible, but this requires such high melt rotation rates that segregation effects appear.
  • these approaches do not allow one to produce single crystals of large diameters with a reduced oxygen content and a homogeneous distribution of doping and background impurities over the radius and length of a mono-crystalline ingot.
  • the annular insert which as a rule is made of quartz, hinders the heating of the starting material in the central zone of the crucible, which prolongs the process of its melting, reducing productivity, and requires an increase in heater output, resulting in considerable overheating of the crucible walls;
  • apparatus for single crystal growth including a chamber housing a heatable crucible having a bottom wall and side walls and being rotatable about an axis, means for feeding raw material into said crucible, and further including a seed crystal mounted on a movable rod along said axis, said apparatus comprising an annular heater disposed in said crucible about said axis and above said bottom wall so as to leave a gap between them for melted crystal material flow from a first heating zone defined by the inner surface of said side walls, the outer surface of said annular heater and the peripheral area of said bottom wall, and a second heating zone defined by the inner surface of said annular heater and the central area of said bottom wall.
  • Fig. 1 is a schematic, cross-sectional view of an apparatus for single crystal growth according to the present invention
  • Fig. 2 is a schematic, cross-sectional view of the embodiment of Fig.
  • Fig. 3 is a schematic, cross-sectional view of a modification of the apparatus of Fig. 1
  • Fig. 4 is a schematic cross-sectional view of a still further modification of the apparatus of Fig. 1. Description of Preferred Embodiments
  • the apparatus for single crystal growth according to the present invention as illustrated in Fig. 1 includes an air-tight growth chamber 1 housing a quartz crucible 2 for retaining a melt 3 of semiconductor material, e.g., silicon.
  • the crucible 2 is installed on a graphite support 4. which is, in turn, fixed to a shaft 5.
  • the shaft 5 is equipped with mechanisms (not shown) for its rotation and vertical displacement, as indicated by arrows.
  • Heater 6 and heat shields 7 disposed between the heater and the chamber, are mounted around the crucible 2.
  • annular channel 8 open from above and closed from below, is mounted inside the crucible 2 coaxially to the latter, so as to retain a gap d between its lower end and the bottom of crucible 2 for a hydraulic connection between the peripheral P and central C zones of the crucible 2.
  • the annular channel 8 is fixed by several holders 9, disposed symmetrically over the crucible's circumference. One end of each holder 9 is fixed to the support 4, whereas the second end is connected with the annular channel 8 in such a way that the annular channel 8 can be vertically displaced, either together with the crucible 2, or independently.
  • the annular channel 8 can be made of insulating material, e.g., quartz, or conducting material, e.g., graphite; iridium, depending on the physio-chemical properties of the melt, from which a single crystal is pulled.
  • Heater 10, having flexible current leads 1 1, is disposed inside annular channel 8.
  • the heater 10 provides the possibility of creating a longitudinal temperature gradient along its axis.
  • a heat shield 12 is disposed between the heater 10 and the inner wall of annular channel 8.
  • Per-se known means preferably an inductor 13 for agitating the melt and accelerating its melting, made as an inductor of an alternating (travelling, rotating or pulsating) magnetic field connected with a corresponding power source, is mounted around the chamber 1.
  • the chamber 1 is equipped from above with means 14 for feeding additional amounts of raw material to the crucible 2 for realization of the continuous growth process of a single crystal 15.
  • the single crystal 15 is pulled from the melt to a seed crystal 16 affixed on a rod 17 connected with mechanisms (not shown) for its rotation and vertical displacement in the directions indicated by arrows.
  • the heater 6 disposed around the crucible 2, and the heater 10 disposed inside the annular channel 8, are connected, respectively, to AC or DC power sources (not shown). Depending on specific conditions and requirements, they can be connected in circuits of a travelling, rotating or pulsating magnetic field. In another possible embodiment, heaters can be simultaneously connected to DC and AC sources. Optionally, heaters can be equipped with means for varying the frequency of their supply current.
  • a temperature gradient may be provided which is directed from the device axis to its periphery. This direction of the temperature gradient may provide the formation of a hard silicon crust, the width of which may be controlled, on the wall of the crucible 2. In doing so, the silicon mono-crystal grows from the silicon crucible (i.e., scale melting takes place). This excludes the undesirable effect of admixture transfer, mainly of oxygen, from the walls of the external crucible 2.
  • growth with scale melting provides an increase in the service lifetime of the crucible.
  • the duration of one growth cycle is determined exclusively by the dynamics of admixture accumulation in the silicon melt.
  • the heater 10 can be equipped with an electromagnetic field concentrator 18 connected, respectively, with a HF power source.
  • flux layers 19 and 20 can be built up, the thickness of these layers being essentially different in each zone: from a zero value of thickness in layer 19 to a thickness of twice the growing crystal diameter in layer 20.
  • FIG. 4 there is illustrated a further possible modification of the subject apparatus in which the annular channel 8 is mounted on an apertured ring 21 so as to allow melt 3 to flow therethrough from the peripheral zone P to the central zone C * .
  • the apparatus operates as follows: The crucible 2, disposed in the growth chamber 1, is charged with raw material, for instance, with polycrystalline silicon. Then the heaters 6 and 10 are switched on, and the heat released ensures heating and melting of the raw material.
  • the presence of an additional heater 10 in the annular channel 8 considerably intensifies the process of silicon heating and melting, especially at large crucible diameters. This makes it possible not to overheat the walls of the crucible 2 and of the annular channel 8 much above the melting temperature of silicon. As a result, quartz wall erosion and, respectively, oxygen incorporation into the melt 3, are considerably reduced.
  • an inductor 13 of alternating (travelling, rotating or pulsating) magnetic field is connected. It excites electromagnetic forces in the melt, causing the appearance therein of intense mixing flows.
  • a similar effect is achieved by supplying alternating current to the heaters 6 and 10 and connecting them in circuits of a travelling, rotating or pulsating electromagnetic field.
  • the raw material melting time is considerably reduced, despite a slight overheating of the walls of the crucible and of the annular channel, which time reduction increases apparatus productivity.
  • a seed crystal 16 affixed on rod 17 is lowered into the C zone of the melt 3.
  • the seed crystal 16 and the crucible 2 are set in rotation. Since the annular channel 8 is fixed at the support 4, it rotates in synchronism with the crucible 2, thus ensuring a homogeneous temperature distribution within zone C, from which the single crystal is pulled.
  • the seed crystal 16 whose temperature is below the melt temperature, touches the melt, a single crystal 15 starts crystallizing on the former, which is grown up to the required size and then pulled upward by the mechanism of vertical displacement of the rod 17.
  • the operation mode of the heaters 10 is maintained in such a way that, taking into account the heat shield 12, the temperature of the inner wall of the annular channel 8 is somewhat lower than the temperature of the outer wall of the annular channel 8, whereas convective flows formed in the melt due to the vertical temperature gradient in the zone C are directed in the zone below the crystal in such a way that the supply to the growing crystal is realized by surface flows of the melt directed radially from the crucible wall to its center. Intense oxygen evaporation takes place in said surface flows, so that oxygen is incorporated into the single crystal in minimum amounts.
  • the formation of a scale silicon layer on the internal wall of the crucible 2 is implemented at a relative decrease of the capacity of heater 6 and at a corresponding increase of the capacity of heater 10.
  • the width of the scale layer is adjusted by trial -and- error, at the expense of changing the proportions of the capacities' values.
  • the formation of a temperature gradient directed from the annular channel 8 to the surface of the crucible 2 creates a convective silicon flow to the peripheral area of the melt. In addition, this gradient decreases the probability of oxygen atoms being washed out from the annular channel 8 and getting into the growth area. At the same time, the process of oxygen transfer from the walls of crucible 2 into the silicon melt ceases, the temperature of crucible 2 decreases, and its service lifetime increases correspondingly.
  • Radial and vertical gradients of temperature, intensity and direction of mixing flows in the vicinity of the phase boundary required for the production of high-quality single crystals, as well as conditions of dislocation-free growth, are realized by supplying the heater 10 with alternating (travelling, rotating or pulsating) and/or direct current, or with their combinations.
  • the necessary optimum operation mode of the heaters 10 is selected experimentally for each standard size of a single crystal to be grown.
  • 1 1 heater 10 is equipped with an electromagnetic field concentrator 18 and connected to an HF source of alternating current. Under the action of the HF electromagnetic field concentrated in the vicinity of the phase boundary of the growing crystal (Fig. 2), a constriction of its diameter (neck) is formed, and then the crystal is grown again up to the necessary dimensions. The appearance of a neck causes oxygen evacuation by evaporation out of the narrow constriction zone, and further growth of the single crystal proceeds without any contact with the solid quartz walls. The absence of contact with the walls ensures the production of dislocation-free silicon single crystals with a very low oxygen content ( ⁇ 2 ⁇ 3 ⁇ l0 17 at/cm 3 ).
  • zone P of crucible 2 When additional raw material is fed to zone P of crucible 2, agitating flows excited by the inductor 13 rapidly mix it into the bulk of the melt and promote its accelerated melting.
  • the heaters 6 and 10 still make it possible to implement this process at an insignificant overheating (15 ⁇ 20°C) of the walls of crucible 2 and of annular channel 8, without breaking the optimum conditions of single crystal growth in zone C.
  • a flux layer e.g., gallium arsenide single crystals
  • level 20 of the flux surrounding the crystal in zone C considerably exceeds level 19 of the flux in zone P and equals 0.1 ⁇ 2 diameters of the single crystal.
  • a sufficiently high level 20 of the flux heated by the heater 10 ensures a gradual, smooth temperature decrease in a solid single crystal, preventing its cracking and dislocation generation.
  • a longitudinal temperature gradient of heater 10 contributes to the appearance of convective flows in the flux, thus promoting a smooth temperature decrease in a mono-crystalline ingot and respectively reducing the probability of dislocation generation.
  • the apparatus for single crystal growth by the Czochralski method according to the invention makes it possible:

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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)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

La présente invention concerne un appareil destiné à la croissance de monocristaux, comprenant une enceinte renfermant un creuset, doté de parois latérales et de fond, qu'il est possible de chauffer et de mettre en rotation autour d'un axe, des moyens d'introduction de matière première dans le creuset et un cristal germe monté sur une tige amovible placée selon l'axe. L'appareil comprend aussi un chauffage annulaire disposé dans le creuset autour de l'axe et au dessus de la paroi de fond de manière à laisser un espace entre eux pour que le flux de cristaux fondus passe d'une première zone de chauffage définie par la surface intérieure des parois latérales, la surface extérieure du chauffage annulaire et la zone périphérique de la paroi de fonds, à une seconde zone définie par la surface intérieure du chauffage annulaire et la zone centrale de la paroi de fond.
PCT/IL2000/000120 1999-03-04 2000-02-28 Appareil de croissance de monocristaux Ceased WO2000052233A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020017011261A KR20010113724A (ko) 1999-03-04 2000-02-28 단결정 성장장치
AU29367/00A AU2936700A (en) 1999-03-04 2000-02-28 Apparatus for growing single crystals

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IL12882799A IL128827A0 (en) 1999-03-04 1999-03-04 Apparatus for growing single crystals
IL128827 1999-03-04

Publications (1)

Publication Number Publication Date
WO2000052233A1 true WO2000052233A1 (fr) 2000-09-08

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PCT/IL2000/000120 Ceased WO2000052233A1 (fr) 1999-03-04 2000-02-28 Appareil de croissance de monocristaux

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KR (1) KR20010113724A (fr)
AU (1) AU2936700A (fr)
IL (1) IL128827A0 (fr)
WO (1) WO2000052233A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113502546A (zh) * 2021-07-06 2021-10-15 中国电子科技集团公司第十三研究所 一种磁场下合成及连续生长磷化物的方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR200446667Y1 (ko) * 2008-12-29 2009-11-19 주식회사수성기술 솔라셀용 실리콘 잉곳 제조장치

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3002824A (en) * 1956-11-28 1961-10-03 Philips Corp Method and apparatus for the manufacture of crystalline semiconductors
EP0206514A1 (fr) * 1985-05-21 1986-12-30 Sumitomo Electric Industries Limited Creuset double pour la croissance de monocristaux
US4822449A (en) * 1987-06-10 1989-04-18 Massachusetts Institute Of Technology Heat transfer control during crystal growth
EP0340941A1 (fr) * 1988-04-28 1989-11-08 Nkk Corporation Procédé et appareillage pour la production de monocristaux de silicium
US4963334A (en) * 1989-08-14 1990-10-16 The United States Of America As Represented By The Secretary Of The Air Force High temperature heat pipe coracle and process
WO1991017290A1 (fr) * 1990-04-27 1991-11-14 Nkk Corporation Appareil de fabrication de monocristaux de silicium

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3002824A (en) * 1956-11-28 1961-10-03 Philips Corp Method and apparatus for the manufacture of crystalline semiconductors
EP0206514A1 (fr) * 1985-05-21 1986-12-30 Sumitomo Electric Industries Limited Creuset double pour la croissance de monocristaux
US4822449A (en) * 1987-06-10 1989-04-18 Massachusetts Institute Of Technology Heat transfer control during crystal growth
EP0340941A1 (fr) * 1988-04-28 1989-11-08 Nkk Corporation Procédé et appareillage pour la production de monocristaux de silicium
US4963334A (en) * 1989-08-14 1990-10-16 The United States Of America As Represented By The Secretary Of The Air Force High temperature heat pipe coracle and process
WO1991017290A1 (fr) * 1990-04-27 1991-11-14 Nkk Corporation Appareil de fabrication de monocristaux de silicium
US5279798A (en) * 1990-04-27 1994-01-18 Nkk Corporation Silicon single crystal manufacturing apparatus

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113502546A (zh) * 2021-07-06 2021-10-15 中国电子科技集团公司第十三研究所 一种磁场下合成及连续生长磷化物的方法
CN113502546B (zh) * 2021-07-06 2022-08-19 中国电子科技集团公司第十三研究所 一种磁场下合成及连续生长磷化物的方法

Also Published As

Publication number Publication date
KR20010113724A (ko) 2001-12-28
IL128827A0 (en) 2000-01-31
AU2936700A (en) 2000-09-21

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