US3351433A - Method of producing monocrystalline semiconductor rods - Google Patents

Method of producing monocrystalline semiconductor rods Download PDF

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Publication number
US3351433A
US3351433A US563301A US56330166A US3351433A US 3351433 A US3351433 A US 3351433A US 563301 A US563301 A US 563301A US 56330166 A US56330166 A US 56330166A US 3351433 A US3351433 A US 3351433A
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United States
Prior art keywords
rod
melt
recess
thick
rim
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Expired - Lifetime
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US563301A
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English (en)
Inventor
Keller Wolfgang
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Siemens Schuckertwerke AG
Siemens Corp
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Siemens Corp
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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
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28—Controlling or regulating
    • C30B13/30—Stabilisation or shape controlling of the molten zone, e.g. by concentrators, by electromagnetic fields; Controlling the section of the crystal
    • 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
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/906—Special atmosphere other than vacuum or inert
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1032—Seed pulling
    • Y10T117/1068—Seed pulling including heating or cooling details [e.g., shield configuration]

Definitions

  • FIG. 2 W. KELLER Nov. 7, 1967 METHOD OF PRODUCING MONOCRYSTALLINE SEMICONDUCTOR RODS 2 Sheets-Sheet 1 Original Filed NOV. 29, 1963 FIG. 2
  • M-onocrystalline semiconductor rods can be produced by pulling them from a melt, according to Czochralski, or by floating zone melting, according to Theuerer. Also known is the so-called pedestal method (Growth and Perfection of Crystals by Doremus, Roberts and Turnbull, published 1958, by Wiley and Sons Inc, New York, treatise by Dash, page 363; also US Patent No. 2,961,- 305) according to which a small mound of semiconductor material is molten, for instance by induction heating, on top of a slotted semiconductor rod, and a monocrystal is then pulled from the melt after immersing a monocrystalline seed therein.
  • the known crystal-pulling methods requiring a crucible involve appreciable risk of contaminating the crystal thus making it unsuitable or inferior for electronic or related purposes; whereas the floating-zone and pedestal methods, avoiding such contamination, have been limited to small diameters or also to short lengths of the resulting monocrystals.
  • I mount a massive and relatively thick semiconductor rod in vertical position so as to leave the top face unattached, the diameter of the thick rod being larger than, for example more than twice or three times, the diameter of the monocrystalline rod to be produced. Thereafter, I apply heat to the top face and concentrate the heating in a center area of the top face so that the annular margin area of the top face is heated to a lower temperature than the center, thus producing on the top face a melt laterally held in position by the top-face margin. Now, I immerse a crystal seed from above into the melt and, while continuing the heating as described, withdraw the seed in the vertically upward direction at such a speed that the growing monocrystal assumes the rated diameter.
  • FIG. 1 shows a vacuum vessel in which the process can be carried out.
  • FIG. 2 shows a portion of FIG. 1 on enlarged scale.
  • FIGS. 3, 4 and 5 show other types of embodiments relating to the process according to the invention.
  • FIG. 1 shows a vacuum vessel designed for this purpose.
  • a box-type housing 2 is equipped with a glass window 3 through which the actual process within the vessel can be observed.
  • the vessel can be evacuated by means of a connecting duct 4.
  • Located within the vessel is a thick rod 5 in coaxial relation to a thin rod 6 produced from the thick rod. Between these two rods, there is a melt 7 produced and kept heated by concentratable heating means such as electron rays or an induction coil. In the illustrated embodiment an induction coil 8 is used.
  • the carrier 9 contains the insulated electric leads for the heating coil, as Well as the inlet and outlet tubes for a coolant which is designed to cool the heating coil.
  • the carrier 9 and coil 8 may be in accordance with US. Patent 2,904,663.
  • the arrow it serves to indicate that the carrier 9 with the heating coil 8 can be displaced vertically from the outside.
  • a lower mounting 12, attached to a guide bar 13 holds the thick rod 5.
  • the guide bar 13 also passes to the outside through an airtight seal 14 and can be moved in a vertical direction from the outside.
  • the thinner rod 6 is held in a similar fashion in an upper mounting 15 which is attached to a shaft 16.
  • This shaft 16 also passes to the outside through an airtight seal 17 and can be moved from the outside in a vertical direction, as well as rotated about its own axle.
  • the melt 7 is heated in such a manner that it can be held in place by the rim of the top face of the thick rod 5 (FIG. 2). This is achieved primarily by bunching the heating effect.
  • One way of doing this is to concentrate electron rays or heat (infrared) rays approximately in the center of the top face of the thick rod 5.
  • Another, or an additional way is to construct an induction-heating coil in such a manner that the desired bunching of the heating effect is achieved.
  • the illustrated embodiment shows such a heating coil 8 in the form of a pancake helical winding. However, the heating coil may also be designed in the form of a cylindrical winding.
  • the pulling process can be started up as follows. First the thick rod 5 is mounted on its holder 12, leaving the top face of the rod exposed, and the seed 6 is mounted on holder but kept axially away from the top of rod 5. Next the top of rod 5 is heated by infrared radiation focused onto the center area of the top face, the heat source being preferably mounted in the vessel, although it may also act from the outside through a lateral window similar to that shown at 3.
  • an electron gun mounted in the vessel and directed onto the center area on the top face of rod 5.
  • the coil 8 may be kept away from the top face. However, when the top face commences to become red hot, the coil 8 is placed close to the top-face plane to raise the temperature to the melting point. Thereafter only induction heating by coil 8 is needed for maintaining the melt on top of rod 5. After lowering the seed until its tip dips into the melt, the crystal pulling proper can commence and is preferably conducted in the following manner.
  • the heating coil should be supplied with hi h frequency in the short-wave range, for instance with approximately 5 megacycles per second.
  • the heating power amounts to approximately 5 to 10 kw.
  • the growing monocrystal is being rotated around its own axle in the usual manner, so that an axially symmetrical growth is assured.
  • the preferred speed of rotation is between 10 and 150 r.p.m., and may amount to 40 rpm. for instance.
  • the heating coil 8 may be kept stationary relative to the vacuum vessel, merely pushing up the thick rod 5 from below, while the thin rod 6 is being pulled out upwardly.
  • the upward pulling speed of the rod is preferably kept at 2 to 4 mm./sec. in relation to the heating coil.
  • the thick rod 5 may be kept stationary, and the heating coil 3 is then moved downward with the aid of the carrier 9.
  • the ratio between the diameter of the thick rod 5 and the diameter of the thin rod 6 should preferably be greater than 1.4.
  • the thick rod 5 may have a diameter of 60 mm. for a thin-rod diameter of 35 mm.
  • Applicable as a thick rod 5 is a polycrystalline semiconductor rod obtained by pyrolytic dissociation and precipitation from the gaseous phase, for example in accordance with the process described in Patent 3,011,877.
  • FIG. 3 shows another example of the process according to the invention, in which the rim of the top face of the thick rod 5 does not only remain intact and thus is capable of holding the melt 7, but in which the melt rests on the bottom of a crucible formed by the semiconductor rod itself.
  • the rim of the thick rod remains intact even after this rod, for the purpose of replenishing the melt, has been moved up.
  • the rim forms the wall of a crucible as the melt advances toward the foot of the rod.
  • FIG. 3 shows the melt 21 kept molten by the heating coil 22. while located within a cavity in the thick rod lit. The thin monocrystal rod 23 is being pulled from the melt in the upward direction.
  • FIG. 3 shows a slot 24 through which powdery or granular semiconductor material is added to the melt.
  • an additional induction heating coil 25 into which a semiconductor rod 26 is being introduced from the top in a diagonal or vertical direction.
  • the lower part of the semiconductor rod 26 is inductively heated to such an extent that the material melts and drips off, thus replenishing the melt 21 with liquid semiconductor material.
  • all parts of the entire apparatus, with the exception of the rod produced 23, may be stationary.
  • FIG. 4 exemplifies another way of practicing the invention.
  • a thin rod 32 is being pulled in an upward direction form a melt 31 located in a thick rod 3%.
  • the melt 31 is inductively heated by a heating coil 33. Through the heating process, the melt acquires such a form that it advances into the thick rod.
  • An additional heating coil 34 serves to melt the semiconductor material that would otherwise remain solid along the rim.
  • the melting material then flows, in the form of droplets into the melt 31 at the edge of the depression created by the melt 31.
  • the semiconductor rod 30 within the area of the heating coil 34 is heated in such a way that the edges which are to be molten continuously melt towards the center. This can also be achieved if the melt 31 supplies continuous radiant heat to the interior wall of the depression thus formed.
  • a portion of the heating effect of the induction coil 33 also acts upon the interior edge of the retained edges of the cavity.
  • a thin rod 41 is derived from a thick rod whose top face carries a melt 42 produced by an induction coil 43.
  • the crosssectional shape of the melt is approximately of the wavy configuration illustrated in FIG. 5, although, for emphasis, the shape of the melt has been shown somewhat exaggerated.
  • the induction heating being primarily effective in the immediate vicinity of the turns of the heating coil 43.
  • This effect can be reduced by pre-heating the thick rod with the aid of a reflector as shown in FIG. 2, which reflects radiant heat back to the semiconductor material.
  • a better remedy is to provide for additional heating, for example with the aid of an additional induction coil 4d, illustrated in FIG 5.
  • the pre-heating coil 44 may surround the thick rod along 40 mm., starting 20 mm. below the top face down to approximately 60 mm. It is advantageous to adjust the heating effect of the pre-heating coil 44 in such a manner that the temperature of the semiconductor material in that area approachces 1200 C. if silicon is used. It will be understood, however, that the invention is also applicable to germanium, III-V semiconductors and any other semiconductor substances amenable to crystal pulling operations.
  • heating of the entire semiconductor material may also be carried out by direct flow of current. This can be done, for instance, by designing the seals 14 and 17, shown in FIG. 1, as electric insulations, and by supplying electric current through the parts 12, 13, 15 and 16. Direct or alternating current of or c.p.s. at a current density of A./cm. may be used for this purpose.
  • Method according to claim 1 which includes placing a supply rod for replenishing semiconductor material pulled from the melt so that an end thereof is located in the magnetic field of the second induction heating coil.
  • Method according to claim 1 which includes disposing an additional induction heating coil around the thick semiconductor rod and energizing the additional heating coil to heat the thick rod to a temperature below the melting point of the semiconductor material thereof.
  • Method according to claim 1 which includes energizing the second induction heating coil so as to produce a magnetic field of such strength as to melt the solid rim of the thick rod surrounding the recess formed therein.
  • Method according to claim 1 which includes adjustably displacing the thick semiconductor rod and the first induction coil relative to one another in the direction of the longitudinal axis of the thick rod.
  • Method according to claim 5 which includes maintaining the first coil and the melt stationary during crystal pulling while advancing the thick rod upwardly to progressively replenish the melt by melting material of the thick rod.
  • Method according to claim 5, which includes maintaining the thick rod stationary while pulling the monocrystal upwardly from the'melt, and progressively shifting the first induction heating coil downwardly for replenishing the melt by melting material of the thick rod.
  • Method according to claim 5 which includes pulling the seed from the melt so as to produce the melt containing recess in the top face of the thick semiconductor rod, and continuing the pulling operation so that the recess advances axially into the thick rod for replenishing the melt by melting material of the thick rod.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US563301A 1962-12-12 1966-07-06 Method of producing monocrystalline semiconductor rods Expired - Lifetime US3351433A (en)

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DES0082820 1962-12-12

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JP (1) JPS5021431B1 (en:Method)
BE (1) BE641090A (en:Method)
CH (1) CH420072A (en:Method)
DE (1) DE1444530B2 (en:Method)
GB (1) GB1029804A (en:Method)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3630684A (en) * 1966-09-24 1971-12-28 Siemens Ag Device for heater movement in crucible-free zone melting a crystalline rod
US3650700A (en) * 1968-01-16 1972-03-21 Siemens Ag Device for crucible-free zone melting having sealing means for a sliding member
US3660062A (en) * 1968-02-29 1972-05-02 Siemens Ag Method for crucible-free floating zone melting a crystalline rod, especially of semi-crystalline material
US3977934A (en) * 1975-01-02 1976-08-31 Motorola, Inc. Silicon manufacture
US3986837A (en) * 1973-03-08 1976-10-19 Nikkei Kako Kabushiki Kaisha Method of and apparatus for manufacturing single crystal compound semiconductor
US3996094A (en) * 1975-01-02 1976-12-07 Motorola, Inc. Silicon manufacture
US4060401A (en) * 1975-04-02 1977-11-29 National Research Development Corporation Method for making aligned fibrous crystals
US4784715A (en) * 1975-07-09 1988-11-15 Milton Stoll Methods and apparatus for producing coherent or monolithic elements
US5258092A (en) * 1991-03-22 1993-11-02 Shin-Etsu Handotai Co., Ltd. Method of growing silicon monocrystalline rod

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4721688A (en) * 1986-09-18 1988-01-26 Mobil Solar Energy Corporation Method of growing crystals
RU182737U1 (ru) * 2016-12-29 2018-08-29 Федеральное государственное бюджетное образовательное учреждение высшего образования "Северо-Кавказский горно-металлургический институт (государственный технологический университет)" (СКГМИ (ГТУ) Устройство для получения высокочистого монокристалла зонной плавкой

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2743199A (en) * 1955-03-30 1956-04-24 Westinghouse Electric Corp Process of zone refining an elongated body of metal
GB775817A (en) * 1954-03-09 1957-05-29 Siemens Ag Improvements in or relating to processes and apparatus for drawing crystalline bodies , such as semi-conductor bodies
FR1235341A (fr) * 1958-03-05 1960-07-08 Siemens Ag Procédé et appareil de fabrication continue de tiges mono-cristallines minces
US2992311A (en) * 1960-09-28 1961-07-11 Siemens Ag Method and apparatus for floatingzone melting of semiconductor rods
US2999737A (en) * 1954-06-13 1961-09-12 Siemens And Halske Ag Berlin A Production of highly pure single crystal semiconductor rods
US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation
GB908370A (en) * 1959-05-29 1962-10-17 Siemens Ag A method of zone-melting a rod of crystalline material
GB911360A (en) * 1959-10-16 1962-11-28 Westinghouse Electric Corp Process for growing crystals
US3113841A (en) * 1959-05-08 1963-12-10 Siemens Ag Floating zone melting method for semiconductor rods
SE347579B (en:Method) * 1970-11-27 1972-08-07 Aga Ab

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB775817A (en) * 1954-03-09 1957-05-29 Siemens Ag Improvements in or relating to processes and apparatus for drawing crystalline bodies , such as semi-conductor bodies
US2999737A (en) * 1954-06-13 1961-09-12 Siemens And Halske Ag Berlin A Production of highly pure single crystal semiconductor rods
US2743199A (en) * 1955-03-30 1956-04-24 Westinghouse Electric Corp Process of zone refining an elongated body of metal
FR1235341A (fr) * 1958-03-05 1960-07-08 Siemens Ag Procédé et appareil de fabrication continue de tiges mono-cristallines minces
US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation
US3113841A (en) * 1959-05-08 1963-12-10 Siemens Ag Floating zone melting method for semiconductor rods
GB908370A (en) * 1959-05-29 1962-10-17 Siemens Ag A method of zone-melting a rod of crystalline material
GB911360A (en) * 1959-10-16 1962-11-28 Westinghouse Electric Corp Process for growing crystals
US2992311A (en) * 1960-09-28 1961-07-11 Siemens Ag Method and apparatus for floatingzone melting of semiconductor rods
SE347579B (en:Method) * 1970-11-27 1972-08-07 Aga Ab

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3630684A (en) * 1966-09-24 1971-12-28 Siemens Ag Device for heater movement in crucible-free zone melting a crystalline rod
US3650700A (en) * 1968-01-16 1972-03-21 Siemens Ag Device for crucible-free zone melting having sealing means for a sliding member
US3660062A (en) * 1968-02-29 1972-05-02 Siemens Ag Method for crucible-free floating zone melting a crystalline rod, especially of semi-crystalline material
US3986837A (en) * 1973-03-08 1976-10-19 Nikkei Kako Kabushiki Kaisha Method of and apparatus for manufacturing single crystal compound semiconductor
US3977934A (en) * 1975-01-02 1976-08-31 Motorola, Inc. Silicon manufacture
US3996094A (en) * 1975-01-02 1976-12-07 Motorola, Inc. Silicon manufacture
US4060401A (en) * 1975-04-02 1977-11-29 National Research Development Corporation Method for making aligned fibrous crystals
US4784715A (en) * 1975-07-09 1988-11-15 Milton Stoll Methods and apparatus for producing coherent or monolithic elements
US5258092A (en) * 1991-03-22 1993-11-02 Shin-Etsu Handotai Co., Ltd. Method of growing silicon monocrystalline rod

Also Published As

Publication number Publication date
JPS5021431B1 (en:Method) 1975-07-23
GB1029804A (en) 1966-05-18
BE641090A (en:Method) 1964-06-11
CH420072A (de) 1966-09-15
DE1444530A1 (de) 1969-04-24
DE1444530B2 (de) 1970-10-01

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