US3477811A - Method of crucible-free zone melting crystalline rods,especially of semiconductive material - Google Patents

Method of crucible-free zone melting crystalline rods,especially of semiconductive material Download PDF

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Publication number
US3477811A
US3477811A US564118A US3477811DA US3477811A US 3477811 A US3477811 A US 3477811A US 564118 A US564118 A US 564118A US 3477811D A US3477811D A US 3477811DA US 3477811 A US3477811 A US 3477811A
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United States
Prior art keywords
rod
zone
holder
rod portion
crucible
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Expired - Lifetime
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US564118A
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English (en)
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Wolfgang Keller
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Siemens AG
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Siemens AG
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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
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28—Controlling or regulating
    • 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
    • C30B13/32—Mechanisms for moving either the charge or the heater
    • 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
    • C30B15/08—Downward pulling
    • 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
    • Y10S117/901—Levitation, reduced gravity, microgravity, space
    • 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
    • Y10S117/91—Downward pulling
    • 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
    • Y10S117/911—Seed or rod holders
    • 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
    • Y10S117/912—Replenishing liquid precursor, other than a moving zone
    • 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
    • Y10S117/917—Magnetic
    • 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
    • Y10T117/1072—Seed pulling including details of means providing product movement [e.g., shaft guides, servo means]

Definitions

  • My invention relates to method of crucible-free zone melting crystalline rods, especially of semiconductive ma terial.
  • I provide a method according to this invention, wherein subsequent to the steps of the method disclosed in my aforementioned issued patent, the holder of the resolidifying rod portion is laterally displaced in the opposite transverse direction, whereby the melting zone is drawn away from the rim of the resolidified rod portion.
  • the holder of the resolidifying rod portion is repeatedly shifted or reciprocated laterally or transversely to the vertical axis of the rod. It has been found particularly useful to repeat the aforementioned lateral or transverse to-and-fro movement several times during one pass of the melting zone.
  • FIGS. 1 to 5 are elevational views, partly broken away and partly in section, showing various phases during the carrying out of the method of the invention
  • FIG. 6 is an elevational view, partly broken away and partly in section, showing a phase comparable to that of FIG. 4 during the carrying out of a variation of the method of this invention.
  • FIGS. 7 and 8 are plots of the local resistivity distribution over the cross section or diameter of the crystalline rod produced by conventional zone melting methods.
  • FIG. 9 is a schematic elevational view of apparatus for carrying out the method in accordance with this invention.
  • FIG. 1 there is shown a semiconductor rod 2, to the lower end of which a seed crystal 5 is fused with the aid of an induction heating coil 3 energized by a suitable high frequency current.
  • a melting zone 4 is thus produced in the rod 2 and can be passed in the longitudinal or vertical direction of the rod, as shown in FIG. 1, by moving the heating coil 3 upwardly or, when the heating coil is stationary, by moving the holders of the crystalline rod 2 downwardly.
  • the seed crystal 5 may be a monocrystal so as to effect the growth of a monocrystalline rod 2.
  • This monocrystalline seed 5, as well as the recrystallized rod portion are rotated about their vertical axis, as shown in FIG. 1, the lower holder for instance being driven by means of an electric motor.
  • the melting zone has reached the point of development in which the transition from the thin seed crystal to a larger diameter of the lower rod portion has been achieved, it being noted however that this larger diameter of the lower rod portion does not exceed the inner diameter of the heating coil 3.
  • the seed crystal 5 is not only moved downwardly with respect to the heating coil 3 which is assumed to be stationary, but is also simultaneously moved laterally or in a direction transverse to the vertical or longitudinal axis of the rod 2, for instance, to the right-hand side of FIG. 2, so that the lower part of the melting zone 4 is also stretched or drawn toward the right.
  • the material crystallizing from the melt grows or solidifies substantially symmetrically to the rotary axis of the lower rod holder (not shown in FIG. 2).
  • the upper rod portion 2 is moved downwardly from above at a suitable rate. It can also be rotated about its longitudinal axis.
  • FIG. 3 a later phase of the method is shown in which, by further displacing the seed crystal 5 toward the right-hand side a further enlargement of the diameter of the lower rod portion 2a up to a desired value is achieved.
  • the direction of the lateral displacement of the lower holder is being reversed, and this holder is now beginning to be moved from the right toward the left-hand side of the figure. Since the lower holder is steadily rotating about its axis at the same time, it would be sufiicient to move it back laterally only to a middle position in which both rod portions are coaxially aligned.
  • the lateral displacement can be continued beyond the middle position, however, until the melting zone extends to the opposite rim of the lower rod portion 2a, as shown in FIG. 4, wherein the lower rod holder which holds the seed crystal 5 has reached the left-hand limit of its displacement.
  • the horizontal arrow indicates in FIG. 4, during the continued movement of both rod portions 2, 2a in downward direction of the rod axis, the direction of lateral displacement is again reversed.
  • FIG. 6 a variation of the method of my invention is shown, in which the recrystallizing rod portion 12a above the heating coil 13 is drawn away in an upward direction, and also the rod portion 12 is moved upwardly relatively to the heating coil 13.
  • the melting zone 14 can be maintained at the upper rod portion 12a due to surface tension and because of the large area of cohesion if it is particularly short in length, i.e. in the direction of the longitudinal axis of the rod.
  • heating by a flat induction coil with helical windings is particularly advantageous.
  • FIG. 7 there is shown a plot of the resistivity of the recrystallized rod across the cross section thereof as achieved after several repeated passes of the melting zone through the rod in accordance with prior art methods of crucible-free zone melting. It is desirable, of course, that the most uniform distribution of resistivity be obtained.
  • the curve shown in FIG. 7 is produced, wherein the resistivity p, beginning at one peripheral location of the rod denoted by O in FIG. 7 remains uniform at first along the diameter of the rod, until about the center of the rod denoted by r,
  • the resistivity increases symmetrically with respect to the center of the rod up to its original value, which then remains constant up to a diametrically opposite peripheral location D of the rod.
  • FIG. 8 is presented for the purpose of comparison with FIG. 7, and shows the local resistivity across the cross section of a rod produced by the method of my aforementioned copending application. Since the melting zone in the described embodiments is formed in a semiconductive rod about half the thickness of the semiconductive rod which is to be grown, there is produced in the grown rod 2a a local resistivity distribution which corresponds to a doubling of the curve in FIG. 7. In the case shown in FIG. 8, the decreases in the resistivity are not located in the center r of the rod cross section but at a location which is a distance /zr from the initial peripheral location 0 or from the center r of the rod.
  • FIG. 9 is a diagrammatic view of apparatus for carrying out the method of the invention in this application, and corresponds substantially to the apparatus described in my aforementioned copending application.
  • a rod comprising an upper rod portion 2 and a lower seed crystal portion 5 is vertically supported by the end holders 101, 102.
  • a slider 103, displaceable on a rotary spindle 104, has an extension abutting the holder 101 so as to be able to displace the holder 101 and the rod portion 2 in either vertical direction depending on the direction of rotation of a reversible motor M
  • a reversible motor M is supported on the extension 105 for rotating the holder 101 and the rod portion 2.
  • the motor M is supported on a base 106 of the apparatus.
  • the holder 102 of the seed crystal is rotatable by a motor M which has a displaceable shaft at one end of which the holder 102 is secured.
  • the motor M is fastened to a slide 107 which is horizontally displaceable by a rack and pinion mechanism driven by a reversible motor M mounted on the base 106 whereby the holder 102 and the seed crystal 5 are displaceable in reciprocatingly opposite directions transverse to the vertical axis of the rod.
  • a motor M also mounted on the base 106-, drives a rotary spindle 108 provided with a spindle head that is in engagement with the displaceable shaft of the motor M for vertically displacing the holder 102 and the seed crystal 5 being formed into a lower rod portion.
  • the horizontal displacement distances of the seed crystal 5 and the holder 102 are relatively small so that the relatively wide abutting surface of the head on the spindle 108 engages the displaceable shaft of motor M in all of the possible horizontally displaced positions of the slide 107 and the motor M secured thereto.
  • An induction heating coil 3, preferably with a fiat winding surrounds and is spaced from the molten zone 4 of the rod portion 2 and is vertically displaceable by a slider 109 and a rotary spindle 110 driven by a motor M which is mounted on the base 106.
  • the apparatus of my invention is located in a vacuum or protective gas atmosphere.
  • a method of zone melting a semiconductor rod wherein the rod is supported vertically by end holders located in the vertical axis of the rod, and a molten zone is formed in the rod by an annular heating device surrounding and spaced from the rod and being relatively displaced along the rod axis, whereby the molten zone is passed along the rod in the direction away from one of the end holders which one is meanwhile rotated, the end holders being relatively moved in an axial direction with respect to one another, which comprises reciprocating said one end holder transversely to the vertical axis of the rod and the annular heating device so as to alternately draw the molten zone toward the periphery of the rod portion located between the one end holder and the molten zone at most over a distance limited by the propensity of the molten material to drip from the molten zone, and withdraw the molten zone from the periphery of the rod portion.

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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)
  • Silicon Compounds (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US564118A 1964-02-01 1966-07-11 Method of crucible-free zone melting crystalline rods,especially of semiconductive material Expired - Lifetime US3477811A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DES89317A DE1218404B (de) 1964-02-01 1964-02-01 Verfahren zum tiegelfreien Zonenschmelzen eines kristallinen Stabes, insbesondere Halbleiterstabes
NL656506040A NL138766B (nl) 1964-02-01 1965-05-12 Werkwijze voor het met behulp van kroesloos zonesmelten vergroten van de dwarsdoorsnede van een monokristallijn staafvormig lichaam.
DES98115A DE1275032B (de) 1964-02-01 1965-07-10 Verfahren zum tiegelfreien Zonenschmelzen eines kristallinen Stabes, insbesondere Halbleiterstabes
DES98712A DE1263698B (de) 1964-02-01 1965-08-07 Verfahren zum tiegelfreien Zonenschmelzen

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Publication Number Publication Date
US3477811A true US3477811A (en) 1969-11-11

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Application Number Title Priority Date Filing Date
US564118A Expired - Lifetime US3477811A (en) 1964-02-01 1966-07-11 Method of crucible-free zone melting crystalline rods,especially of semiconductive material
US664211A Expired - Lifetime US3414388A (en) 1964-02-01 1967-08-29 Method and apparatus for increasing the cross section of a crystalline rod during crucible-free zone melting
US853596A Expired - Lifetime US3658598A (en) 1964-02-01 1969-08-19 Method of crucible-free zone melting crystalline rods, especially of semiconductor material

Family Applications After (2)

Application Number Title Priority Date Filing Date
US664211A Expired - Lifetime US3414388A (en) 1964-02-01 1967-08-29 Method and apparatus for increasing the cross section of a crystalline rod during crucible-free zone melting
US853596A Expired - Lifetime US3658598A (en) 1964-02-01 1969-08-19 Method of crucible-free zone melting crystalline rods, especially of semiconductor material

Country Status (9)

Country Link
US (3) US3477811A (xx)
BE (3) BE664435A (xx)
CH (3) CH413785A (xx)
DE (3) DE1218404B (xx)
DK (2) DK124458B (xx)
FR (1) FR1444259A (xx)
GB (3) GB1044592A (xx)
NL (3) NL138766B (xx)
SE (3) SE309965B (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607109A (en) * 1968-01-09 1971-09-21 Emil R Capita Method and means of producing a large diameter single-crystal rod from a polycrystal bar
US3716341A (en) * 1969-11-29 1973-02-13 Siemens Ag Crucible-free zone melting device having an angled heating coil
US3915660A (en) * 1972-07-13 1975-10-28 Siemens Ag Preparing oriented semiconductor monocrystalline rods

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1272886B (de) * 1966-09-24 1968-07-18 Siemens Ag Vorrichtung zum tiegelfreien Zonenschmelzen eines kristallinen Stabes, insbesondere Halbleiterstabes
DE1544301A1 (de) * 1966-09-28 1970-05-27 Siemens Ag Verfahren zum tiegelfreien Zonenschmelzen eines kristallinen Stabes,insbesondere Halbleiterstabes
DE1619996A1 (de) * 1967-03-18 1971-07-08 Siemens Ag Verfahren zum Herstellen eines einkristallinen Stabes,insbesondere aus Halbleitermaterial
US4002523A (en) * 1973-09-12 1977-01-11 Texas Instruments Incorporated Dislocation-free growth of silicon semiconductor crystals with <110> orientation
US5156211A (en) * 1991-06-10 1992-10-20 Impact Selector, Inc. Remotely adjustable fishing jar and method for using same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation
US3159459A (en) * 1958-02-19 1964-12-01 Siemens Ag Method for producing semiconductor crystals

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2972525A (en) * 1953-02-26 1961-02-21 Siemens Ag Crucible-free zone melting method and apparatus for producing and processing a rod-shaped body of crystalline substance, particularly semiconductor substance
US3036812A (en) * 1958-11-19 1962-05-29 Dewrance & Co Butterfly valves
AT223659B (de) * 1960-11-25 1962-10-10 Siemens Ag Verfahren zur Herstellung von versetzungsfreiem einkristallinem Silizium durch tiegelfreies Zonenschmelzen

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3159459A (en) * 1958-02-19 1964-12-01 Siemens Ag Method for producing semiconductor crystals
US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3607109A (en) * 1968-01-09 1971-09-21 Emil R Capita Method and means of producing a large diameter single-crystal rod from a polycrystal bar
US3716341A (en) * 1969-11-29 1973-02-13 Siemens Ag Crucible-free zone melting device having an angled heating coil
US3915660A (en) * 1972-07-13 1975-10-28 Siemens Ag Preparing oriented semiconductor monocrystalline rods

Also Published As

Publication number Publication date
BE664435A (xx) 1965-11-25
NL146402B (nl) 1975-07-15
NL6506040A (xx) 1966-11-14
CH442245A (de) 1967-08-31
DE1263698B (de) 1968-03-21
CH442246A (de) 1967-08-31
GB1044592A (en) 1966-10-05
GB1079870A (en) 1967-08-16
DE1275032B (de) 1968-08-14
SE309965B (xx) 1969-04-14
DK124458B (da) 1972-10-23
NL138766B (nl) 1973-05-15
BE683852A (xx) 1967-01-09
NL6605968A (xx) 1967-01-11
NL6607827A (xx) 1967-02-08
DE1218404B (de) 1966-06-08
SE323654B (xx) 1970-05-11
US3414388A (en) 1968-12-03
DK124459B (da) 1972-10-23
SE323655B (xx) 1970-05-11
FR1444259A (fr) 1966-07-01
GB1081600A (en) 1967-08-31
US3658598A (en) 1972-04-25
BE685153A (xx) 1967-02-06
CH413785A (de) 1966-05-31

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