US3592611A - Floating-zone melting apparatus - Google Patents

Floating-zone melting apparatus Download PDF

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Publication number
US3592611A
US3592611A US797296*A US3592611DA US3592611A US 3592611 A US3592611 A US 3592611A US 3592611D A US3592611D A US 3592611DA US 3592611 A US3592611 A US 3592611A
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US
United States
Prior art keywords
rod
free
floating
ball
zone
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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.)
Expired - Lifetime
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US797296*A
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English (en)
Inventor
Georg Eder
Reimer Emeis
Wolfgang Keller
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.)
Siemens Schuckertwerke AG
Siemens Corp
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Siemens Corp
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Publication date
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B13/00Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28Controlling or regulating
    • C30B13/285Crystal holders, e.g. chucks
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B13/00Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/32Mechanisms for moving either the charge or the heater
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/911Seed or rod holders
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10Apparatus
    • Y10T117/1024Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1076Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone
    • Y10T117/1084Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone having details of a stabilizing feature
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T74/00Machine element or mechanism
    • Y10T74/18Mechanical movements
    • Y10T74/18568Reciprocating or oscillating to or from alternating rotary
    • Y10T74/18576Reciprocating or oscillating to or from alternating rotary including screw and nut
    • Y10T74/18656Carriage surrounded, guided, and primarily supported by member other than screw [e.g., linear guide, etc.]

Definitions

  • Apparatus for refining a rod according to the floatingzone melting technique includes rotary shaft means adapted to carry and rotate a rod during subjection thereof to the floating-zone melting technique, play-free wormdrive means operatively connected to the rotary shaft means for rotating the latter, carriage means carrying the rotary shaft means, ball-bearing guide means guiding the carriage means for movement, and rotary ball-bearing spindle means operatively connected to the carriage means for displacing the latter, so that the rod is maintained free of mechanical vibrations during treatment of the rod according to the floating-zone melting technique.
  • the main crystalline body of semiconductor structures such as rectifiers, transistors, thyristors, photodiodes, and the like, consist for themost part of germanium, silicon or an intermetallic compound of Group III and Group V elements of the Periodic System, such as InSb or InAs.
  • semiconductor materials such as rectifiers, transistors, thyristors, photodiodes, and the like
  • germanium, silicon or an intermetallic compound of Group III and Group V elements of the Periodic System such as InSb or InAs.
  • the material of the rod is placed in a molten condition at a localized area for example by heating the rod at the localized area by means of an induction coil supplied with high frequency alternating current.
  • This localized zone of molten material is then shifted a number of times along the entire length of the rod.
  • Treatment of the rod in this way results in enriching the molten zone of the rod with impurities while the recrystallizing material of the rod becomes depleted in its content of impurities.
  • the impurities will be transported in this latter direction to the end of the rod so as to provide the rod with an enrichment of impurities at the latter end thereof.
  • Apparatus for carrying out floating-zone melting of rods is of course known in which the semiconductor rod is surrounded by an induction coil and is supported in a suitable holder at one end while at its other end the rod is fused, by means of the induction coil, with an initially free-standing rod-shaped monocrystalline seed crystal. After the zone of contact between the semiconductor rod and the seed crystal has been melted through, the semiconductor rod and/ or the seed crystal are set into rotary movement about their longitudinal axes. Then the melting zone is shifted in a vertical direction along the semiconductor rod.
  • the objects of our invention especially include the provision of guiding and bearing structures which by their combination and arrangement, according to our invention, will result in a vibration-free treatment of the rod enabling improper crystal formation to be reliably avoided.
  • FIG. 1 is a partly schematic side elevation of one possible embodiment of an apparatus constructed according to our invention for practicing the method of our invention
  • FIG. 2 is a partly broken away front elevation of the apparatus of FIG. 1;
  • FIGS. 2a and 212 show partly sectional side and top views, respectively, of a modified embodiment
  • FIG. 3 is a sectional plan view taken along line III-III of FIG. 1;
  • FIG. 4 is a sectional elevation of the structure shown in FIG. 3, taken along line IVIV of FIG. 3 in the direction of the arrows.
  • the apparatus of our invention illustrated in FIGS. 1 and 2 includes a support means made up in part of a rigid standard 2.
  • This standard 2 is hollow and made of a material of high specific weight, such as, for example, steel.
  • the standard 2 may have a height of 4 m., for example.
  • the support means of our apparatus includes in addition to the standard 2, a primary foundation 3 made in the form of a robust concrete block and situated on the floor of the shop.
  • the standard 2 is provided with a pair of parallel vertical guide rails 6 the cross-sectional configuration of which is apparent from FIG. 3. These rails 6 form part of a guide means of our invention and may be made of a material such as hardened steel.
  • the guide means which is formed partly of the rails 6 serves to guide a carriage means composed of a pair of carriages 7 and 8 which are guided for vertical movement.
  • the carriage 7 is shown in a sectional plan view in FIG. 3 and in vertical section in FIG. 4.
  • the carriage 8 has a construction identical with that of the carriage 7.
  • the standard 2 fixedly carries supporting arms 9 and which project forwardly from the standard with the arm 9 situated beneath the arm 10, as is apparent from FIGS. 1 and 2. These arms fixedly carry a container 41 which can either be evacuated or can be filled with a suitable inert or protective gas. Thus, this container is situated at the front side of the standard 2.
  • the carriages 7 and 8 serve as a support for a rotary shaft means formed by the coaxial vertical shafts 13 and 14, which are also supported for rotary movement by the arms 9 and 10 and which extend through gas-tight seals into the interior of the container 41 which is provided with an inspection window.
  • the ends of the shafts 13 and 14 which are situated within the container 41 carry holders 26 and 27 for the crystalline rod 28 which forms the work material treated with the apparatus and method of our invention.
  • This rod 28 is made of a semiconductor material such as, for example, silicon, and it is this rod 28 which is subjected to the floating-zone melting process.
  • a stationary heating coil 23 which surrounds the crystalline rod 28 and which is energized with a high-frequency alternating current.
  • a motor means is operatively connected with the rotary shaft means 13, 14 for rotating the latter, and this motor means is formed by a pair of motors 13a and 14a which serve through transmissions described below to drive the Shafts 13 and 14, respectively.
  • These motors are especially balanced so as to be free of vibrations and all rotary parts of the motors are supported for rotation by play-free bearings which may take the form of suitable journals or slide bearings.
  • the motors 13a and 14a drive the shafts 13 and 14, respectively, through worm-drives 15 (FIG. 1) made up of especially constructed worms and worm wheels which are free of vibrations.
  • the motors 13a and 14:: are respectively carried by the carriages 7 and 8 which are in turn vertically displaced by way of a spindle means formed by a pair of ball-bearing spindles 16 and 17. These spindles 16 and 17 are driven through a transmission 19 which is in turn driven from a plurality of shafts linked together and including the shaft 20 linked by the universal joints 21 to the other shafts.
  • the system of linked shafts is driven through a step-down transmission 22a by a driving motor 22 (FIG. 1).
  • a monocrystalline seed which is fixed in the lower holder 27, for example, is fused with the crystalline rod 28 which initially is fixedly carried only by the upper holder 26.
  • our invention includes, as one of its features, the provision of the worm-drive transmissions 15 between the motors 13a and 14a and the shafts 13 and 14, these transmissions being substantially free of any play and being carried by the carriages 7 and 8 between the motors 13a and 14a and the shafts 13 and 14, as pointed out above. It is of particular advantage to use for the play-free worm-drives 15 commercially available worm gearing known in the trade under the trademark Cavex worm gears. These transmissions have worms provided witha concave flank profile.
  • the spindle means which is operatively connected to the carriage means 7, 8 for displacing the latter is formed by the pair of spindles 16 and 17, as pointed out above,
  • these spindles are in the form of play-free ball-bearing spindles.
  • the threads of the spindles 16 and 17 are constructed in such a way that they can be filled with spherical members which can freely roll along the thread grooves, and in this way ball-bearing spindles of almost no capability of setting up or transmitting the vibrations are provided.
  • the spherical ball-bearing members guided along the threads thereof are returned through suitable passages so as to again move along their initial path of helical movement along the spindle members.
  • the return elements for the spherical members of the ball-bearing spindles are con structed so as to interfere in no way with the nuts 16a and 17a respectively carried by the carriages 7 and 8 and cooperating with the spindles 16 and 17.
  • These ballbearing spindles 16 and 17 are, according to a further feature of our invention, supported for rotary movement in vibration-free bearings 16! and 17b which preferably take the form of slide bearings.
  • the guide means of our invention which includes the rails 6, as pointed out above, has a construction which is particularly free of play and which at the same time renders the carriages very easy to move.
  • This guide means includes the pre-stressed ball-bearing guides 18 (FIGS. 3 and 4) which are stressed in the sense that they act with a given pressure on the spherical bearing members. These prestressed guides 18 for the ball members have proved to be extremely free of any play while at the same time guaranteeing that the carriages can easily be set into movement.
  • each of the pre-stressed ball-bearing guides 18 is made up of a pair of pre-stressed ball passages 18a cooperating with one of the rails 6 and communicating at their upper and lower ends with semi-circular ball passages which in turn communicate with non-pre-stressed return passages 18b in which the balls move freely without any of the pressure applied thereto as in the case of the prestressed guide passages 18a.
  • the guide means includes the endless passages formed by the ball guides 18a and 18b and the semi-circular portions interconnecting these guides at their ends, and it will be noted that each rail 6 has along its outer edge a fin or rib extending between a pair of rows of the ball members, these rows being maintained separate from each other at each of the guides 18.
  • the balls are arranged along an endless path as is apparent from FIG. 4, and these balls continuously circulate along this endless path to provide the vibration-free guiding of our invention.
  • the shafts 13 and 14 are supported for rotary movement by bearings 11 and 12 which preferably take the form of slide bearings which are free of any play and which are carried by the car riages 7 and 8 as indicated for the upper carriage 7 in FIG. 1. It is also of benefit, in accordance with our invention, to provide in the arms 9 and 10 suitable vibrationfree slide bearings for the shafts 13 and 14. As was indicated above the motors 13a and 14a which are carried by the carriages 7 and 8 are especially balanced so as to be free of vibrations and in addition the rotary shafts of these motors are supported for rotation in vibration-free slide bearings.
  • the transmission of vibrations from the shafts 13 and 14 to the rod 28 is avoided by driving the ball-bearing spindles 16 and 17 from a play-free worm-drive means 19 situated in the lower part of the standard 2. Also for this purpose it is desirable to use a play-free worm drive available on the market and known as Cavex worm drives.
  • the transmission of motion from the driving motor 22 to the worm drive means 19 is brought about, as pointed out above, by a series of shafts which include the shaft 20 and which are linked to each other by universal joints 21.
  • these universal joints 21 include elastic motion-transmitting members made of suitable plastic discs, so that no jarring impacts or vibratory movements can be transmitted from the driving motor 22 to the floating-zone melting apparatus.
  • This driving motor 22 whose speed of rotation must be controlled and from which therefore it is possible to derive undesirable vibrations is separated from the primary foundation 3, together with the stepdown transmission 22a, by being mounted together with the latter on a secondary foundation 29 situated on the floor of the shop and located at a place separate and spaced from the primary foundation 3. In this way any vibratory movements situated at the motor 22 or the transmission 22a will be prevented from reaching the foundation 3 and thus from reaching the floating-zone melting apparatus.
  • the structure includes an unillustrated control and service desk where the operator will manipulate control elements so as to control the operation of the apparatus, and in accordance with a further feature of our invention this latter desk is mounted on a further unillustrated secondary or auxiliary foundation 42 of the control or service desk or cabinet 43, which is separate and spaced from the foundation 3, so that manual movement of manually engageable elements or any movable control elements will be prevented from inducing vibrations in the molten zone of the rod during the crystalpulling process.
  • the primary foundation 3 can, in the event that it is necessary to shield the apparatus from extraneous sources of vibration, take the form of a concrete block 44 (FIGS. 2a, 2b) which is mounted on a spring assembly which will damp out any vibrations to prevent them from reaching the concrete block of the support means of our invention.
  • the concrete block 44 is located in a pit lined with concrete 47 and is supported at four lugs 49 only.
  • Each lug 49 is fastened to a vertical rod 50 whose upper end is seated on a spring 45 abutting against two rigid bases 48.
  • a dashpot or shock absorber is mounted on each rod 50 between the spring 45 and the lug 49.
  • a plate 51 covers the pit.
  • the stationary heating coil 23 which is situated within the container 41 can, for example, be supplied with a high frequency alternating current having a frequency in the range of between 1 and megacycles (m.c.p.s.), and a suitable HF-generator may be used for this purpose.
  • a suitable HF-generator may be used for this purpose.
  • the use of such a generator involves the danger of exciting in the molten zone of the crystalline rod 28 vi brations resulting from modulation of the high frequency heating current with low frequency alternating current. This latter danger can be avoided by using a high frequency heating current whose ripple amplitude is considerably below 1%.
  • the d1rect current required for the high frequency generator is derived by rectification of alternating current, it is possible to achieve this later maintenance of the ripple amplitude below 1% by smoothing the direct current with extreme care.
  • the standard 2 As a further feature of our invention contributing to insulation of the rod 28 from vibrations, it is of advantage to make the standard 2 hollow, so that it has a free interior space 4, and this space can be filled with a granular material 4a of high specific Weight, such as, for example, dry sand, so that the occurrence of vibrations in the standard 2 is avoided and in this way any vibrations of the standard 2 are damped.
  • a granular material 4a of high specific Weight such as, for example, dry sand
  • the carriages 7 and 8 are preferably provided with additional vibratory auxiliary mass systems 24, and the upper end of the standard 2 is provided with a similar auxiliary system 25.
  • Apparatus for refining a rod according to the floating-zone melting technique comprising rotary shaft means adapted to carry and rotate a rod during subjection thereof to the floating-zone melting technique, play-free wormdrive means operatively connected to said rotary shaft means for rotating the latter, carriage means carrying said rotary shaft means, ball-bearing guide means guiding said carriage means for movement, and rotary ballbearing spindle means operatively connected to said carriage means for displacing the latter, so that the rod is maintained free of mechanical vibrations during treatment of the rod according to the floating-zone melting technique and including a hollow standard carrying said spindle means and said guide means, said hollow standard being adapted to be filled with a granular material for increasing the stability of the apparatus so as to further contribute to the vibration-free treatment of a rod.
  • Apparatus for floating-zone melting a rod of crystallizable material comprising a processing container, a pair of holder means for vertically holding a rod of crystalliieree material therebetween, said pair of holder means mounted in said container and extending vertically upwardly and downwardly, respectively, through openings in opposing walls of said container, a stationary heating device mounted in said container coaxially with said pair of holder means so as to surround a rod of crystalliieree material held by said pair of holder means for forming a molten zone therein, means for displacing said pair of holder means in axial direction thereof, said displacing means comprising a pair of vertically displaceable carriages located one above and the other below said processing container, each of said carriages being firmly connected respectively with one of said pair of holder means, ball-bearing spindle drive means operatively connected to said carriages for displacing the same, said ball-bearing spindle drive means including a pair of drive spindles formed with a thread
  • connecting members interconnecting said motor means and said drive spindles comprises a respective step-down transmission operatively connected to said motor means, a respective play-free worm drive connected to each of said drive spindles, and a universal drive shaft interconnecting said transmission and said drive shaft.
  • said universal drive shaft comprises a rigid shaft portion having at both ends thereof, respectively, a universal joint formed of elastic discs of plastic material, a driving rotary shaft shaft operatively connecting the other of said universal joints with one of said drive spindles.
  • said heat- 8 ing device comprises an induction coil energizable by a high frequency alternating current.

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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)
  • Vertical, Hearth, Or Arc Furnaces (AREA)
US797296*A 1965-05-27 1968-10-25 Floating-zone melting apparatus Expired - Lifetime US3592611A (en)

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DES0096982 1965-05-27

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BE (1) BE680555A (enrdf_load_stackoverflow)
GB (1) GB1151054A (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3994690A (en) * 1974-02-15 1976-11-30 Elphiac Universal apparatus for elaborating semiconductive monocrystals
US4045183A (en) * 1974-11-21 1977-08-30 Siemens Aktiengesellschaft Support device for use in a crucible-free floating zone melting apparatus
US5217565A (en) * 1991-11-13 1993-06-08 Wisconsin Alumni Research Foundation Contactless heater floating zone refining and crystal growth

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3994690A (en) * 1974-02-15 1976-11-30 Elphiac Universal apparatus for elaborating semiconductive monocrystals
US4045183A (en) * 1974-11-21 1977-08-30 Siemens Aktiengesellschaft Support device for use in a crucible-free floating zone melting apparatus
US5217565A (en) * 1991-11-13 1993-06-08 Wisconsin Alumni Research Foundation Contactless heater floating zone refining and crystal growth

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DE1519871B2 (enrdf_load_stackoverflow) 1973-12-20
DE1519871A1 (de) 1970-02-26
GB1151054A (en) 1969-05-07
BE680555A (enrdf_load_stackoverflow) 1966-11-07

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