US2892739A - Crystal growing procedure - Google Patents

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US2892739A
US2892739A US459685A US45968554A US2892739A US 2892739 A US2892739 A US 2892739A US 459685 A US459685 A US 459685A US 45968554 A US45968554 A US 45968554A US 2892739 A US2892739 A US 2892739A
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ingot
melt
crystal
rate
composition
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George W Rusler
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Honeywell Inc
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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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • 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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10Crucibles or containers for supporting the melt
    • C30B15/12Double crucible methods
    • 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
    • Y10S117/912Replenishing liquid precursor, other than a moving zone
    • 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
    • Y10S65/00Glass manufacturing
    • Y10S65/04Electric heat

Definitions

  • the present invention relates to a procedure and apparatus for growing crystals having a substantially constant composition, and more particularly to growing of semi-conductor crystals having substantially constant composition characteristics over an extended portion of their length.
  • a single-crystal ingot is grown from a melt, the usable portions of the ingot separated from the remainder of the ingot and the usable portion further processed.
  • the usable Y portions of the ingot amount to only a relatively small portion of the entire ingot and for this reason the operation is considered rather ineflicient at this point.
  • the usable portions of the crystals may be increased somewhat if the rate of pull is properly programmed. That is, the solid-liquid segregation constant of the mixture may be increased or decreased in accordance with the manner that the crystal is pulled from the melt, for example, if the crystal is pulled mo-re slowly, the segregation constant drops, and the concentration of impurities in the crystal as pulled remains fairly constant over a relatively longer portion of the crystal. This is due to the slow increase in impurity concentration as the crystal pulling progresses. While this method is generally practiced, it is not entirely satisfactory since the size of crystals produced in this manner is limited, and further, the programming rate requires a skilled operators constant attention over long periods of time.
  • the composition of the material added to the melt is substantially the same as the composition of the withdrawn ingot. Accordingly, an ingot is obtained having a composition which is relatively constant from one end to the other, an achievement which has been heretofore impossible to accomplish. In'other words, an extended portion of the crystal has a useful range of composition. According to present day procedures, one would need an indefinitely long crystal' to obtain a substantial amount of usable material from a single crystalline ingot. In other words, my procedure now makes it possible to obtain a singlecrystal ingot which has only a small portion of waste material therein. Therefore, fewer crystal growing cycles are needed in order to provide the same quantity of p 2,892,739 Patented June 30, 1959 ICC It is still a further object of the present invention 'to provide apparatus for growing the improved crystals as set forth herein.
  • the figure is a vertical sectional view of a crystal growing apparatus particularly adapted for carrying out the present invention.
  • a crystal growing assembly generally designated 10 which includes a crucible system 11 and crystal pulling mechanism generally designated 12 mounted within the shell or housing 14.
  • Metal feeding means 15, heating coils 16, and inert gas supply and exhaust tubes 17 and 18 respectively are also included in the system, and contained at least partially within the housing 14.
  • the crucible system generally designated 11 includes an inner container 20 surrounded and spaced from an outer shell 21.
  • the space between the inner and outer shells 20 and 21 defines an annular chamber as at 22.
  • Spaced ribs 24 are provided in the annular chamber 22 in order to hold the inner and outer shells 20 and 21 respectively in relatively spaced relationship.
  • the inner container 20 is provided with a hole or port at 25 which provides communication between the inner chamber 26 and the outer annular chamber 22.
  • the crucible system 11 is mounted on the plate 28 which is situated on the shaft 29 and adapted for axial rotation therewith. Shaft 29 is adapted for axial rotation in the bearing 29A.
  • the crystal pulling mechanism 12 includes a pulling shaft 30 which is provided with a seed crystal retaining member 31 adapted to retain a seed crystal 32 by any convenient means, such as, for example, the set screw 33.
  • the ingot 35 is fused onto the seed crystal 32 and an extended ingot is formed or grown as the crystal pulling mechanism 12 is moved in the direction of the arrow 36 at a proper rate for growing or forming of the ingot 35.
  • the crucible 11 is heated by the induction heating coils 16, which are supplied with high frequency energy from an external source of conventional or well known design, not Sho-wn.
  • the coils 16 are provided with cores 37 through which a suitable coolant, such as water, may ilow.
  • the metal feeding means 15 includes a hopper member 40 containing a quantity of finely divided semi-conductor metal as shown at 41.
  • Control means such as the damper 42, are provided in the shaft 43 which extends from the hopper 40 to a point directly above the annular melting chamber 22.
  • Control means 42 are adapted to permit passage of solid material into the chamber 22 at a rate substantially equal to the rate at which material is drawn from the system in the form of the crystalline ingot 35, thereby maintaining the quantity of metal within the crucible system 11 at a constant level at all times, even when the crystalline ingot is being pulled.
  • the improved process of the present invention may be conveniently carried out inthe apparatus described hereinabove as follows.
  • the crucible is filled with a charge of doped germanium having a resistivity which is lower than that desired in the grown crystalline ingot product'. Since in germanium the ratio between impurity content in the solid phase to thatin the melt, the segregation constant, is very low, a charge having a bulk resistivity substantially lower than that desired in the ingot is rutilized. g In other words, the impurity content of the charge is higher than that desired in the ingot.
  • the charge is heated to a surface temperature of 940 F. and the crucible is then set into rotation about its axis, along with.
  • the shaft 29 At this time, the seed crystal 32 is lowered and placed in contact with the surface of the melt, permitted to' remain there for about 30 seconds, or until the crystal commences to form about the seed, at which time the seed crystal is slowly withdrawn, at a rate such that the crystalline ingot 35 forms thereon.
  • the shaft 30 is drawn upwardly at a relatively constant rate, that is, at a rate substantially equal to the rate of forming of the crystalline ingot. For germanium, this rate is about 25 mils per minute at a surface temperature of 940 F. and withV the crucible rotating at about 150 r.p.m.
  • the new material added to the melting zone 22 be permitted to reach a. suiiiciently high temperature for the period of time necessary for the material to become thoroughly molten and thereby lose its memory of crystallization, before it reaches the port 25.
  • It is important that the addition of new material is maintained substantially at the rate of withdrawal of material in the form of the crystalline ingot, the volume of metal in the crucible remaining substantially constant. This insures that the resistivity of the crystalline ingot as it is withdrawn will likewise remain constant.
  • the Crucible 11 is filled with a charge of n-type antimony doped germanium having a bulk resistivity of about 300. times that desired in the crystal.
  • doping substances such as arsenic, phosphorous, bismuth, indium or the like.
  • the charge is then heated to a surface temperature of 940 F. and the seed crystal immersed a distance of 1/32 inch into the surface of the melt contained in the molten zone 26 of the crucible 11.
  • the seed crystal is permitted to remain in contact with the surface of the melt for about 30 seconds before rotation of the crucible is commenced, rotation is begun and a slow, constant withdrawal ofthe ingot is then started.
  • the ingot is withdrawn from the Crucible at a rate of about 11/2 inches per hour, and an ingot having a diameter of between l and 2 inches is formed.
  • the segregation constant for this material is 0.003 for a non-agitated solution and 0.005 for a solution agitated and a crystal pulled at the rate set forth in this example.
  • control member 42 Upon commencement of withdrawal of the ingot from the melt, control member 42 is opened and additional material 41 comprising bulk germanium n-type, doped with antimony to a resistivity of from 4 to 6 ohm-centimeters is permitted to enter the system by way of the melting zone 22.
  • additional material 41 comprising bulk germanium n-type, doped with antimony to a resistivity of from 4 to 6 ohm-centimeters is permitted to enter the system by way of the melting zone 22.
  • This addition of material is closely controlled at a rate substantially equal to the rate of withdrawal of material from the crucible system in the form of an ingot, and the bulk composition of this substance is substantially the same as the composition of the ingot.
  • This composition control may also be achieved by the rate at which new material is added to the melt, since generally the composition of the melt will be more heavily contaminated than that of the ingot drawn therefrom. Therefore the ingot composition will approach a more heavily contaminated level as the quantity of the melt decreases due to lower or no addition of new material to the melt.
  • This feature may be utilized for varying the composition of the ingot by a controlled addition of new material at a rate which Varies from the rate of withdrawal.
  • the method'of growing crystalline ingots of a serniconductor material selectedffromA the class consisting of germanium and silicon and having a controlled rst predetermined concentration of a certain doping impurity which method includes providing a melt of said semiconductor material together with a second predetermined concentration of said certain doping impurity, said second predetermined concentration of said certain doping impurity being greater than said controlled first predetermined concentration thereof, and withdrawing an ingot from said melt at a predetermined rate, a substantial portion of which ingot contains said certain doping impurity in said controlled first predetermined concentration while maintaining the volume of the melt and the concentration of said certain doping impurity therein constant after said body has acquired said predetermined concentra- "tion at the interface with said melt by simultaneously adding to the melt additional amounts of said semiconductor material and said certain doping impurity at a rate equal to the rate at which the material is being Withdrawn from the melt in the formation of said ingot and melting said additional semiconductor material, the concentration of said certain doping impurity in the newly 15 2,

Description

` June 30, 1959 G. w. RusLER 2,892,739
' CRYSTAL GROWING PROCEDURE Filed oct. 1. 1954 INVENTOR ATTORNEY ,GEoRGE wl RusLvl-:R
BY'U? A! GAS OUTLET United States Patent O M' CRYSTAL GROWING PROCEDURE George W. Rusler, Minneapolis, Minn., assignor to Minneapolis-Honeywell Regulator Company, Minneapolis, Minn., a corporation of Delaware Application October 1, 1954, Serial No. 459,685
3 Claims. (Cl. 14S-1.5)
The present invention relates to a procedure and apparatus for growing crystals having a substantially constant composition, and more particularly to growing of semi-conductor crystals having substantially constant composition characteristics over an extended portion of their length.
According to procedures presently utilized in semiconductor crystal growing applications, a single-crystal ingot is grown from a melt, the usable portions of the ingot separated from the remainder of the ingot and the usable portion further processed. Generally, the usable Y portions of the ingot amount to only a relatively small portion of the entire ingot and for this reason the operation is considered rather ineflicient at this point.
The usable portions of the crystals may be increased somewhat if the rate of pull is properly programmed. That is, the solid-liquid segregation constant of the mixture may be increased or decreased in accordance with the manner that the crystal is pulled from the melt, for example, if the crystal is pulled mo-re slowly, the segregation constant drops, and the concentration of impurities in the crystal as pulled remains fairly constant over a relatively longer portion of the crystal. This is due to the slow increase in impurity concentration as the crystal pulling progresses. While this method is generally practiced, it is not entirely satisfactory since the size of crystals produced in this manner is limited, and further, the programming rate requires a skilled operators constant attention over long periods of time. It is Well known that in any system wherein the solid and liquid phases are in equilibrium with each other, portions of the impurities present tend to migrate to one phase or the other, and in particular in present day semi-conductor work, the impurities tend to migrate to the liquid phase. Therefore, as a crystal is being withdrawn from a melt the composition of the liquid phase is constantly changing, that is, the liquid portion becomes more heavily contaminated with impurities or in other words contains a relatively higher percentage of impurity members. According to my improved procedure, the composition of the liquid phase is held substantially constant by the addition of new raw material to the melt at a rate substantially equal to the rate of withdrawal of material in the form of the crysalline ingot. Of course, the composition of the material added to the melt is substantially the same as the composition of the withdrawn ingot. Accordingly, an ingot is obtained having a composition which is relatively constant from one end to the other, an achievement which has been heretofore impossible to accomplish. In'other words, an extended portion of the crystal has a useful range of composition. According to present day procedures, one would need an indefinitely long crystal' to obtain a substantial amount of usable material from a single crystalline ingot. In other words, my procedure now makes it possible to obtain a singlecrystal ingot which has only a small portion of waste material therein. Therefore, fewer crystal growing cycles are needed in order to provide the same quantity of p 2,892,739 Patented June 30, 1959 ICC It is still a further object of the present invention 'to provide apparatus for growing the improved crystals as set forth herein.
The invention may be more easily and fully comprehended with reference to the accompanying drawing in which:
The figure is a vertical sectional view of a crystal growing apparatus particularly adapted for carrying out the present invention.
The improved process of the present invention is conveniently carried out in the crystal growing apparatus as illustrated in the accompanying drawing. Accordingly, there is provided a crystal growing assembly generally designated 10 which includes a crucible system 11 and crystal pulling mechanism generally designated 12 mounted within the shell or housing 14. Metal feeding means 15, heating coils 16, and inert gas supply and exhaust tubes 17 and 18 respectively are also included in the system, and contained at least partially within the housing 14. The crucible system generally designated 11 includes an inner container 20 surrounded and spaced from an outer shell 21. The space between the inner and outer shells 20 and 21 defines an annular chamber as at 22. Spaced ribs 24 are provided in the annular chamber 22 in order to hold the inner and outer shells 20 and 21 respectively in relatively spaced relationship. The inner container 20 is provided with a hole or port at 25 which provides communication between the inner chamber 26 and the outer annular chamber 22. The crucible system 11 is mounted on the plate 28 which is situated on the shaft 29 and adapted for axial rotation therewith. Shaft 29 is adapted for axial rotation in the bearing 29A.
The crystal pulling mechanism 12, includes a pulling shaft 30 which is provided with a seed crystal retaining member 31 adapted to retain a seed crystal 32 by any convenient means, such as, for example, the set screw 33. In operation, the ingot 35 is fused onto the seed crystal 32 and an extended ingot is formed or grown as the crystal pulling mechanism 12 is moved in the direction of the arrow 36 at a proper rate for growing or forming of the ingot 35.
The crucible 11 is heated by the induction heating coils 16, which are supplied with high frequency energy from an external source of conventional or well known design, not Sho-wn. The coils 16 are provided with cores 37 through which a suitable coolant, such as water, may ilow.
The metal feeding means 15 includes a hopper member 40 containing a quantity of finely divided semi-conductor metal as shown at 41. Control means, such as the damper 42, are provided in the shaft 43 which extends from the hopper 40 to a point directly above the annular melting chamber 22. Control means 42 are adapted to permit passage of solid material into the chamber 22 at a rate substantially equal to the rate at which material is drawn from the system in the form of the crystalline ingot 35, thereby maintaining the quantity of metal within the crucible system 11 at a constant level at all times, even when the crystalline ingot is being pulled.
The improved process of the present invention may be conveniently carried out inthe apparatus described hereinabove as follows. In operation, the crucible is filled with a charge of doped germanium having a resistivity which is lower than that desired in the grown crystalline ingot product'. Since in germanium the ratio between impurity content in the solid phase to thatin the melt, the segregation constant, is very low, a charge having a bulk resistivity substantially lower than that desired in the ingot is rutilized. g In other words, the impurity content of the charge is higher than that desired in the ingot. The charge is heated to a surface temperature of 940 F. and the crucible is then set into rotation about its axis, along with. the shaft 29; At this time, the seed crystal 32 is lowered and placed in contact with the surface of the melt, permitted to' remain there for about 30 seconds, or until the crystal commences to form about the seed, at which time the seed crystal is slowly withdrawn, at a rate such that the crystalline ingot 35 forms thereon. The shaft 30 is drawn upwardly at a relatively constant rate, that is, at a rate substantially equal to the rate of forming of the crystalline ingot. For germanium, this rate is about 25 mils per minute at a surface temperature of 940 F. and withV the crucible rotating at about 150 r.p.m. When the crystalline ingot being withdrawn from the melting zone 26- reaches an optimum composition as indicated by its-resistivity, new material having a resistivity or impurity content substantially equal to that of the withdrawn ingot 35 is added to the melting zone 22 through the conduit or shaft 43 which extends from the hopper 40. The proper times for adding new material to the melt is readily determined by practice. This new material is permitted to melt under the influence of the induction heating coils 16, and under static pressure influence, eventually passes through the port 25 into the molten zone 26 of the inner crucible 20.
It is preferable that the new material added to the melting zone 22 be permitted to reach a. suiiiciently high temperature for the period of time necessary for the material to become thoroughly molten and thereby lose its memory of crystallization, before it reaches the port 25. In practice, it may be necessary in some instances to commence the pulling of a crystal before additional new material is added to the melting zone 22. This would ocour in instances Where the crystal ingot being pulled has an original resistivity which is higher than that desired in the final product. It is important that the addition of new material is maintained substantially at the rate of withdrawal of material in the form of the crystalline ingot, the volume of metal in the crucible remaining substantially constant. This insures that the resistivity of the crystalline ingot as it is withdrawn will likewise remain constant.
Example In order to prepare al crystalline ingot having a desired l resistivity of from, for example, 4 to 6 ohm-centimeters, the Crucible 11 is filled with a charge of n-type antimony doped germanium having a bulk resistivity of about 300. times that desired in the crystal. Of course, other doping substances may be utilized, such as arsenic, phosphorous, bismuth, indium or the like. The charge is then heated to a surface temperature of 940 F. and the seed crystal immersed a distance of 1/32 inch into the surface of the melt contained in the molten zone 26 of the crucible 11. The seed crystal is permitted to remain in contact with the surface of the melt for about 30 seconds before rotation of the crucible is commenced, rotation is begun and a slow, constant withdrawal ofthe ingot is then started. For a' temperature of 940 F., the ingot is withdrawn from the Crucible at a rate of about 11/2 inches per hour, and an ingot having a diameter of between l and 2 inches is formed. The segregation constant for this material is 0.003 for a non-agitated solution and 0.005 for a solution agitated and a crystal pulled at the rate set forth in this example. Upon commencement of withdrawal of the ingot from the melt, control member 42 is opened and additional material 41 comprising bulk germanium n-type, doped with antimony to a resistivity of from 4 to 6 ohm-centimeters is permitted to enter the system by way of the melting zone 22. This addition of material is closely controlled at a rate substantially equal to the rate of withdrawal of material from the crucible system in the form of an ingot, and the bulk composition of this substance is substantially the same as the composition of the ingot.
Although specific reference has been made to germanium in this apparatus, the method is equally applicable to silicon and other metallic systems. As a slightly modified procedure in accordance with the present invention, it is possible to obtain an elongated crystal having a composition which varies over a desired impurity range by varying the rate of addition or composition of the addition material. In this regard new material having a composition substantially equal to that desiredy in the final crystal may be added to the melt as the ingot is Withdrawn. Of course, as the drawing of the ingot is continued,- the composition of the ingot will approach that of the added material, and close control of product composition is therefore possible. This composition control may also be achieved by the rate at which new material is added to the melt, since generally the composition of the melt will be more heavily contaminated than that of the ingot drawn therefrom. Therefore the ingot composition will approach a more heavily contaminated level as the quantity of the melt decreases due to lower or no addition of new material to the melt. This feature may be utilized for varying the composition of the ingot by a controlled addition of new material at a rate which Varies from the rate of withdrawal.
Although various specific embodiments of the invention herein have been disclosed, it will be understood that there is no intention to limit the scope of the present invention to these specific embodiments alone, since they are used for purposes of illustration only. Many details of composition and procedure may be varied Without departing from the principles of this invention. It is therefore not my purpose to limit the patent granted on this application otherwise than necessitated by the scope of the appended claims.
I claim as my invention:-
l. The method of growing a uniformly oriented body of a semiconductor material selected from the class consisting of germanium and silicon and including a substantial portion with a uniform and predetermined concentration of a certain doping impurity dispersed therethrough from a melt of said semiconductor material including a concentration of said doping impurity which is greater than said predetermined concentration, said method comprising withdrawing saidl body from said melt at a predetermined rate, and maintaining said melt at constant volume and constant concentration of said doping impurity after said body has acquired said predeterminedl concentration at the interface with said melt by simultaneonsly adding new material to said melt at a rate equal to the rate at which the material is being Withdrawn from said melt in the formation of said body and melting said new material in said melt, said new material consisting essentially of said semiconductor material and said dopingA irnpurity, with the concentration of said doping impurity in said new materiall being equal to said predeterminedl concentration.
2. The method'of growing crystalline ingots of a serniconductor material selectedffromA the class consisting of germanium and silicon and having a controlled rst predetermined concentration of a certain doping impurity which method includes providing a melt of said semiconductor material together with a second predetermined concentration of said certain doping impurity, said second predetermined concentration of said certain doping impurity being greater than said controlled first predetermined concentration thereof, and withdrawing an ingot from said melt at a predetermined rate, a substantial portion of which ingot contains said certain doping impurity in said controlled first predetermined concentration while maintaining the volume of the melt and the concentration of said certain doping impurity therein constant after said body has acquired said predetermined concentra- "tion at the interface with said melt by simultaneously adding to the melt additional amounts of said semiconductor material and said certain doping impurity at a rate equal to the rate at which the material is being Withdrawn from the melt in the formation of said ingot and melting said additional semiconductor material, the concentration of said certain doping impurity in the newly 15 2,739,088
References Cited in the tile of this patent UNITED STATES PATENTS 1,353,571 Dreibrodt Sept. 21, 1920 2,553,921 Jordan May 22, 1951 2,651,831 Bond et al. Sept. 15, 1953 2,709,842 Findlay June 7, 1955 2,727,839 Sparks Dec. 20, 1955 Pfann Mar. 20, 1956
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Cited By (71)

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US2977258A (en) * 1958-04-09 1961-03-28 Philco Corp Production of semiconductors and the like
US2993818A (en) * 1959-04-23 1961-07-25 Texas Instruments Inc Method for growing semiconductor crystals
US2999737A (en) * 1954-06-13 1961-09-12 Siemens And Halske Ag Berlin A Production of highly pure single crystal semiconductor rods
US3002824A (en) * 1956-11-28 1961-10-03 Philips Corp Method and apparatus for the manufacture of crystalline semiconductors
US3025191A (en) * 1953-07-13 1962-03-13 Raytheon Co Crystal-growing apparatus and methods
US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation
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US3050407A (en) * 1959-08-25 1962-08-21 Bell Telephone Labor Inc Single crystal garnets
US3070465A (en) * 1957-07-26 1962-12-25 Sony Corp Method of manufacturing a grown type semiconductor device
US3078151A (en) * 1958-11-17 1963-02-19 Siemens Ag Apparatus for drawing semiconductor bodies from a melt
US3098741A (en) * 1958-04-03 1963-07-23 Wacker Chemie Gmbh Process for effecting crucibleless melting of materials and production of shaped bodies therefrom
US3110674A (en) * 1959-09-23 1963-11-12 Bell Telephone Labor Inc Piezoelectric-ferromagnetic material
US3119778A (en) * 1959-01-20 1964-01-28 Clevite Corp Method and apparatus for crystal growth
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US3198606A (en) * 1961-01-23 1965-08-03 Ibm Apparatus for growing crystals
US3212871A (en) * 1960-12-16 1965-10-19 Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh Electrically heated tank furnace for melting quartz
US3240568A (en) * 1961-12-20 1966-03-15 Monsanto Co Process and apparatus for the production of single crystal compounds
US3305485A (en) * 1962-04-18 1967-02-21 Philips Corp Method and device for the manufacture of a bar by segregation from a melt
US3320045A (en) * 1962-06-25 1967-05-16 Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh Furnace for the manufacture of fused quartz
US3337303A (en) * 1965-03-01 1967-08-22 Elmat Corp Crystal growing apparatus
US3340016A (en) * 1963-09-26 1967-09-05 Consortium Elektrochem Ind Producing and regulating translatory movement in the manufacture of semiconductor bodies
US3342560A (en) * 1963-10-28 1967-09-19 Siemens Ag Apparatus for pulling semiconductor crystals
US3488157A (en) * 1964-07-03 1970-01-06 Wacker Chemie Gmbh Apparatus for manufacturing,purifying and/or doping mono- or polycrystalline semi-conductor compounds
US3607115A (en) * 1969-10-29 1971-09-21 Gen Motors Corp Crystal pulling from molten melts including solute introduction means below the seed-melt interface
US3637439A (en) * 1968-11-13 1972-01-25 Metallurgie Hoboken Process and apparatus for pulling single crystals of germanium
US3716345A (en) * 1969-03-18 1973-02-13 Siemens Ag Czochralski crystallization of gallium arsenide using a boron oxide sealed device
US3877880A (en) * 1971-07-31 1975-04-15 Kuhlmann Schafer Wilhelm Crystal melting apparatus fashioned to eliminate bubbles entrapped in the melt
US4036595A (en) * 1975-11-06 1977-07-19 Siltec Corporation Continuous crystal growing furnace
US4190631A (en) * 1978-09-21 1980-02-26 Western Electric Company, Incorporated Double crucible crystal growing apparatus
US4203951A (en) * 1976-11-23 1980-05-20 Eidelman Lev G Apparatus for growing single crystals from melt with additional feeding of comminuted charge
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US5306474A (en) * 1991-07-30 1994-04-26 Mitsubishi Materials Corporation Apparatus for growing single crystals
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US20050092236A1 (en) * 2003-11-03 2005-05-05 Bender David L. System for continuous growing of monocrystalline silicon
US20080134962A1 (en) * 2004-04-05 2008-06-12 Yasunao Oyama Crystallization method and crystallization apparatus
US8652257B2 (en) 2010-02-22 2014-02-18 Lev George Eidelman Controlled gravity feeding czochralski apparatus with on the way melting raw material
US20150144056A1 (en) * 2013-11-22 2015-05-28 Sunedison, Inc. Crystal growing systems and crucibles for enhancing heat transfer to a melt
US10407797B2 (en) * 2017-05-04 2019-09-10 Corner Start Limited Crystal pulling system and method including crucible and barrier

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US3036892A (en) * 1958-03-05 1962-05-29 Siemens Ag Production of hyper-pure monocrystal-line rods in continuous operation
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US3716345A (en) * 1969-03-18 1973-02-13 Siemens Ag Czochralski crystallization of gallium arsenide using a boron oxide sealed device
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US4036595A (en) * 1975-11-06 1977-07-19 Siltec Corporation Continuous crystal growing furnace
US4203951A (en) * 1976-11-23 1980-05-20 Eidelman Lev G Apparatus for growing single crystals from melt with additional feeding of comminuted charge
US4190631A (en) * 1978-09-21 1980-02-26 Western Electric Company, Incorporated Double crucible crystal growing apparatus
US4352784A (en) * 1979-05-25 1982-10-05 Western Electric Company, Inc. Double crucible Czochralski crystal growth apparatus
US4456499A (en) * 1979-05-25 1984-06-26 At&T Technologies, Inc. Double crucible Czochralski crystal growth method
US4246064A (en) * 1979-07-02 1981-01-20 Western Electric Company, Inc. Double crucible crystal growing process
JPS5768263A (en) * 1980-10-09 1982-04-26 Fujikura Ltd Dip forming method and crucible device for forming
JPS6350105B2 (en) * 1980-10-09 1988-10-06 Fujikura Cable Works Ltd
US4410494A (en) * 1981-04-13 1983-10-18 Siltec Corporation Apparatus for controlling flow of molten material between crystal growth furnaces and a replenishment crucible
US4659421A (en) * 1981-10-02 1987-04-21 Energy Materials Corporation System for growth of single crystal materials with extreme uniformity in their structural and electrical properties
EP0149898A3 (en) * 1983-12-24 1985-08-21 Sumitomo Electric Industries Limited An lec method and apparatus for growing a single crystal of compound semiconductors
EP0149898A2 (en) * 1983-12-24 1985-07-31 Sumitomo Electric Industries Limited An LEC method and apparatus for growing a single crystal of compound semiconductors
US4973454A (en) * 1983-12-24 1990-11-27 Sumitomo Electric Industries Ltd. LEC method and apparatus for growing a single crystal of compound semiconductors
US4638980A (en) * 1985-03-05 1987-01-27 Kloeckner-Humboldt-Deutz Ag Apparatus and method for maintaining the temperature of molten metal
WO1986006109A1 (en) * 1985-04-16 1986-10-23 Energy Materials Corporation Method and apparatus for growing single crystal bodies
WO1986006764A1 (en) * 1985-05-17 1986-11-20 J.C. Schumacher Company Continuously pulled single crystal silicon ingots
US4750969A (en) * 1985-06-27 1988-06-14 Research Development Corporation Of Japan Method for growing single crystals of dissociative compound semiconductor
US5030315A (en) * 1985-09-19 1991-07-09 Kabushiki Kaisha Toshiba Methods of manufacturing compound semiconductor crystals and apparatus for the same
US5021118A (en) * 1985-11-25 1991-06-04 Sumitomo Electric Industries, Ltd. Method of drawing-up a single crystal using a double-crucible apparatus and double-crucible apparatus and double-crucible apparatus therefor
US4894206A (en) * 1986-09-22 1990-01-16 Kabushiki Kaisha Toshiba Crystal pulling apparatus
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US4936949A (en) * 1987-06-01 1990-06-26 Mitsubishi Kinzoku Kabushiki Kaisha Czochraski process for growing crystals using double wall crucible
US5009862A (en) * 1987-06-01 1991-04-23 Mitsubishi Kinzoku Kabushiki Kaisha Apparatus and process for growing crystals of semiconductor materials
EP0294758A1 (en) * 1987-06-08 1988-12-14 Mitsubishi Materials Corporation Apparatus for growing crystals of semiconductor materials
EP0296401A1 (en) * 1987-06-09 1988-12-28 Nitto Chemical Industry Co., Ltd. Process for manufacturing fine silica particles
US5180562A (en) * 1987-10-03 1993-01-19 Leybold Aktiengesellschaft Apparatus for pulling monocrystals
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US5080873A (en) * 1987-11-02 1992-01-14 Mitsubishi Materials Corporation Apparatus for growing crystals
US5098674A (en) * 1987-12-03 1992-03-24 Toshiba Ceramics Co., Ltd. Powder supply device and method for a single crystal pulling apparatus
US5087321A (en) * 1987-12-08 1992-02-11 Nkk Corporation Manufacturing method and equipment of single silicon crystal
US5073229A (en) * 1988-02-25 1991-12-17 Kabushiki Kaisha Toshiba Semiconductor crystal pulling method
US5087429A (en) * 1988-04-28 1992-02-11 Nkk Corporation Method and apparatus for manufacturing silicon single crystals
US5196173A (en) * 1988-10-13 1993-03-23 Mitsubishi Materials Corporation Apparatus for process for growing crystals of semiconductor materials
US5009863A (en) * 1988-11-11 1991-04-23 Nkk Corporation Apparatus for manufacturing silicon single crystals
US4980015A (en) * 1989-02-03 1990-12-25 Mitsubishi Metal Corporation Method for pulling single crystals
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US5139750A (en) * 1989-10-16 1992-08-18 Nkk Corporation Silicon single crystal manufacturing apparatus
US5252175A (en) * 1990-06-29 1993-10-12 The United States Of America As Represented By The Secretary Of The Air Force Capillary pressure relief for magnetic Kyropoulos growth of semiconductor crystals
US5290395A (en) * 1990-07-26 1994-03-01 Sumitomo Electric Industries, Ltd. Method of and apparatus for preparing single crystal
US5292487A (en) * 1991-04-16 1994-03-08 Sumitomo Electric Industries, Ltd. Czochralski method using a member for intercepting radiation from raw material molten solution and apparatus therefor
US5306474A (en) * 1991-07-30 1994-04-26 Mitsubishi Materials Corporation Apparatus for growing single crystals
US5419462A (en) * 1992-09-09 1995-05-30 Albemarle Corporation Apparatus for recharging a heated receptacle with particulate matter at a controlled velocity
US5700321A (en) * 1994-10-14 1997-12-23 Komatsu Electronic Metals Co., Ltd. Method of feeding a dopant in a continuously charging method
US5900055A (en) * 1996-03-27 1999-05-04 Shin-Etsu Handotai Co., Ltd. Method of manufacturing silicon monocrystal by continuously charged Czochralski method
US20050092236A1 (en) * 2003-11-03 2005-05-05 Bender David L. System for continuous growing of monocrystalline silicon
US20080134958A1 (en) * 2003-11-03 2008-06-12 Solaicx, Inc System For Continuous Growing of Monocrystalline Silicon
US7635414B2 (en) 2003-11-03 2009-12-22 Solaicx, Inc. System for continuous growing of monocrystalline silicon
US8317919B2 (en) 2003-11-03 2012-11-27 Solaicx, Inc. System for continuous growing of monocrystalline silicon
US20100162946A1 (en) * 2004-02-27 2010-07-01 Solaicx, Inc. System for continuous growing of monocrystalline silicon
US20080134962A1 (en) * 2004-04-05 2008-06-12 Yasunao Oyama Crystallization method and crystallization apparatus
US7875118B2 (en) * 2004-04-05 2011-01-25 Canon Kabushiki Kaisha Crystallization method and crystallization apparatus
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US20150144056A1 (en) * 2013-11-22 2015-05-28 Sunedison, Inc. Crystal growing systems and crucibles for enhancing heat transfer to a melt
WO2015084602A1 (en) * 2013-11-22 2015-06-11 Sunedison, Inc. Crystal growing system and crucibles for enhancing the heat transfer to the melt by desinging a double crucible
CN106414815A (en) * 2013-11-22 2017-02-15 爱迪生太阳能公司 Crystal growing system and crucibles for enhancing the heat transfer to the melt by desinging a double crucible
US9822466B2 (en) * 2013-11-22 2017-11-21 Corner Star Limited Crystal growing systems and crucibles for enhancing heat transfer to a melt
US20180044815A1 (en) * 2013-11-22 2018-02-15 Corner Star Limited Crystal growing systems and crucibles for enhancing heat transfer to a melt
CN106414815B (en) * 2013-11-22 2019-01-11 各星有限公司 For enhancing the crystal growth system from the heat transmitting to melt and crucible of by designing double crucibles
TWI652380B (en) 2013-11-22 2019-03-01 香港商各星有限公司 Crystal growing systems and crucibles for enhancing heat transfer to a melt
US10407797B2 (en) * 2017-05-04 2019-09-10 Corner Start Limited Crystal pulling system and method including crucible and barrier
CN110741111A (en) * 2017-05-04 2020-01-31 各星有限公司 Crystal pulling system and method including crucible and barrier
CN110741111B (en) * 2017-05-04 2022-01-04 各星有限公司 Crystal pulling system and method including crucible and barrier

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