US3372003A - Apparatus and method for producing silicon single crystals for semiconductor - Google Patents

Apparatus and method for producing silicon single crystals for semiconductor Download PDF

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Publication number
US3372003A
US3372003A US383529A US38352964A US3372003A US 3372003 A US3372003 A US 3372003A US 383529 A US383529 A US 383529A US 38352964 A US38352964 A US 38352964A US 3372003 A US3372003 A US 3372003A
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United States
Prior art keywords
pulling
single crystal
crucible
silicon
crystal
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Expired - Lifetime
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US383529A
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English (en)
Inventor
Yamase Hideo
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JNC Corp
Shin Nippon Chisso Hiryo KK
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Chisso 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
    • C30B15/30—Mechanisms for rotating or moving either the melt or 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
    • C30B15/20—Controlling or regulating
    • 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
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • 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
    • Y10T117/1056—Seed pulling including details of precursor replenishment
    • 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
    • Y10T117/106—Seed pulling including sealing means details
    • 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
    • Y10T117/1064—Seed pulling including a fully-sealed or vacuum-maintained crystallization chamber [e.g., ampoule]

Definitions

  • ABSTRACT OF THE DISCLOSURE Method and apparatus for producing silicon single crystal by pulling a silicon single crystal from to 60% by weight of molten silicon in a crucible charged with polycrystalline silicon in one pulling cycle, transferring a pulling apparatus together with a pulled single crystal to a single crystal detaching position while simultaneously applying another pulling apparatus to the crucible and charging polycrystalline silicon in an amount corresponding to the pulled single crystal for use of subsequent pulling cycle and repeating the operation.
  • This invention relates to an apparatus and a method for producing silicon single crystal, by use of one crucible and a plurality of transferable pulling mechanisms.
  • Silicon single crystal with relatively higher resistivity is hard to obtain by this method, compared with the methods of float zone and others.
  • the resistivity distribution in the axial direction of the crystal is determined by the segregation coefficient of the adulterant impurities in this silicon single crystal.
  • an object of this invention to provide a method for producing silicon single crystal whose distribution of resistivity in the axial direction is comparable to that obtained by the ideal continuous charging pulling method and distribution of resistivity in the horizontal cross section is uniform, i.e. radial spread is narrow.
  • the objects of this invention have been accomplished by repetition of the operation consisting of pulling a silicon single crystal from 10 to 60% by weight of molten silicon in a crucible charged with polycrystalline silicon in one pulling cycle, transferring a pulling apparatus together with a pulled up single crystal to a single crystal detaching position while simultaneously applying another pulling apparatus to the said crucible, and charging polycrystalline silicon in an amount corresponding to the pulled up amount of single crystal for use of subsequent pulling cycle.
  • the method and the apparatus of this invention will be more fully understood referring to drawings.
  • FIG. 1 shows an elevation of vertical cross section taken along the line passing the center of turn table and the center of crucible of single crystal pulling apparatus according to the present invention.
  • FIG. 2 shows a plan of the sliding turn table, constituting the said apparatus.
  • FIG. 3 shows the theoretical resistivity distribution curves in axial direction of pulled silicon single crystals doped by boron, phosphorous or antimony.
  • FIG. 4 shows the actual resistivity distribution curves in axial direction of silicon single crystals doped by boron, phosphorous or antimony pulled by this invented method and apparatus.
  • FIG. 5 shows the relation between molten polycrystalline crystals in the crucible and a growing single crystal.
  • Polycrystalline silicon is charged from a charging hole 11 through a introducing pipe 12 to a quartz crucible 3 fixed in a carbon crucible 2, and molten therein.
  • the introducing pipe 12 can be lifted up to the position not inconvenient to the pulling up operation during the time when this operation is being carried out while maintaining the air-tightness of the apparatus. Melting is carried out by use of a high frequenc induction heating coil 1 to which high frequency electric power is fed from a high frequency oscillator, not shown.
  • thermo-couple radiation detector 5 connected to automatic temperature control system, not shown.
  • the quartz crucible has much larger capacity (the kg), and the crucible rotation system 4 makes the cru niechie rotate so as to enable to heat by the high frequency heating coilun'iforrrily.
  • the rotation mechanism 8 of the pulling shaft and rotating mechanism 9 of pulling work to pull up gradually the silicon single crystal, and the single crystal grows at the end of the seed in a bar form of specified shape and diameter. The growth can be controlled by the temperature controlling mechanism.
  • the cover 10 of the cone type furnace is made of transparent Pyrex glass or transparent quartz glass to make it easy to watch the single crystal being pulled.
  • At least two pulling mechanisms are fixed to the top surface of the fixing board, and the bottom surface of sliding turn table 16 is turned by the rotating shaft while sliding with-out leaking gas from the inside of the furnace by use of such elas-tomeric material as O-ring of Teflon rubber, Viton or the like as packing.
  • Each pulling shaft is moved by turning the table from the place 18 to the place 20, from the place 19 to the place 18, after the shaft being pulled up at a position higher than the level of the sliding turn table.
  • the pulling shaft contacts the melted silicon and the pulling operation begins, but if it is required to cut off the crystal when it pulls 10 to 60% of the melted polycrystalline silicon in the crucible depending on its specification of the single crystal product required, by suddenly speeding up the pulling speed.
  • the shaft with the single crystal thus cut off is further pulled u wards above the level of the sliding turn table, and the sliding turn table is turned to move the pulling shaft from the place 18 to the place 21 and at the same time the pulling shaft at the place 19 where another pulling shaft having a piece of seed under its tail and wating its turn to pull the crystal comes to the place 18, contact the furnace and begins to pull the crystal.
  • the polycrystalline silicon in the crucible may be left at molten state, but it is advisable to decrease the high frequency input and the temperature in the crucible to about 900 C. to solidify the molten polycrystalline silicon in the crucible in order that the subsequent operation can be carried out at stabilized condition.
  • the polycrystalline silicon are gradually supplied through 11 and 12 to the crucible, in an amount corresponding to the quantity pulled in the above-mentioned cycle.
  • the pipe 12 After charging the polycrystalline silicon, the pipe 12 is slide back upwards to its position normally placed during the time when charging is not conducted so as not to prevent the pulling operation, and the high frequency input is increased gradually to melt the material in the crucible and to make the material ready to be pulled.
  • FIG. 3 shows the tendency of the theoretical distribution of resistivity in the axial direction of the single crystal bar when doped phosphorous, boron or antimonyn
  • the segregation coefficient (K) of each dopant is as follows:
  • p(O) means the top resistivity of the single crystal
  • p(X) means the resistivity at the place of X% in the axial direction.
  • FIG. 4 shows the actual curves of resistivity, actually measured which is considered to be also influenced by the vaporized impurities from the molten polycrystalline silicon in the large crucible used in this invention.
  • the curves in FIG. 4 is flatter than those in FIG. 3.
  • the material which can be used for semiconductor is the part between or and ⁇ 3 in FIG. 4 namely the fiat part of the resistivity.
  • the apparatus of the present invention has a plurality of pulling mechanisms, it is possible to take a emergency measure quickly.
  • Do means a diameter of a crucible
  • Ds means a diameter of a growing single crystal
  • 7 means a growing surface of the single crystal.
  • melting is performed by use of a high frequency induction heating furnace, but it is to be understood that a resistivity heating furnace can also be applied in very much the same way.
  • a method for producing ultra pure silicon single crystals from molten polycrystalline silicon crystals comprising a repetition of the steps consisting of pulling a silicon single crystal from 10 to 60 percent by weight of molten silicon in a crucible having capacity from one to three kg. charged with polycrystalline silicon in one pulling cycle, transferring a pulling apparatus together with a pulled single crystal to a detaching position when the above-mentioned pulling is finished while applying another pulling apparatus to the said crucible and charging polycrystalline silicon in an amount corresponding to the pulled quantity of single crystal for use of subsequent pulling cycle.
  • An apparatus for producing ultra pure silicon crystals from molten polycrystalline silicon crystals comprising a turn table which is rotatable around a central axis and a fixed table which supports a furnace and has elastomeric rings between the above-mentioned turn table for securing the tightness of the furnace, the above mentioned furnace having a crucible in the inside and equipped with a heating mechanism, a temperature measuring mechanism and a polycrystalline silicon crystals charging pipe and at least two pulling shafts which can be rotated and moved in a case communicated to the furnace when used in the pulling between the distance which enables its tail to touch the molten polycrystalline silicon in the crucible and to be lifted up to the level higher than the fixed bed forming the upper mouth of the furnace.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
US383529A 1963-07-19 1964-07-17 Apparatus and method for producing silicon single crystals for semiconductor Expired - Lifetime US3372003A (en)

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Application Number Priority Date Filing Date Title
JP3889763 1963-07-19

Publications (1)

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US (1) US3372003A (enrdf_load_stackoverflow)
BE (1) BE650792A (enrdf_load_stackoverflow)
GB (1) GB1027662A (enrdf_load_stackoverflow)
NL (1) NL6408232A (enrdf_load_stackoverflow)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3865554A (en) * 1971-09-23 1975-02-11 Little Inc A Pressure-and temperature-controlled apparatus for large-scale production of crystals by the czochralski technique
US3929557A (en) * 1973-06-11 1975-12-30 Us Air Force Periodically and alternately accelerating and decelerating rotation rate of a feed crystal
US5135727A (en) * 1990-11-29 1992-08-04 Shin-Etsu Handotai Co., Ltd. Automatic single crystal ingot disconnector for single crystal pulling apparatus
FR3055562A1 (fr) * 2016-09-08 2018-03-09 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de tri de plaquettes en silicium en fonction de la variation du dopage net
US11077469B2 (en) * 2016-09-08 2021-08-03 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for sorting silicon wafers according to their bulk lifetime
CN116411351A (zh) * 2023-03-07 2023-07-11 襄阳鸿凯智能装备有限公司 一种硅碳材料生产装置

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL139601B1 (en) * 1983-08-30 1987-02-28 Inst Tech Material Elekt Method of obtaining cristals in particular those of semiconductor materials
FR2551470B1 (fr) * 1983-09-06 1985-11-08 Crismatec Tete de tirage de monocristaux

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2753280A (en) * 1952-05-01 1956-07-03 Rca Corp Method and apparatus for growing crystalline material
US2889240A (en) * 1956-03-01 1959-06-02 Rca Corp Method and apparatus for growing semi-conductive single crystals from a melt
US3154384A (en) * 1960-04-13 1964-10-27 Texas Instruments Inc Apparatus for growing compound semiconductor crystal

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2753280A (en) * 1952-05-01 1956-07-03 Rca Corp Method and apparatus for growing crystalline material
US2889240A (en) * 1956-03-01 1959-06-02 Rca Corp Method and apparatus for growing semi-conductive single crystals from a melt
US3154384A (en) * 1960-04-13 1964-10-27 Texas Instruments Inc Apparatus for growing compound semiconductor crystal

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3865554A (en) * 1971-09-23 1975-02-11 Little Inc A Pressure-and temperature-controlled apparatus for large-scale production of crystals by the czochralski technique
US3929557A (en) * 1973-06-11 1975-12-30 Us Air Force Periodically and alternately accelerating and decelerating rotation rate of a feed crystal
US5135727A (en) * 1990-11-29 1992-08-04 Shin-Etsu Handotai Co., Ltd. Automatic single crystal ingot disconnector for single crystal pulling apparatus
FR3055562A1 (fr) * 2016-09-08 2018-03-09 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de tri de plaquettes en silicium en fonction de la variation du dopage net
WO2018046854A1 (fr) * 2016-09-08 2018-03-15 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procédé de tri de plaquettes en silicium en fonction de la variation du dopage net
US11077469B2 (en) * 2016-09-08 2021-08-03 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for sorting silicon wafers according to their bulk lifetime
CN116411351A (zh) * 2023-03-07 2023-07-11 襄阳鸿凯智能装备有限公司 一种硅碳材料生产装置
CN116411351B (zh) * 2023-03-07 2023-09-26 襄阳鸿凯智能装备有限公司 一种硅碳材料生产装置

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Publication number Publication date
BE650792A (enrdf_load_stackoverflow) 1964-11-16
GB1027662A (en) 1966-04-27
NL6408232A (enrdf_load_stackoverflow) 1965-01-20

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