US3499736A - X-ray or gamma ray use in control of crystal diameter - Google Patents

X-ray or gamma ray use in control of crystal diameter Download PDF

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Publication number
US3499736A
US3499736A US584584A US3499736DA US3499736A US 3499736 A US3499736 A US 3499736A US 584584 A US584584 A US 584584A US 3499736D A US3499736D A US 3499736DA US 3499736 A US3499736 A US 3499736A
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United States
Prior art keywords
crystal
diameter
crucible
melt
ray
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Expired - Lifetime
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US584584A
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English (en)
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Gooitzen Zwanenburg
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US Philips Corp
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US Philips 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
    • C30B15/20—Controlling or regulating
    • C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
    • C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
    • 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
    • Y10T117/1004—Apparatus with means for measuring, testing, or sensing
    • Y10T117/1008—Apparatus with means for measuring, testing, or sensing with responsive control means
    • 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
    • Y10T117/1012—Apparatus with means for measuring, testing, or sensing with a window or port for visual observation or examination

Definitions

  • the invention relates to a method for pulling crystals from a melt in a crucible, in which the diameter of the growing crystal is controlled and to a device suitable for carrying out said method.
  • the diameter of the growing portion should be controlled in the desired manner with optimum accuracy, particularly that the diameter of the crystal should have a constant value over large part of its length. It is known that this diameter depends upon various conditions chosen for the growth, for example, the temperature of the melt and the pulling rate and it has been proposed to adjust the desired diameter or the desired varia tion of this diameter by correct adjustment of said conditions.
  • Thecontrol of the diameter involves, however, the difficulty that the growth region of the crystal is located inside the crucible and that the diameter of the growing crystal portion and the possible variation thereof can be checked only by observation via the open upper side of the crucible. This observation is the more difiicult the lower becomes the level of the melt in the crucible and the larger is the diameter of the crystal.
  • the present invention has for its object inter alia to obviate the aforesaid disadvantages.
  • the method of pulling crystals from a melt in a crucible, in which the diameter of the growing crystal is controlled is characterized in accordance with the invention in that the diameter of the growing crystal is determined and/or controlled by means of X-rays or gamma rays passing through the wall of the crucible.
  • an image comprising the shadow of the growing crystal portion, projected outside the crucible by the X-rays or gamma rays may be converted into an image of visible light, for example, by means of a fluorescent screen sensitive to the radiation concerned, if necessary with image intensification or by using a pick-up tube sensitive to the radiation concerned which converts the radiation image into an electrical signal which is used for forming an image of visible light in a display tube.
  • the factor of magnification of the image may be readily determined in advance, for ex- 'ice ample, by means of the dimensions of the apparatus or by calibration with one or more rods of known diameters.
  • the image of the growing portion is not affected by the crystal portions lying above said portion or by the crystal holder.
  • optoelectrical converters for keeping the diameter constant, the signals provided by said converters being employed for adjusting, for example, the temperature of the melt or the pulling rate.
  • the term opto-electrical converters is not restricted to converters responding to visible light, but it includes also converters capable of converting X-rays or gamma radiation into electrical signals, for example, Geiger counters or scintillation counters.
  • Converters of the last-mentioned kind are capable of responding directly to a displacement of the shade boundary of the growing rod portion, whilst other opto-electrical converters, which respond for example to visible light, may be employed in conjunction with an image converter which converts the image projected by the X-rays or gamma rays into an image of visible light.
  • Image intensification and, if desired, optical magnification, for example, by means of lenses may be carried out.
  • the parameters of the pulling apparatus determining the diameter of the growing crystal particularly the increase or the decrease of said diameter, for example the degree of heating of the melt and the pulling rate can be acted upon, in order to reset the diameter in the case of a small deviation therefrom.
  • the invention furthermore relates to a device for pulling crystals from a melt, said device comprising a crucible for the melt, a holder vertically movable with respect to the crucible for pulling a crystal, heating means for the melt and control-means for adjusting and/ or varying one or more of the parameters acting upon the diameter of the crystallizing portion, for example the degree of heating of the melt and the pulling rate.
  • This device is provided, in accordance with the invention, with a source of X-rays or gamma rays, disposed at the side of the crucible and a receiver arranged on the opposite side of the crucible which converts the radiation into a visible image and/0r into one or more electrical signals.
  • the present invention permits inter alia of manufacturing single crystal rods of semiconductor material, for example, germanium or silicon, 0f diameters of more than 25 mms. for example 30 to 50 mms., the rod diameter being kept accurately constant with a tolerance of 1 mm. Since the inner diameter of the crucible need no longer be chosen so large as would be desirable for a satisfactory observation from above, the horizontal dimensions of the crucible and of the heating means, for example, a high-frequency coil, with respect to the known apparatus for maximum crystal diameters of 15 to 25 mms. need not be enlarged proportionally to the relevant crystal diameters. The hindrance of observation is no longer a factor determinative of the height of the crucible, so that the invention furthermore permits of obtaining longer crystals, or particularly when forming crystals of large diameters crystals of reasonable length.
  • semiconductor material for example, germanium or silicon
  • FIG. 1 shows diagrammatically a vertical sectional view of an embodiment of a device for pulling crystals
  • FIG. 2 is a front view of the X-ray image screen designed in FIG. 1 in the direction of the arrows.
  • the apparatus shown in FIG. 1 comprises a quartz tube 1, having an outer diameter of 130 mms. and a wall thickness of 2.5 mms.
  • the lower end and the upper end of the tube are provided with closing members 2 and 3, respectively, in which gas inlet and gas outlet channels (not shown) are provided.
  • On the upper side and on the lower side two shafts 4 and 5 respectively are taken through the wall in a gas-tight manner so as to be vertically movable and rotatable about their centre lines.
  • the lower shaft 5 ness.
  • the crucible 9 is surrounded by a heat-insulating sheath 14 of graphite felt of 5 mms. thickness.
  • the upper shaft 4 is provided at the lower end with a crystal holder 11 for the crystal to be drawn.
  • the tube 1 is surrounded by a. cylindrical high-frequency coil 12 formed by a single winding and a cylindrically curved, copper plate.
  • the coils has an inner diameter of 135 mms. and a height of 130 mms. and is provided with a welded copper cooling duct 13.
  • the high-frequency coil is connected to a high-frequency generator 32.
  • the X-ray tube may be a commercially available tube of the trademark Practix 90/20 type XB 2000, which can be driven continuously at a voltage of 70 kv. and a current intensity of 0.8 ma;
  • an X-ray screen 22 is arranged, which is sensitive to X-rays and which produces a visible image picture of the image projected by the X-rays onto the screen.
  • the X-ray tube 20 and the diaphragm 21 are disposed so that the X-beam emanating from the centre of the diaphragm is horizontally directed to the axis of the cylindrical crucible.
  • the cylindrical high-frequency coil 12, having a wall thickness of 2 mms., comprises two copper windows 23 and 24 of a thickness of 0.15 mm. for passing the X-ray beam towards the image screen.
  • the apparatus comprises furthermore a control for manual adjustment and control of the driving device 7 for the vertical movement of the shaft 4 with the crystal holder 11, a control 31 for the manual adjustment and control of the high-frequency generator 32 supplying the current to the'high-frequency coil 12 and a control 33 for the manual adjustment and control of the driving device 6 for the vertical movement of the shaft 5 with the support 8 and the crucible 9.
  • This apparatus may be used as follows for growing a crystal, for example, of germanium or silicon.
  • a quantity of a material for a crystal to be made, for example germanium or silicon is put in the crucible 9 and a seed crystal 40 is fastened to the crystal holder 11.
  • the high-frequency coil 12 is energized so that the crucible 9 is heated and the crystal material in the crucible is melted.
  • the crucible is simultaneously rotated about its vertical axis. Then the X-ray tube is ignited and driven continuously with a current intensity of 0.8 mat. and a direct voltage of 70 kv.
  • the shaft 5 is displaced vertically so that the meniscus of the melt 41 in the crucible is located approximately at the level of the anode of the X-ray tube 20 and the diaphragm 21, so that an image of this meniscus appears on the screen 22 and the correct height can be adjusted.
  • the shaft 4 with the crystal holder 11 and the seed crystal 40 is then moved downwards to an extent such that the lower end of the seed crystal is just above the melt, which can be observed from the shadow image on the screen 22.
  • the seed crystal 40 is preheated by the radiation from the melt and the wall of the crucible. Then the shaft 4 is moved further downwards until the lower end of the seed crystal is dipped into the melt.
  • the seed crystal is then gradually pulled upwards, whilst the rate of the upward movement of the shaft 4, and by controlling the supply current of the high-frequency generator 32, the temperature of the melt are adjusted so that the diameter of the portion growing on the seed crystal 40 is gradually reduced, after which it is kept constant whilst the image screen 22 is observed.
  • the thin portion 42 of the growing crystal thus formed any dislocations of the seed crystal grow for the major part towards the surface of the thin crystal portion.
  • the temperature of the melt is subsequently reduced, so that the crystal diameter widens conically to the desired rod diameter.
  • the pulling rate of the crystal and the temperature of the melt are adjusted so that a further growth with a substantially constant diameter is obtained.
  • An accurate check of the diameter of the portion 43 of the growing crystal is rendered possible by the picture on the screen 22.
  • FIG. 2 shows clearly the screen 22 with the picture of the lower portion 53 of the growing crystal and the portion of the melt 51 from which the crystal is drawn.
  • the diameter of the growing portion can be accurately determined by means of a calibration 55 on the screen. Since during the growth of the crystal the meniscus of the melt in the crucible falls down at a rate depending upon the quantity of crystallized material per unit time, the crucible is moved upwards by means of the shaft 5 and the driving mechanism 6 so that the height of the meniscus 56 reproduced on the screen 22 is kept constant.
  • said diameter can be returned to the desired value by means of the controls 30 and/or 31.
  • the rod diameter can be gradually reduced by raising the pulling rate and/ or by raising the temperature of the melt, so that a conical portion grows on, the reduced diameter being then maintained until the portion 43 of constant diameter just emerges from the upper edge of the crucible.
  • the portion 43 is thus cooled in the same manner throughout its length, so that the crystal prefection is as uniform as possible throughout its length.
  • the last molten rest of the material to be crystallized is grown on the crystal end.
  • the crucible or at least the inner quartz portion 10 thereof may crack, when the crucible cools down and the rest solidifies.
  • the invention is not restricted to the apparatus described here by way of example, many variants being possible within the scope of the present invention. It is furthermore evident, that the design of the apparatus should be adapted to the use of X-ray and gamma ray radiation, for example, by choosing the material and the thickness of the transmitting parts also with a view to the radiation used, for example the hardness thereof.
  • a method of pulling crystals from a melt in a crucible in which the diameter of the growing crystal is controlled, characterized in that the diameter of the growing portion of the crystal is controlled responsive to X-rays or gamma radiation passing through the wall of the crucible and the grown crystal containing information of the diametral extent of the grown crystal.
  • a method as claimed in claim 1 characterized in that an image projected outside the crucible by the X-rays or gamma rays, including the shadow of the growing portion of the crystal, is converted into an image of visible light.
  • An apparatus for pulling crystals from a melt in which the diameter of the growing crystal is controlled comprising a crucible for the melt, a holder for the crystal to be grown, said holder being vertically movable with respect to the crucible, heating means for the melt, and control-means for adjusting and varying at least one of the parameters acting upon the diameter of the crystallizing portion, said parameters including the degree of heating of the melt and the pulling rate, characterized in that said apparatus further comprises a source of X-rays or gamma radiation arranged at the side of the crucible and means arranged on the opposite side of the crucible for converting said radiation passing through the Walls of said crucible and projecting an image of the diametrical extent of the grown crystal into a visible image or electrical signal.
US584584A 1965-10-06 1966-10-05 X-ray or gamma ray use in control of crystal diameter Expired - Lifetime US3499736A (en)

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NL6512921A NL6512921A (de) 1965-10-06 1965-10-06

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US (1) US3499736A (de)
AT (1) AT296388B (de)
BE (1) BE687917A (de)
CH (1) CH491659A (de)
DE (1) DE1519850C3 (de)
FR (1) FR1509967A (de)
GB (1) GB1154240A (de)
NL (1) NL6512921A (de)
SE (1) SE328851B (de)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3870477A (en) * 1972-07-10 1975-03-11 Tyco Laboratories Inc Optical control of crystal growth
US3998598A (en) * 1973-11-23 1976-12-21 Semimetals, Inc. Automatic diameter control for crystal growing facilities
US4080172A (en) * 1975-12-29 1978-03-21 Monsanto Company Zone refiner automatic control
US4239583A (en) * 1979-06-07 1980-12-16 Mobil Tyco Solar Energy Corporation Method and apparatus for crystal growth control
DE3036178A1 (de) * 1979-10-09 1981-04-23 Siltec Corp., Menlo Park, Calif. Leitung zum ueberfuehren eines fluessigkeitsstroms aus geschmolzenem halbleitermaterial
US4352785A (en) * 1982-01-04 1982-10-05 Western Electric Co., Inc. Crystal grower with torque supportive collapsible pulling mechanism
US4596700A (en) * 1983-11-22 1986-06-24 Sumitomo Electric Industries, Ltd. Apparatus for producing single crystal
US4618975A (en) * 1984-12-21 1986-10-21 At&T Technologies, Inc. Method and apparatus for analyzing a porous nonhomogeneous cylindrical object
US4634490A (en) * 1983-12-16 1987-01-06 Sumitomo Electric Industries, Ltd. Method of monitoring single crystal during growth
US5078830A (en) * 1989-04-10 1992-01-07 Mitsubishi Metal Corporation Method for growing single crystal
US5589690A (en) * 1995-03-21 1996-12-31 National Institute Of Standards And Technology Apparatus and method for monitoring casting process
US20050045094A1 (en) * 2003-08-29 2005-03-03 University Of Alabama In Huntsville Crystallization cassette for the growth and analysis of macromolecular crystals and an associated method
US20070034139A1 (en) * 2003-03-28 2007-02-15 Tsuguo Fukuda Method for analyzing impurities (color centers) of fluoride and process for producing material for growing single crystal
CN105350072A (zh) * 2015-11-06 2016-02-24 南京晶升能源设备有限公司 泡生法晶体生长单晶炉脱锅方法、温控方法和控制方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06102590B2 (ja) * 1990-02-28 1994-12-14 信越半導体株式会社 Ｃｚ法による単結晶ネック部育成自動制御方法
US5746828A (en) * 1996-01-16 1998-05-05 General Signal Corporation Temperature control system for growing high-purity monocrystals
CN112705590B (zh) * 2020-12-11 2023-02-07 山东新升光电科技有限责任公司 一种蓝宝石单晶炉提拉杆矫直装置及方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2992311A (en) * 1960-09-28 1961-07-11 Siemens Ag Method and apparatus for floatingzone melting of semiconductor rods
US3001070A (en) * 1956-02-09 1961-09-19 Jr William H Davis Method of gaging filling heights in closed containers
US3011055A (en) * 1954-06-03 1961-11-28 J J Maguire Method and means for gauging fine strands
US3046379A (en) * 1959-09-11 1962-07-24 Siemens Ag Method and apparatus for zone melting of semiconductor material
US3190727A (en) * 1960-06-25 1965-06-22 Ronette Piezo Electrische Ind Apparatus for melting powdered material by means of a flame elevated temperature
US3265470A (en) * 1959-08-17 1966-08-09 Siemens Ag Method and apparatus for floating-zone melting of semiconductor material
US3372276A (en) * 1965-05-21 1968-03-05 Atomic Energy Commission Usa Method and system for the non-destructive inspection of variable density plates

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3011055A (en) * 1954-06-03 1961-11-28 J J Maguire Method and means for gauging fine strands
US3001070A (en) * 1956-02-09 1961-09-19 Jr William H Davis Method of gaging filling heights in closed containers
US3265470A (en) * 1959-08-17 1966-08-09 Siemens Ag Method and apparatus for floating-zone melting of semiconductor material
US3046379A (en) * 1959-09-11 1962-07-24 Siemens Ag Method and apparatus for zone melting of semiconductor material
US3190727A (en) * 1960-06-25 1965-06-22 Ronette Piezo Electrische Ind Apparatus for melting powdered material by means of a flame elevated temperature
US2992311A (en) * 1960-09-28 1961-07-11 Siemens Ag Method and apparatus for floatingzone melting of semiconductor rods
US3372276A (en) * 1965-05-21 1968-03-05 Atomic Energy Commission Usa Method and system for the non-destructive inspection of variable density plates

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3870477A (en) * 1972-07-10 1975-03-11 Tyco Laboratories Inc Optical control of crystal growth
US3998598A (en) * 1973-11-23 1976-12-21 Semimetals, Inc. Automatic diameter control for crystal growing facilities
US4080172A (en) * 1975-12-29 1978-03-21 Monsanto Company Zone refiner automatic control
US4239583A (en) * 1979-06-07 1980-12-16 Mobil Tyco Solar Energy Corporation Method and apparatus for crystal growth control
DE3036178A1 (de) * 1979-10-09 1981-04-23 Siltec Corp., Menlo Park, Calif. Leitung zum ueberfuehren eines fluessigkeitsstroms aus geschmolzenem halbleitermaterial
US4396824A (en) * 1979-10-09 1983-08-02 Siltec Corporation Conduit for high temperature transfer of molten semiconductor crystalline material
US4352785A (en) * 1982-01-04 1982-10-05 Western Electric Co., Inc. Crystal grower with torque supportive collapsible pulling mechanism
US4596700A (en) * 1983-11-22 1986-06-24 Sumitomo Electric Industries, Ltd. Apparatus for producing single crystal
US4634490A (en) * 1983-12-16 1987-01-06 Sumitomo Electric Industries, Ltd. Method of monitoring single crystal during growth
US4618975A (en) * 1984-12-21 1986-10-21 At&T Technologies, Inc. Method and apparatus for analyzing a porous nonhomogeneous cylindrical object
US5078830A (en) * 1989-04-10 1992-01-07 Mitsubishi Metal Corporation Method for growing single crystal
US5589690A (en) * 1995-03-21 1996-12-31 National Institute Of Standards And Technology Apparatus and method for monitoring casting process
US20070034139A1 (en) * 2003-03-28 2007-02-15 Tsuguo Fukuda Method for analyzing impurities (color centers) of fluoride and process for producing material for growing single crystal
US20050045094A1 (en) * 2003-08-29 2005-03-03 University Of Alabama In Huntsville Crystallization cassette for the growth and analysis of macromolecular crystals and an associated method
US7118626B2 (en) 2003-08-29 2006-10-10 University Of Alabama In Huntsville Crystallization cassette for the growth and analysis of macromolecular crystals and an associated method
CN105350072A (zh) * 2015-11-06 2016-02-24 南京晶升能源设备有限公司 泡生法晶体生长单晶炉脱锅方法、温控方法和控制方法

Also Published As

Publication number Publication date
NL6512921A (de) 1967-04-07
DE1519850A1 (de) 1969-03-20
FR1509967A (fr) 1968-01-19
DE1519850B2 (de) 1974-12-12
CH491659A (de) 1970-06-15
GB1154240A (en) 1969-06-04
SE328851B (de) 1970-09-28
BE687917A (de) 1967-04-06
DE1519850C3 (de) 1975-07-31
AT296388B (de) 1972-02-10

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