US2858199A - Crystal production - Google Patents

Crystal production Download PDF

Info

Publication number
US2858199A
US2858199A US462427A US46242754A US2858199A US 2858199 A US2858199 A US 2858199A US 462427 A US462427 A US 462427A US 46242754 A US46242754 A US 46242754A US 2858199 A US2858199 A US 2858199A
Authority
US
United States
Prior art keywords
block
crystal
crucible
melted
seed crystal
Prior art date
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
Application number
US462427A
Inventor
Larson Christian Charles
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.)
TDK Micronas GmbH
International Telephone and Telegraph Corp
Original Assignee
Deutsche ITT Industries GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to BE542056D priority Critical patent/BE542056A/xx
Application filed by Deutsche ITT Industries GmbH filed Critical Deutsche ITT Industries GmbH
Priority to US462427A priority patent/US2858199A/en
Priority to GB29341/55A priority patent/GB778123A/en
Application granted granted Critical
Publication of US2858199A publication Critical patent/US2858199A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • 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
    • C30B15/14Heating of the melt or the crystallised materials
    • C30B15/16Heating of the melt or the crystallised materials by irradiation or electric discharge
    • 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
    • Y10S117/905Electron beam
    • 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
    • Y10S164/00Metal founding
    • Y10S164/04Dental

Definitions

  • the present invention relates to crystal production, and more particularly to a method for manufacturing crystals which may be used as elements of transistors.
  • meltted silicon in particular is of such high temperature that the usual crucibles are damaged or destroyed. No known crucible materials have yet been developed which will reliably withstand the high temperatures of molten silicon.
  • An object of the present invention is to provide a method for producing crystals without the need of a crucible.
  • Fig. 1 is a vertical sectional elevation of an embodiment of this invention
  • Fig. 2 is a top plan View thereof
  • Fig. 3 is a diagrammatic illustration of an electron gun used in the apparatus of Fig. 1;
  • Fig. 4 is a perspective illustration showing one step of the method of drawing a crystal.
  • the apparatus comprises an evacuated bell jar 1 which is hermetically sealed to a metallic base 2.
  • a shaft or rod 3 is reciprocably mounted in the top portion of the bell jar by means of a suitable threaded connection with a hermetically sealed coupling 4.
  • Suitable constructions for reciprocating the rod 3 from a position outside of the bell jar 1 are wellknown to the art and in particular are described in a publication entitled Vacuum Equipment and Techniques by Guthrie and Wakerling, published by the McGraw-Hill Book Company and copyrighted in 1949.
  • a plurality of suitable electron guns 5 are circumferentially mounted on the top portion of the bell jar in 2,858,199 Patented Oct. 28, 1958 such a manner as to direct high density electron beams along the paths indicated by the dashed lines 6.
  • These electron guns 5 may be of conventional construction and correspond to the electron gun arrangement disclosed in Gardner Patent 2,128,581.
  • a suitable gun construction is diagrammatically illustrated in Fig. 3 wherein electrons emitted by a cathode 7 are concentrated into a pencil-like beam by an anode 8 and accelerated by both this anode 8 and another anode 9. As will become apparent from the following description, this pencil-like beam must be of high density.
  • a block 10 of silicon, germanium, or the like material On the base 2 of the bell jar 1 is placed a block 10 of silicon, germanium, or the like material in such position that the central portion thereof will be bombarded by the respective electron beams 6.
  • These beams 6 are of such high density as to melt the central portion of the block 10. The beams are so controlled that only the central portion of the block is melted, whereby the block serves as a crucible for the melted portion.
  • a seed crystal of the type which is to be finally produced is clamped by some suitable means in the lower end of the reciprocable rod 3, and such a starter or seed crystal is indicated in Figs. 1 and 4 by the reference numeral 11.
  • the rod 3 is lowered until the seed crystal 11 just touches the molten material, and is then withdrawn upwardly at a slow rate which will allow the molten material to continuously form on the lower end of the seed crystal.
  • Continued withdrawal of the seed crystal thereby ostensibly draws or pulls a suitable crystal structure from the solid block.
  • the beams 6 are trained onto the areas surrounding the drawn crystal, whereupon the operation may be continued until the block 10 is substantially consumed.
  • the block 10 acquires an electrostatic charge from the electron beams 6, it is desirable to provide a conductive return path for current fiowfrom the base 10 to one of the gun anodes, such as the anode 9.
  • a wire 12 is shown as providing this conductive path. While there has been shown a plurality of individual electron guns 5, it is possible to utilize a single electron gun of annular configuration which will produce a tapered, hollow electron beam for melting the block 10 in the vicinity surrounding the seed crystal 11.
  • the method of fabricating crystals comprising born barding a portion of a block of material from which a crystal is to be made with electrons, said bombardment serving to melt said portion, said portion being disposed in one block surface inside the perimeter thereof, and drawing a seed crystal from said melted portion, the unmelted portion of said block serving as a crucible for the melted portion.
  • the method of fabricating crystals comprising selective melting a central portion of a block of material from which a crystal is to be made, said portion being disposed in one surface between the lateral block sides, drawing a seed crystal from said melted portion, the unmelted portion of said block serving as a crucible for the melted portion, and continuing to melt said block in the perimetral vicinity of the crystal being drawn.
  • the method of fabricating crystals from a block of material from which a crystal is to be made comprising positioning a self-supporting block of said material in an evacuated container focusing an electron beam on the upper surface of said block, increasing the energy in said beam until a pool of said material meltsv in said upper surface within the perimeter of said upper surface of the block whereby said block serve as a crucible for the pool of melted material, partly immersing in said pool a seed crystal of said material, and lifting the seed crystal from thepool at the rate of solidification ofthe material uplifted from the pool.

Description

Oct. 28, 1958 c. c. LARSON CRYSTAL PRODUCTION Filed Oct. 15. 1954 IN VE N TOR. CHRIS T/A N C. L A RSON BY United States Patent CRYSTAL PRODUCTION Christian Charles Larson,
Fort Wayne, Ind., assignor to International Telephone The present invention relates to crystal production, and more particularly to a method for manufacturing crystals which may be used as elements of transistors.
Conventional techniques for fabricating crystals from such materials as germanium, silicon and the like is to melt the basic material in a crucible and then touch the molten material with a seed crystal and draw the latter upwardly and away from the molten material at a sufiicient rate to continuously draw or grow a crystal. Such methods have been used successfully in the past, but are attended with considerable difiiculties in the cases where in silicon materials are used to produce the crystals.
Melted silicon in particular is of such high temperature that the usual crucibles are damaged or destroyed. No known crucible materials have yet been developed which will reliably withstand the high temperatures of molten silicon.
An object of the present invention is to provide a method for producing crystals without the need of a crucible.
It is another object of this invention to produce crystals from molten material in such a manner that the solid raw material constitutes the crucible for the molten material.
It is still a further object of this invention to utilize electron bombardment for melting a predetermined portion of a block of raw crystal material from which a finished crystal may be drawn.
Other objects will become apparent as the description proceeds.
To the accomplishment of the above and related objects, the invention may be embodied in the forms illustrated in the accompanying drawings, attention being called to the fact, however, that the drawings are illustrative only, and that specific change may be made in the specific constructions illustrated and described, so long as the scope of the appended claims is not violated.
In the drawings:
Fig. 1 is a vertical sectional elevation of an embodiment of this invention;
Fig. 2 is a top plan View thereof;
Fig. 3 is a diagrammatic illustration of an electron gun used in the apparatus of Fig. 1; and
Fig. 4 is a perspective illustration showing one step of the method of drawing a crystal.
Referring to the drawings, the apparatus comprises an evacuated bell jar 1 which is hermetically sealed to a metallic base 2. A shaft or rod 3 is reciprocably mounted in the top portion of the bell jar by means of a suitable threaded connection with a hermetically sealed coupling 4. Suitable constructions for reciprocating the rod 3 from a position outside of the bell jar 1 are wellknown to the art and in particular are described in a publication entitled Vacuum Equipment and Techniques by Guthrie and Wakerling, published by the McGraw-Hill Book Company and copyrighted in 1949.
A plurality of suitable electron guns 5 are circumferentially mounted on the top portion of the bell jar in 2,858,199 Patented Oct. 28, 1958 such a manner as to direct high density electron beams along the paths indicated by the dashed lines 6. These electron guns 5 may be of conventional construction and correspond to the electron gun arrangement disclosed in Gardner Patent 2,128,581. A suitable gun construction is diagrammatically illustrated in Fig. 3 wherein electrons emitted by a cathode 7 are concentrated into a pencil-like beam by an anode 8 and accelerated by both this anode 8 and another anode 9. As will become apparent from the following description, this pencil-like beam must be of high density.
On the base 2 of the bell jar 1 is placed a block 10 of silicon, germanium, or the like material in such position that the central portion thereof will be bombarded by the respective electron beams 6. These beams 6 are of such high density as to melt the central portion of the block 10. The beams are so controlled that only the central portion of the block is melted, whereby the block serves as a crucible for the melted portion.
A seed crystal of the type which is to be finally produced is clamped by some suitable means in the lower end of the reciprocable rod 3, and such a starter or seed crystal is indicated in Figs. 1 and 4 by the reference numeral 11. The rod 3 is lowered until the seed crystal 11 just touches the molten material, and is then withdrawn upwardly at a slow rate which will allow the molten material to continuously form on the lower end of the seed crystal. Continued withdrawal of the seed crystal thereby ostensibly draws or pulls a suitable crystal structure from the solid block. During this pulling operation, the beams 6 are trained onto the areas surrounding the drawn crystal, whereupon the operation may be continued until the block 10 is substantially consumed.
Since the block 10 acquires an electrostatic charge from the electron beams 6, it is desirable to provide a conductive return path for current fiowfrom the base 10 to one of the gun anodes, such as the anode 9. A wire 12 is shown as providing this conductive path. While there has been shown a plurality of individual electron guns 5, it is possible to utilize a single electron gun of annular configuration which will produce a tapered, hollow electron beam for melting the block 10 in the vicinity surrounding the seed crystal 11.
By performing the operation in a vacuum, impurities are prevented from entering the finished crystal. By withdrawing the crystal from the central portion of a solid block, the latter also serves as the crucible, thereby avoiding the prior art problem of preventing destruction of crucibles when materials, such as silicon, are melted.
What is claimed is:
1. The method of fabricating crystals comprising born barding a portion of a block of material from which a crystal is to be made with electrons, said bombardment serving to melt said portion, said portion being disposed in one block surface inside the perimeter thereof, and drawing a seed crystal from said melted portion, the unmelted portion of said block serving as a crucible for the melted portion.
2. The method of fabricating crystals comprising selective melting a central portion of a block of material from which a crystal is to be made, said portion being disposed in one surface between the lateral block sides, drawing a seed crystal from said melted portion, the unmelted portion of said block serving as a crucible for the melted portion, and continuing to melt said block in the perimetral vicinity of the crystal being drawn.
3. The method of fabricating crystals from a block of material from which a crystal is to be made, said method comprising positioning a self-supporting block of said material in an evacuated container focusing an electron beam on the upper surface of said block, increasing the energy in said beam until a pool of said material meltsv in said upper surface within the perimeter of said upper surface of the block whereby said block serve as a crucible for the pool of melted material, partly immersing in said pool a seed crystal of said material, and lifting the seed crystal from thepool at the rate of solidification ofthe material uplifted from the pool.
References Cited inthe file of this patent NITED STATES PATENTS Kjellgren May 3, 1949 4 Malone June 7, 1949 Sparks et al. Mar. 17. 1953 Imber July 28, 1953 Sobek Apr. 6, 1954 Little et al. July 13, 1954 FOREIGN PATENTS France Mar. 10, 1954 OTHER REFERENCES Bell Tel, Lab. Inc. and Western Electric Co. Inc., Transistor Technology, part II, chapter 7, July 1952.

Claims (1)

1. THE METHOD OF FABRICATING CRYSTALS COMPRISING BOMBARDING A PORTION OF A BLOCK OF MATERIAL FROM WHICH A CYRSTAL IS TO BE MADE WITH ELECTRONS, AND BOMBARDMENT SERVING TO MELT SAID PORTION, SAID PORTION BEING DISPOSED IN ONE BLOCK SURFACE INSIDE THE PERIMETER THEREOF, AND DRAWING A SEED CRYSTAL FROM SAID MELTED PORTION, THE UNMELTED PORTION OF SAID BLOCK SERVING AS CRUCIBLE FOR THE MELTED PORTION.
US462427A 1954-10-15 1954-10-15 Crystal production Expired - Lifetime US2858199A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
BE542056D BE542056A (en) 1954-10-15
US462427A US2858199A (en) 1954-10-15 1954-10-15 Crystal production
GB29341/55A GB778123A (en) 1954-10-15 1955-10-14 Crystal production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US462427A US2858199A (en) 1954-10-15 1954-10-15 Crystal production

Publications (1)

Publication Number Publication Date
US2858199A true US2858199A (en) 1958-10-28

Family

ID=23836385

Family Applications (1)

Application Number Title Priority Date Filing Date
US462427A Expired - Lifetime US2858199A (en) 1954-10-15 1954-10-15 Crystal production

Country Status (3)

Country Link
US (1) US2858199A (en)
BE (1) BE542056A (en)
GB (1) GB778123A (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2979386A (en) * 1956-08-02 1961-04-11 Shockley William Crystal growing apparatus
US2997760A (en) * 1957-06-10 1961-08-29 Stauffer Chemical Co Continous vaccum casting process
US3115469A (en) * 1959-06-22 1963-12-24 Monsanto Chemicals Production of single crystals of ferrites
US3160497A (en) * 1962-11-15 1964-12-08 Loung Pai Yen Method of melting refractory metals using a double heating process
DE1191054B (en) * 1962-09-08 1965-04-15 Balzers Vakuum G M B H High power electron beam device
US3219435A (en) * 1959-04-24 1965-11-23 Heraeus Gmbh W C Method and apparatus for producing metal blocks by electron beams
US3226248A (en) * 1962-03-14 1965-12-28 Texaco Experiment Inc Method of producing refractory monocrystalline boron structures
US3237254A (en) * 1962-06-26 1966-03-01 Stauffer Chemical Co Vacuum casting
US3261722A (en) * 1962-12-12 1966-07-19 Siemens Ag Process for preparing semiconductor ingots within a depression
US3278274A (en) * 1963-12-17 1966-10-11 Ibm Method of pulling monocrystalline silicon carbide
US3287107A (en) * 1960-08-22 1966-11-22 Ass Elect Ind Electron beam furnaces
US3360405A (en) * 1964-04-29 1967-12-26 Siemens Ag Apparatus and method of producing semiconductor rods by pulling the same from a melt
US3494804A (en) * 1968-07-15 1970-02-10 Air Reduction Method for growing crystals
US3634045A (en) * 1967-04-14 1972-01-11 Atomic Energy Authority Uk Growing of crystals using electron beam heating and annealize
US4602979A (en) * 1982-10-15 1986-07-29 The United States Of America As Represented By The Secretary Of The Air Force Technique for the growth of compositionally ungraded single crystals of solid solutions
US4650540A (en) * 1975-07-09 1987-03-17 Milton Stoll Methods and apparatus for producing coherent or monolithic elements

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL110575C (en) * 1958-01-17 1965-02-15 Philips Nv
US4548670A (en) * 1984-07-20 1985-10-22 Wedtech Corp. Silicon melting and evaporation method for high purity applications

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1580199A (en) * 1924-09-02 1926-04-13 Hering Carl Process of making fibrous material
US2128581A (en) * 1936-05-18 1938-08-30 Farnsworth Television Inc Fine beam electron gun
US2423729A (en) * 1939-02-22 1947-07-08 Ruhle Rudolf Vaporization of substances in a vacuum
US2468761A (en) * 1946-07-05 1949-05-03 Brush Dev Co Method of growing p-type seed crystals
US2472303A (en) * 1946-06-10 1949-06-07 Brush Dev Co Method of growing crystals
US2631356A (en) * 1953-03-17 Method of making p-n junctions
US2647043A (en) * 1948-09-23 1953-07-28 Imber Oscar Crystal growing apparatus
US2674520A (en) * 1950-04-11 1954-04-06 Clevite Corp Apparatus for growing single crystals of quartz
US2683676A (en) * 1950-01-13 1954-07-13 Bell Telephone Labor Inc Production of germanium rods having longitudinal crystal boundaries
FR1071730A (en) * 1951-09-08 1954-09-03 Licentia Gmbh Process for melting substances with a high degree of purity

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2631356A (en) * 1953-03-17 Method of making p-n junctions
US1580199A (en) * 1924-09-02 1926-04-13 Hering Carl Process of making fibrous material
US2128581A (en) * 1936-05-18 1938-08-30 Farnsworth Television Inc Fine beam electron gun
US2423729A (en) * 1939-02-22 1947-07-08 Ruhle Rudolf Vaporization of substances in a vacuum
US2472303A (en) * 1946-06-10 1949-06-07 Brush Dev Co Method of growing crystals
US2468761A (en) * 1946-07-05 1949-05-03 Brush Dev Co Method of growing p-type seed crystals
US2647043A (en) * 1948-09-23 1953-07-28 Imber Oscar Crystal growing apparatus
US2683676A (en) * 1950-01-13 1954-07-13 Bell Telephone Labor Inc Production of germanium rods having longitudinal crystal boundaries
US2674520A (en) * 1950-04-11 1954-04-06 Clevite Corp Apparatus for growing single crystals of quartz
FR1071730A (en) * 1951-09-08 1954-09-03 Licentia Gmbh Process for melting substances with a high degree of purity

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2979386A (en) * 1956-08-02 1961-04-11 Shockley William Crystal growing apparatus
US2997760A (en) * 1957-06-10 1961-08-29 Stauffer Chemical Co Continous vaccum casting process
US3219435A (en) * 1959-04-24 1965-11-23 Heraeus Gmbh W C Method and apparatus for producing metal blocks by electron beams
US3115469A (en) * 1959-06-22 1963-12-24 Monsanto Chemicals Production of single crystals of ferrites
US3287107A (en) * 1960-08-22 1966-11-22 Ass Elect Ind Electron beam furnaces
US3226248A (en) * 1962-03-14 1965-12-28 Texaco Experiment Inc Method of producing refractory monocrystalline boron structures
US3237254A (en) * 1962-06-26 1966-03-01 Stauffer Chemical Co Vacuum casting
DE1191054B (en) * 1962-09-08 1965-04-15 Balzers Vakuum G M B H High power electron beam device
US3160497A (en) * 1962-11-15 1964-12-08 Loung Pai Yen Method of melting refractory metals using a double heating process
US3261722A (en) * 1962-12-12 1966-07-19 Siemens Ag Process for preparing semiconductor ingots within a depression
US3278274A (en) * 1963-12-17 1966-10-11 Ibm Method of pulling monocrystalline silicon carbide
US3360405A (en) * 1964-04-29 1967-12-26 Siemens Ag Apparatus and method of producing semiconductor rods by pulling the same from a melt
US3634045A (en) * 1967-04-14 1972-01-11 Atomic Energy Authority Uk Growing of crystals using electron beam heating and annealize
US3494804A (en) * 1968-07-15 1970-02-10 Air Reduction Method for growing crystals
US4650540A (en) * 1975-07-09 1987-03-17 Milton Stoll Methods and apparatus for producing coherent or monolithic elements
US4602979A (en) * 1982-10-15 1986-07-29 The United States Of America As Represented By The Secretary Of The Air Force Technique for the growth of compositionally ungraded single crystals of solid solutions

Also Published As

Publication number Publication date
GB778123A (en) 1957-07-03
BE542056A (en)

Similar Documents

Publication Publication Date Title
US2858199A (en) Crystal production
US2880483A (en) Vacuum casting
US2879188A (en) Processes for making transistors
US3016313A (en) Semiconductor devices and methods of making the same
US2860251A (en) Apparatus for manufacturing semi-conductor devices
US4253221A (en) Method of producing low voltage field emission cathode structure
US2997760A (en) Continous vaccum casting process
US3087211A (en) Electron-beam furnace with opposedfield magnetic beam guidance
US2935395A (en) High vacuum metallurgical apparatus and method
US2711379A (en) Method of controlling the concentration of impurities in semi-conducting materials
US3101515A (en) Electron beam furnace with magnetically guided axial and transverse beams
GB1249537A (en) Method of growing semiconductor rods from a pedestal
US2829992A (en) Fused junction semiconductor devices and method of making same
GB1029804A (en) A process for producing a substantially monocrystalline rod of semiconductor material
US3966881A (en) Method of making a single crystal intermetallic compound semiconductor
US2250622A (en) Cathode-ray tube and method of manufacture thereof
US3015586A (en) Method of making charge storage electrodes for charge storage tubes
GB1075706A (en) Production of dislocation-free single crystals of semiconductor material
US3080626A (en) Electron-beam furnace with magnetic guidance and flux concentrator
US2229807A (en) Method of manufacturing selenium rectifiers
US6673148B2 (en) Method of using a magnetic field furnace to manufacture semiconductor substrates
US3403007A (en) Hollow cathode floating zone melter and process
US2452401A (en) Method of regeneration of electron discharge devices
US2141387A (en) Electron discharge device
US3260625A (en) Electron beam method for making contacts and p-n junctions