US3447910A - Roughened surface aluminum cylinder in zone refining - Google Patents

Roughened surface aluminum cylinder in zone refining Download PDF

Info

Publication number
US3447910A
US3447910A US497999A US3447910DA US3447910A US 3447910 A US3447910 A US 3447910A US 497999 A US497999 A US 497999A US 3447910D A US3447910D A US 3447910DA US 3447910 A US3447910 A US 3447910A
Authority
US
United States
Prior art keywords
zone
melting
wall
vacuum chamber
vacuum
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
US497999A
Other languages
English (en)
Inventor
Ludwig Sporrer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens AG
Siemens Corp
Original Assignee
Siemens Corp
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
Application filed by Siemens Corp filed Critical Siemens Corp
Application granted granted Critical
Publication of US3447910A publication Critical patent/US3447910A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28—Controlling or regulating
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
    • 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
    • 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
    • Y10T117/1076—Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone
    • Y10T117/1088—Apparatus for crystallization from liquid or supercritical state having means for producing a moving solid-liquid-solid zone including heating or cooling details

Definitions

  • My invention relates to apparatus for zone melting in vacuum.
  • Apparatus for zone melting in vacuum have already become known and comprise a vacuum chamber in which the workpiece to be processed with a melting zone is located.
  • the walls of the vacuum chamber which tend to become heated by heat radiation from the melting Zone are generally cooled by suitable means such as coolant coils. If they were not cooled there would be a great danger that impurities would emerge from the wall of the vacuum chamber and contaminate the workpiece of semiconductor material, such as silicon for example, which is being processed. Difi'lculties are consequently encountered in that material is deposited on the cooled walls of the vacuum chamber which may scale off again in solid form and cause disturbances of the growth of the monocrystals during the course of the zone-melting process.
  • I provide apparatus for zone melting in vacuum with a vacuum chamber in which the workpiece which is to be processed with a melting zone is located, the vacuum chamber being further provided with cooled walls.
  • My invention is characterized by the fact that there is located within the vacuum chamber, an inner uncooled wall, spaced a relatively great distance from the melting zone as compared to the diameter of the melting zone and spaced from the cooled wall of the vacuum chamber.
  • the side of the uncooled wall facing the melting zone has a roughened surface.
  • FIG. 1 is a longitudinal section through the vacuum chamber constructed in accordance with my invention.
  • FIG. 2 is a cross-sectional view of FIG. 1 taken along the line II-II in the direction of the arrows.
  • a housing 2 consisting for example of thick sheet steel.
  • the vacuum chamber is connected by a connecting conduit 3 with a vacuum pump (not shown) which can produce a vacuum of for example 10* to l0 torr in the vacuum chamber.
  • the apparatus shown in the figures is adapted for performing a crucible-free zone melting process.
  • this apparatus is also adapted for a zone melting process which employs an elongated boat or crucible because the same problems exist with such apparatus and can be solved in accordance with the invention of this application.
  • Apertured fittings 4 and 5 are located in the wall 2 of the vacuum chamber and maintain a vacuum seal thereof.
  • Two shafts 6 and 7 extend respectively through the fittings 4 and 5 and are provided with holders 8 and 9 respectively for supporting the rod-shaped workpiece 10 at the respective ends thereof.
  • the material of the workpiece 10 can consist for example of semiconductor material such as silicon or germanium or of a metal melting at high temperatures such as tungsten, for example.
  • a melting zone 12 is produced in the workpiece 10 with the aid of an induction heating coil 11.
  • the induction heating coil is mounted on a guide 13 extending through an apertured fitting 14 similar to fittings 4 and 5 located in the wall 2 of the vacuum chamber.
  • the guide 13 and the induction heating coil 11 supported thereon can be actuated from the outside by a movement vertically upward and downward as viewed in FIG. 1 whereby the melting zone 12 can be passed through the rod-shaped member 10 along the longitudinal axis thereof.
  • the guide 13 contains the electrical leads (not shown) to the heating coil 11 as well as a coolant loop (not shown) if desired for cooling the induction heating coil 11 which is preferably formed of tubular windings.
  • One holder 9 can be rotatably mounted for example whereas the other holder 8 can be mounted on a shaft 6 which is displaceable vertically upward and downward as shown by the double-headed arrow in FIG. 1, whereby variations in the diameter of the workpiece being processed can be equalized or compensated, or the diameter of this workpiece can be varied.
  • a very large opening is provided through which necessary manipulations can be carried out within the vacuum vessel.
  • the opening is closed by a door 15 which can also be formed of steel.
  • the door 15 is advantageously mounted at one edge on hinges 15.
  • the door 15 is automatically kept closed by pressure thereof against the seals 16 and 17 due to the pressure differential between the vacuum within the vacuum chamber and the ambient air pressure on the outside thereof.
  • An opening is also provided in the door 15 which is vacuum-tightly closed by a viewing window 18 which can consist for example of glass or quartz glass and more specifically and advantageously of so-called bullet-proof glass.
  • an additional transparent pane for example of a transparent plastic material can be located in front of i.e. to the left-hand side of the viewing window pane 18 as viewed in the figures, which protects against flying fragments of the glass pane 18 in the event of an implosion.
  • the aforedescribed difliculties of the material vaporizing from the melting zone occurs in the course of carrying out the zone-melting process in vacuum, especially the crucible-free zone-melting process.
  • the cooling of the walls of the vacuum chamber at least by means of the outer air and if necessary, however, by an additionally mounted cooling fan, or by means of cooling coils which are soldered or welded to the walls and are traversed by coolant liquid, is absolutely necessary and cannot be avoided because otherwise the seals necessary for the production of a high vacuum cannot remain secure if temperature variations were to occur.
  • the solution in accordance with my invention is to provide a second and inner uncooled wall which is located within the vacuum vessel, out of engagement with the cooled wall and surrounding the melting zone at a relatively great distance therefrom.
  • This inner wall can for example be heated by radiation heating from the melting zone to a small extent whereby danger of scaling oil? is markedly reduced.
  • the side of this uncooled wall which faces the melting zone can be provided with a roughtened surface which additionally prevents scaling off of the deposited material.
  • this additionally installed wall can, if necessary, be shaped so that it is easily removable and replaceable by a new clean wall during any pause or lull in the zone-melting operation.
  • the additional uncooled wall 20 consists of a cylindrically bent or curved metal sheet.
  • a wide slot is formed in the cylindrical sheet facing the door 15 so that the movement of the melting zone can be observed therethrough.
  • Practically all metals can be used as the material for the wall 20 and if desired also other materials such as for example quartz, ceramic or graphite can also be used therefor.
  • Aluminum is preferably employed because the surface of this material can be roughened relatively easily by sand blasting and, after such roughening, has a surface so formed as to prevent flaking off of material deposited thereon better than for other metals or the aforementioned other materials.
  • the wall 20 can be held in place within the vacuum chamber by spacer members 21 and 22 consisting for example of ceramic.
  • the wall 20 is expediently located with such great clearance from the melting zone 10 that for example a coupling of the wall 20, when consisting of metal, to the magnetic field of the induction heating coil 11, can be safely avoided.
  • cover members 23 and 24, complementing the cylindrical wall 20 at the top and bottom thereof as shown in FIG. 1, can also be provided in addition. Attention must be given, however, to the fact that sufficiently large clearances and sufiiciently large openings are provided so that necessarily free pathways are thereby afforded for producing a high vacuum.
  • Device for zone-melting a workpiece in vacuum comprising a vacuum chamber wherein the workpiece and heating means for forming a melting zone in the workpiece are located, said vacuum chamber being defined by cooled walls, and a secondary uncooled wall mounted in the interior of said vacuum chamber spaced from the cooled walls thereof and located at a relatively great distance from the melting zone when compared to the diameter of the melting zone, said secondary uncooled wall consisting of aluminum and having a roughened surface facing the melting zone.
  • Device according to claim 3 including a cover member located at the ends of said uncooled cylindrical wall.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Furnace Details (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
US497999A 1965-02-27 1965-10-19 Roughened surface aluminum cylinder in zone refining Expired - Lifetime US3447910A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES0095711 1965-02-27

Publications (1)

Publication Number Publication Date
US3447910A true US3447910A (en) 1969-06-03

Family

ID=7519569

Family Applications (1)

Application Number Title Priority Date Filing Date
US497999A Expired - Lifetime US3447910A (en) 1965-02-27 1965-10-19 Roughened surface aluminum cylinder in zone refining

Country Status (6)

Country Link
US (1) US3447910A (enrdf_load_stackoverflow)
JP (1) JPS4822562B1 (enrdf_load_stackoverflow)
BE (1) BE676974A (enrdf_load_stackoverflow)
CH (1) CH431472A (enrdf_load_stackoverflow)
DE (1) DE1519867A1 (enrdf_load_stackoverflow)
GB (1) GB1120554A (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090025415A1 (en) * 2007-07-24 2009-01-29 Hsin-Wen Kung Device and method for vacuum-sealing a cooling medium
CN102925962A (zh) * 2012-11-06 2013-02-13 浙江晶盛机电股份有限公司 一种用于正压晶体生长炉的操作及观察窗口
CN113648933A (zh) * 2021-08-07 2021-11-16 北京双吉制药有限公司 一种膏剂生产用液化装置

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2890139A (en) * 1956-12-10 1959-06-09 Shockley William Semi-conductive material purification method and apparatus
US2904512A (en) * 1956-07-02 1959-09-15 Gen Electric Growth of uniform composition semiconductor crystals
US2912321A (en) * 1956-09-04 1959-11-10 Helen E Brennan Continuous casting and refining of material
US3173765A (en) * 1955-03-18 1965-03-16 Itt Method of making crystalline silicon semiconductor material
US3211881A (en) * 1962-08-28 1965-10-12 Westinghouse Electric Corp Apparatus for zone heating
US3261671A (en) * 1963-11-29 1966-07-19 Philips Corp Device for treating semi-conductor materials by melting
US3282654A (en) * 1964-05-18 1966-11-01 Union Carbide Corp Crystal growing furnace with an alumina liner

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3173765A (en) * 1955-03-18 1965-03-16 Itt Method of making crystalline silicon semiconductor material
US2904512A (en) * 1956-07-02 1959-09-15 Gen Electric Growth of uniform composition semiconductor crystals
US2912321A (en) * 1956-09-04 1959-11-10 Helen E Brennan Continuous casting and refining of material
US2890139A (en) * 1956-12-10 1959-06-09 Shockley William Semi-conductive material purification method and apparatus
US3211881A (en) * 1962-08-28 1965-10-12 Westinghouse Electric Corp Apparatus for zone heating
US3261671A (en) * 1963-11-29 1966-07-19 Philips Corp Device for treating semi-conductor materials by melting
US3282654A (en) * 1964-05-18 1966-11-01 Union Carbide Corp Crystal growing furnace with an alumina liner

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090025415A1 (en) * 2007-07-24 2009-01-29 Hsin-Wen Kung Device and method for vacuum-sealing a cooling medium
US7866178B2 (en) * 2007-07-24 2011-01-11 Asia Vital Components Co., Ltd. Device and method for vacuum-sealing a cooling medium
CN102925962A (zh) * 2012-11-06 2013-02-13 浙江晶盛机电股份有限公司 一种用于正压晶体生长炉的操作及观察窗口
CN102925962B (zh) * 2012-11-06 2015-05-20 浙江晶盛机电股份有限公司 一种用于正压晶体生长炉的操作及观察窗口
CN113648933A (zh) * 2021-08-07 2021-11-16 北京双吉制药有限公司 一种膏剂生产用液化装置

Also Published As

Publication number Publication date
GB1120554A (en) 1968-07-17
JPS4822562B1 (enrdf_load_stackoverflow) 1973-07-06
CH431472A (de) 1967-03-15
DE1519867A1 (de) 1970-02-26
BE676974A (enrdf_load_stackoverflow) 1966-08-24

Similar Documents

Publication Publication Date Title
US3265469A (en) Crystal growing apparatus
US6632280B2 (en) Apparatus for growing single crystal, method for producing single crystal utilizing the apparatus and single crystal
US4650540A (en) Methods and apparatus for producing coherent or monolithic elements
EP0591525A1 (en) Device for pulling up single crystal
EP0581496A2 (en) Molecular beam epitaxy (MBE) effusion source utilizing heaters to achieve temperature gradients
US3716345A (en) Czochralski crystallization of gallium arsenide using a boron oxide sealed device
US3798007A (en) Method and apparatus for producing large diameter monocrystals
US3031275A (en) Process for growing single crystals
US11821104B2 (en) Apparatus for manufacturing single crystal
US3051555A (en) Crucible for melting silicon of highest purity and method of making it
US3447910A (en) Roughened surface aluminum cylinder in zone refining
US3226203A (en) Apparatus for preparing semiconductor rods
US3492969A (en) Apparatus for indiffusing impurity in semiconductor members
US3235339A (en) Device for floating zone melting
US3189415A (en) Device for crucible-free zone melting
US3481711A (en) Crystal growth apparatus
US4784715A (en) Methods and apparatus for producing coherent or monolithic elements
Sworn et al. The growth of dislocation-free copper crystals
US3819421A (en) Method for the manufacture of dislocation-free, single-crystal gallium arsenide rod
US3503717A (en) Crystallization at high pressure to prevent self diffusion of materials
Gerk Growth of tungsten carbide monocrystals
JP3220542B2 (ja) 半導体単結晶棒製造装置
US3296036A (en) Apparatus and method of producing semiconductor rods by pulling the same from a melt
GB2047113A (en) Method for producing gadolium gallium garnet
US3242015A (en) Apparatus and method for producing single crystal structures