US3086850A - Method and means for growing and treating crystals - Google Patents

Method and means for growing and treating crystals Download PDF

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Publication number
US3086850A
US3086850A US820938A US82093859A US3086850A US 3086850 A US3086850 A US 3086850A US 820938 A US820938 A US 820938A US 82093859 A US82093859 A US 82093859A US 3086850 A US3086850 A US 3086850A
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Prior art keywords
seed
crystal
molten
tip
coil
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US820938A
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Jr Anthony J Marino
Donald C Seeley
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TDK Micronas GmbH
International Telephone and Telegraph Corp
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Deutsche ITT Industries GmbH
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Priority to US820938A priority Critical patent/US3086850A/en
Priority to ES0258156A priority patent/ES258156A1/es
Priority to BE591978A priority patent/BE591978A/fr
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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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
    • C30B11/08—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt every component of the crystal composition being added during the crystallisation
    • C30B11/10—Solid or liquid components, e.g. Verneuil method
    • 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
    • Y10T117/1016—Apparatus with means for treating single-crystal [e.g., heat treating]
    • 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
    • Y10T117/1028—Crucibleless apparatus having means providing movement of discrete droplets or solid particles to thin-film precursor [e.g., Verneuil method]

Definitions

  • Another object of this invention is to provide crystal growing methods and means 'which are applicable to the growth of crystals of dielectric materials.
  • Yet another object of this invention is to provide methods and means for growing crystals wherein impurities maybe introduced in solid or vapor form or wherein the constituents of the feed may be varied without interrupting the process.
  • One of the features of this invention is the method of growing crystals of a given material which is conductive at a temperature below its melting point by subjecting a seed of the given material to induction heating to render a portion of the seed molten while the remainder of the seed is in solid state, thereby inducing eddy currents in the molten portion which stir the molten portion and by dissolving additional material in said molten portion and withdrawing the seed from the zone of induction heating to control growth of the solid portion thereof.
  • Still another feature of this invention is the utilization of doping materials in particle or vapor form to change the properties of the crystal being grown.
  • FIG. 1 is a view in elevation with parts in section of apparatus according to the principles of this invention.
  • FIG. 2 is an enlarged cross-sectional view of the induction coils, field concentrator and molten tip of the crystal seed.
  • FIG. 1 there is shown a partial crosssectional view of the apparatus utilized in the practice of this invention.
  • a seed 1 of the highest purity obtainable of the material desired to be grown is mounted on and fastened to a pedestal member 2.
  • Pedestal 2 is in turn mounted on and fixed to rotatable shaft 3.
  • Shaft 3 is rotated by the action of motor 4 and beveled gears 5, one of which is coupled to shaft 3.
  • Shaft 3 is held by bearings 6, the outer races of which are coupled to a rack 7.
  • Rack 7 is capable of motion vertically upwards and downwards by the engagement of the teeth of the rack 8 with a gear 9 which is actuated by a handle or other driving member 10-.
  • shaft 3 is held by bearings 6 in fixed position relative to rack 7, but is rotatable about its own axis and is capable of being moved vertically by virtue of the combination of rack 7 and gear 9.
  • Two serially connected radio frequency coils 11 and 12, an annealing coil and a work coil, respectively, are shown disposed in juxtaposition to high purity seed 1.
  • Coils 11 and 12 are actuated by a radio frequency source and tuner 13 which delivers radio frequency energy power to coils 11 and 12 in the form of radio frequency power.
  • Coil 11 is disposed below coil 12 and is spaced from but coiled circumferentially about seed 1.
  • Work coil 12 is disposed slightly above seed 1 and is disposed internally of field concentrator element 14.
  • Field concentrator 14- is a hollow truncated cone made of copper and work coil 12 is substantially conformal with the inner surface of concentrator '14 such that it forms a helical coil tapering from a large diameter to a small diameter at a point nearest the seed.
  • Field concentrator 14 is utilized to direct or concentrate the radio frequency field in the region or zone of the tip of seed 1 to cause the tip of seed 1 to become molten due to the action of the radio frequency field known as induction heating.
  • Feld concentrator 14 has a gap 14' radially thereof to prevent the concentrator from acting as a shorted turn to prevent bum-out of the radio frequency source 13.
  • Quartz tube 15 leads from one or more reservoirs 16 through work coil 12 to a point adjacent the tip of seed 1 which is to be made molten upon the application of radio frequency energy.
  • Reservoir 16 is utilized to hold particles of the material of which a single crystal is to be made utilizing the technique of this invention. Quartz tube 15 is utilized merely as a convenience to guide the particles being dispensed from reservoir 16 to the region of the molten pool on the tip of seed 1.
  • a tapper arrangement 17 driven by motor 18 is utilized to cause the particles in reservoir 16 to be agitated at a given rate and passed through mesh 19 to the molten tip of seed 1.
  • seed 1 Upon application of radio frequency energy from source 13 to induction coils 11 and 12, seed 1 becomes molten at its tip. Seed 1 is then rotated by actuating motor 4 which, through bevel gears 5, actuates shaft 3 in a rotational manner. Motor 18 actuates tappet 17 and particles of feed material are dispensed through quartz tube 15 to the molten tip of seed 1. As the particles dissolve in the molten tip and accumulate therein, the rotation of the seed causes or permits a uniform build-up in the molten region. As the particles accumulate in the molten tip of seed 1, the seed 1 must be gradually withdrawn so that the distance d between the tip of seed 1 and the edge of field concentrator 14 is held at a substantially constant value.
  • the withdrawal of seed 1 is accomplished by actuating handle which turns gear 9 thereby gradually withdrawing shaft 3 at whatever rate is desired depending upon the rate. of accumulation of particles in the. molten tip of seed 1.
  • the annealing coil 11 maintainsthe region below the molten tip of seed 1 at a temperature just below the melting point. In this manner, sharp temperature gradients which lead to cracking of the crystal are eliminated.
  • Coils 11 and 12 are shown serially connected but they may be connected in parallel without departing from the operation of this apparatus as just described. Thus, it can be seen that a crystal may be grown continuously. and that by using two or more hoppers, as shown, various materials may be introduced into the molten pool thereby doping the crystal being grown or otherwise varying some physical or chemical property of the crystal being grown.
  • An enclosure 20 of dielectric material, designed to withstand considerable internal and external pressure is disposed about induction coils 11, 112 and seed 1 and isolated from the ambient atmosphere by O-ring seals 21, 22 which are disposed about quartz tube 15 and rotating shaft 3, respectively.
  • Input and output ports 23, 24, respectively, permit any of the various gases such as oxygen, hydrogen, argon or any mixture of gases desired to be introduced and removed from the region of seed 1 thereby providing the various atmospheres required in accordance with the teaching of this invention.
  • the leads 25, 26 of induction coils 11, 12 from radio frequency source and tuner are fed through enclosure by means of insulators 27, 28.
  • a vacuum sufficient for the needs of this invention is maintainable by virtue of seals 21 and 22 and considerable pressure may also be applied and maintained within enclosure 20 by these seals.
  • the design of heating coil 12 is varied in accordance with the type of atmosphere used. For instance, parameters such as pressure and ionization capability of the atmosphere being utilized determines the design of the coil 12.
  • seed 1 has a convex shape. This shape is due partially to the surface tension of the molten tip of the seed, to levitation by the radio frequency field but is due principally to magnetic stirring by the radio frequency energy of the molten tip of seed 1.
  • the interface between the molten tip of the seed and the seed which is in substantially solid form is shown by line aka. The shape ofthis interface is due to the manner in which the molten pool is agitated by magnetic stirring and thermal gradients within the tip of seed 1.
  • the temperature at point b is the greatest and the molten material travels away from point 12 towards points a and 0, respectively, which are cooler, along the paths X and Y.
  • points a and 0 As the material moves away from point b, material from points a and 0 moves toward point I) to take the place of the material flowing away from point b.
  • a circulation of molten material is set up which travels over path X and Y. This flow occurs in a radial direction from. point b towards the outer edge of seed 1 in the manner just described and, therefore, a section through any diametric portion of seed 1 would appear to have a flow as shown in the cross-sectional view of the present figure.
  • the field provided by work coil 12 and field concentrator 14 is shown in FIG. 2 as lines of force 29' perpendicular to the turns of coil 12 and entering into the molten tip of seed 1, as shown, to provide heating thereof so that the tip of seed 1 becomes molten.
  • the coil 12 and concentrator 14 are so designed that the lower most turn near the tip of seed 1 is in contacting relationship with the portion of field concentrator adjacent it. In this manner, the field concentrator becomes an extension or the lowermost turn of coil 12 and by properly adjusting the length of the turns of coil 12, such that the currents in the coil are all in the same direction at a given instant, the field 20 is concentrated in the tip of seed 1.
  • Quartz tube 15 is shown guiding particles of the material of which the crystal is to be formed toward the molten tip of seed 1.
  • Annealing coil 11 is shown coiled about and spaced from seed 1 and slightly below the molten tip of seed 1 to provide, by induction heating, sufficient thermal energy to the solid portion of seed 1. In this manner, a sutliciently high temperature is maintained by coil 11 to prevent cracking due to sharp thermal gradients.
  • a resistive element 31 is shown coupled about seed holder 2. This element is utilized to apply radiant energy to materials which require initiation by thermal energy to make them conductive to radio frequency energy. These materials include silicon and barium titanate, for instance. Element 31 could be any source of radiant energy such as infrared rays, ultraviolet or other forms of radiation. The showing of element 31 is not intended to be a limitation on the type of radiant energy source utilized for initiating conduction.
  • the first step is the step of preparing a given material which is conductive at a temperature below its melting point so that an area thereof is in molten phase and the remainder of the given material is in substantially solid phase.
  • the step of preparing a given material is the step of selecting a seed of a given material of the highest Purity possible which may be either a conductor, such as the elemental metals, normally non-conductive material, such as silicon which is non-conductive at room temperature and certain dielectrics such as barium titanate, which become conductive on heating or semi-conductive materials, such as germanium, which are normally conductive at room temperature.
  • step of preparing a given material is the step of either maintaining a gaseous atmosphere or maintaining a vacuum around the seed of the given material which has an area thereof in molten phase.
  • a gaseous atmosphere or maintaining a vacuum around the seed of the given material which has an area thereof in molten phase.
  • one may be required to maintain an inert, oxidizing or reducing atmosphere or mixtures of these gases, or may be required to maintain a vacuum in the region of the seed if this is a condition for growing a crystal of that particular type of material.
  • the step of preparing a seed of a given material which is normally non-conductive at room temperature includes the step of pre-heating the seed such as by irradiation with infrared, light, X- rays or radiant heat and should be applied in connection with materials such as silicon or barium titanate.
  • the final two-steps included in the step of preparing a given material in the process of growing crystals are the steps of positioning a radio frequency coil in juxtaposition to an area of the given material which is to be placed in a molten phase and the step of applying radio frequency energy by means of said coil to that area to melt that area of the given material.
  • the material to be grown be conductive, or be capable of being made conductive can now be seen.
  • the material In order to couple electromagnetic energy to a material, the material must be in an electrically conducting state. Since many materials which are normally non-conductive or, which are used as dielectric become conductive upon heating, the process of the present invention may be utilized with any material which can be made conductive at a temperature below its melting point.
  • the first main step in the process of growing crystals in accordance with the teachings of this invention is the step of subjecting the seed of given material to high frequency induction heating to render one portion of seed 1 molten while the remainder of the seed is in solid state.
  • the application of radio frequency energy to the materials which are conductive, normally non-conductive or semiconductive causes an area of one of these materials to be raised to the melting point and by maintaining the application of radio frequency energy, as from coils 11, 12 of FIGS. 1 and 2, sufiicient power is coupled by induction heating to maintain the area of the given material in molten phase.
  • the molten area is generally disposed at the tip of the seed of the given material and appears as shown in FIG. 2.
  • the second basic step in the process of growing crystals in accordance with the teachings of this invention is the step of dissolving additional material in said molten porton of said seed.
  • step of dissolving additional material in the molten portion of said seed is the step of introducing solid particles having the same composition as that of the given material.
  • solid particles having the same composition as that of the given material would be introduced into the molten area at the tip of the seed.
  • germanium in solid particle form would be introduced into the molten area of the germanium.
  • the step of adding a given quantity of a desired material to dissolve in the molten area is the step of introducing solid particles having the same composition as that of the given material and simultaneously introducing solid particles of other compositions which act to change the properties of the given material.
  • semiconductors such as germanium, for instance, well-known donor or acceptor impurities such as aluminum or arsenic in solid particle form.
  • the conductivity type of the semi-conductive material may be changed without interrupting the process.
  • the magnetic properties, the dielectric constant or the tensile and compressive properties of the given material may likewise be varied at will.
  • a step which produces the same result as the foregoing step, which is included in the step of dissolving additional material in the molten portion of the seed is the step of introducing solid particles having the same composition as that of the given material and simultaneously introducing a vapor of another composition which acts to change the properties of the given material.
  • silicon may have impurities introduced into it by introducing the gases arsine, AsH or pentaborane-9, B H
  • Other doping agents which may be utilized to vary the conductivity type of silicon are stibine, S H which produces a conductivity of the N-type and halides of boron which produce conductivity of the P-type.
  • the final basic step is the step of withdrawing the seed from the zone of induction heating to control the growth of the solid portion thereof. That is, to permit solidification in crystalline form of the molten area as the desired material accumulates in liquid form in the molten area.
  • the seed of the given material is slowly withdrawn as the material being added accumulates in liquid form in the molten area. The rate of withdrawal is adjusted so that cooling is not accomplished too rapidly and so that a portion or an area at one end of the seed of the given material is always maintained in molten condition.
  • This step includes the step of rotating the seed to prevent undesirable build up of material as the particles accumulate in the molten portion of the seed.
  • the given material which is conductive below its melting point may be a metal.
  • the metals preferably utilized in this process are those which are normally solid at room temperature and which are conductive at room temperature.
  • -metals such as hafnium, beryllium, titanium, vanadium, chromium, zirconium, tungsten or molybdenum may be utilized and either single crystals or poly-crystalline forms of these metals may be grown by the process of this invention.
  • materials which are normally non-conductive but which can be rendered electrically conducting upon heating may also be utilized.
  • Materials such as silicon, a semiconductor, and barium titanate, a dielectric, fall into the category of substances which are normally nonconductive but which become conductive by elevating their temperature from room temperature to some temperature below their melting point. The change in temperature, in many instances, is very slight as in the case of Silicon when this material is rendered conductive by the application of light.
  • a resistive element 31 as shown in FIG. 1 may be placed around a seed of the normally non-conductive material and heated to a high temperature by radio frequency induction heating. The radiation from the ring in the form of heat then raises the temperature of the material to a point'where conduction is initiated. After conduction has been initiated, the ring may be re moved and heating is continued by radio frequency means alone.
  • crystals of dielectrics such as strontium and barium titanate
  • characteristics such as permeability and dielectric constant and saturation magnetization may be varied during growth by simply varying the composition of the particles being introduced.
  • the ferrites need not have exactly the same crystal lattice structure and for this reason materials having a similar lattice structure may be introduced, thereby producing a crystal which is composed of, in one portion, a cobalt ferrite and, in another portion, a nickel ferrite.
  • the process of the present invention may also be utilized in growing alloys which have special and desirable characteristics and which, at the present time, can only be obtained with great difficulty. Materials which fall into this category are high temperature alloys of titanium and cobalt.
  • the temperature in the region of the molten area at one end of the seed of the given material should be preferably at the melting point. It is possible, however, to utilize this technique even at temperatures which are higher than the melting point.
  • the temperature may be changed in an upward direction depending on rate of growth on whether one desires to grow a single or polycrystalline form, or depending on which crystal form is desired of a material which has several crystal forms.
  • the size of the particles utilized in this process is not critical. The only criterion which should be fulfilled is that the particles be small enough to dissolve without difficulty in the molten area at the tip of the seed.
  • the length of the crystal which can be grown is theoretically unlimited because the crystal can be grown in a continuous manner.
  • the materials utilized in the growth of the crystal can be fed continuously from a source which is easily replenished and which does not require the cessation of growing to recharge with new materials in particle form.
  • the rate of withdrawal of the crystal is governed by the rate of accumulation of the melted particles in the molten area at the tip of the crystal.
  • any gaseous atmosphere may be introduced as long as the gases do not react with each other and do not contaminate the crystal being grown.
  • the oxygen-nitrogen atmosphere is utilized to maintain the chemical balance of the ferrite, that is, to make certain that on melting the ferrite does not release oxygen thereby disturbing the desired composition of the material.
  • the particle size of the ferrite material may be, for instance, less than mesh.
  • the process utilizes no crucible and because of this, -a source of contamination not easily dealt with in some prior art schemes, has been eliminated.
  • the process of the present invention requires no combustion supporting atmosphere. That is, it is a fiameless process in which solid or gaseous particles melt or dissolve in the molten area at the tip of the seed. This step may be differentiated from the prior art step wherein solid particles of a given material are actually melted in a flame and are then allowed to accumulate in molten form at the tip of a seed.
  • the steps in the process of growing a crystal of silicon inrissas the steps of irradiating a seed of silicon to initiate conduction and, further, shows the step of adding impurities to the silicon crystal by introducing impurities in vapor form.
  • the steps in growing a crystal of silicon are as follows:
  • Radiation in the form of infrared rays, gamma rays or X-rays may be utilized to initiate conduction. Any form of radiation may be used and is not limited to the examples given.
  • a vapor selected from the group consisting of arsine, stibine, pentaborane-9 aluminum trichloride and halides of boron to change the conductivity type of the silicon.
  • the amount of P-type or N-type impurity introduced can be very carefully controlled and that the number of parts per million of impurity introduced can be varied as the crystal growth progresses. Itis also possible to grow a crystal having N-type impurities and then change over to a crystan having P-type impurities while growing the crystal in a continuous manner.
  • the steps of growing a crystal of germanium are shown below. This process is very similar to that of growing a crystal of silicon with the exception that irradiation is not required to initiate conduction. In this process, the step of introducing impurities to vary the conductivity of the germanium is shown byintroducing impurities in solid particle form rather than in vapor form as was done with silicon. v
  • a doping material of a desired composition selected from the group consisting of aluminum, gallium, indium, phosphorous, arsenic and antimony in particle size.
  • hafnium which is a metal, normally conductive at room temperature.
  • This metal has been selected rather than one of the better known metals, such as cobalt or iron, to show the versatility of the process of this invention.
  • Hafnium usually presents a number of difficulties in manufacture and handling, but ,as will be seen from a consideration of the steps in the growth of a crystal of this material, it may be handled with little difiiculty utilizing the teaching of this invention.
  • the steps of the process of this invention are shown adapted to a material which is a dielectric and which falls into the general category of being normally a non-conductor.
  • the following process may be utilizedwith other dielectrics, such as strontium titanate and quartz without departing from the spirit of this invention.
  • the steps for growing a crystal of barium titanate are as follows:
  • Apparatus for growing crystals from a given material which is conductive at a temperature below its melting point and which upon solidification from a melted phase is capable of forming a crystalline structure comprising:
  • a movable pedestal disposed to extend into said enclosure along the longitudinal axis thereof;
  • a first high frequency induction heating coil having a truncated conical configuration disposed in said enclosure coaxial of said longitudinal axis having the smaller diameter thereof above and in juxtaposition to the tip of said crystal seed;
  • a field concentrator having a truncated conical configuration disposed in said enclosure concentric of and substantially coextensive with said first coil having only the smaller diameter end thereof in electrical contact with the smallest diameter turn of said first coil to concentrate the high frequency field of said first coil in the tip of said crystal seed to melt the tip of said crystal seed and leave the remainder of said crystal seed in a solid state;
  • a second high frequency induction heating coil having a substantially cylindrical configuration disposed in said enclosure coaxial of said longitudinal axis coiled about and spaced from said crystal seed below the molten tip of said crystal seed in an electromagnetic coupling relation with said crystal seed to anneal the solid portion of said seed as said seed is withdrawn from the smaller diameter of said first coil.
  • Apparatus according to claiml further including means disposed in said enclosure to irradiate said crystal seed to render said material which is normally nonconductive at room temperature conductive at a temperature below its melting point;
  • Apparatus according to claim 1, wherein said means to introduce additional material includes means to introduce particles of said material to the molten tip of said crystal seed.
  • Apparatus according to claim 1, wherein said means to withdraw includes means to rotate said crystal seed as said crystal seed is withdrawn.

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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)
US820938A 1959-06-17 1959-06-17 Method and means for growing and treating crystals Expired - Lifetime US3086850A (en)

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US820938A US3086850A (en) 1959-06-17 1959-06-17 Method and means for growing and treating crystals
ES0258156A ES258156A1 (es) 1959-06-17 1960-05-17 Un procedimiento para la formaciën y tratamiento de cristales
BE591978A BE591978A (fr) 1959-06-17 1960-06-17 Fabrication de cristaux, notamment pour les applications en électricité.

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Cited By (9)

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US3233977A (en) * 1961-05-31 1966-02-08 Westinghouse Electric Corp Furnace with means for adjusting a crucible in growing crystals
US3519394A (en) * 1965-02-10 1970-07-07 Ugine Kuhlmann Apparatus for the fabrication of a synthetic ruby
US3655415A (en) * 1968-12-31 1972-04-11 Union Carbide Corp Asteriated synthetic corundum gem stones and method and apparatus for their production
US3870472A (en) * 1969-11-26 1975-03-11 Joseph A Adamski Method and apparatus for growing crystals by annealing the crystal after formation
US4062653A (en) * 1975-09-25 1977-12-13 Siemens Aktiengesellschaft Powder flow control device for growing Verneuil crystals
US4242175A (en) * 1978-12-26 1980-12-30 Zumbrunnen Allen D Silicon refining process
US5367981A (en) * 1992-04-10 1994-11-29 Maruyama; Mitsuhiro Apparatus for manufacturing crystals through floating zone method
US20120049103A1 (en) * 2010-08-31 2012-03-01 Shirron Peter J Adr salt pill design and crystal growth process for hydrated magnetic salts
US20210222320A1 (en) * 2016-07-28 2021-07-22 Crystal Systems Corporation Method of Producing a Single-Crystal

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US2686864A (en) * 1951-01-17 1954-08-17 Westinghouse Electric Corp Magnetic levitation and heating of conductive materials
US2686865A (en) * 1951-10-20 1954-08-17 Westinghouse Electric Corp Stabilizing molten material during magnetic levitation and heating thereof
GB774270A (en) * 1952-12-17 1957-05-08 Western Electric Co Method of producing bodies of metals or matalloids
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US2686864A (en) * 1951-01-17 1954-08-17 Westinghouse Electric Corp Magnetic levitation and heating of conductive materials
DE901413C (de) * 1951-09-23 1954-03-15 August Monath Dr Ing Einrichtung zum Erschmelzen von Kristallen hochschmelzender Mineralien, insbesondere kuenstlicher Edelsteine
US2686865A (en) * 1951-10-20 1954-08-17 Westinghouse Electric Corp Stabilizing molten material during magnetic levitation and heating thereof
GB774270A (en) * 1952-12-17 1957-05-08 Western Electric Co Method of producing bodies of metals or matalloids
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US2893847A (en) * 1954-02-23 1959-07-07 Siemens Ag Apparatus for preparing rod-shaped, crystalline bodies, particularly semiconductor bodies
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US2897329A (en) * 1957-09-23 1959-07-28 Sylvania Electric Prod Zone melting apparatus

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3233977A (en) * 1961-05-31 1966-02-08 Westinghouse Electric Corp Furnace with means for adjusting a crucible in growing crystals
US3519394A (en) * 1965-02-10 1970-07-07 Ugine Kuhlmann Apparatus for the fabrication of a synthetic ruby
US3655415A (en) * 1968-12-31 1972-04-11 Union Carbide Corp Asteriated synthetic corundum gem stones and method and apparatus for their production
US3870472A (en) * 1969-11-26 1975-03-11 Joseph A Adamski Method and apparatus for growing crystals by annealing the crystal after formation
US4062653A (en) * 1975-09-25 1977-12-13 Siemens Aktiengesellschaft Powder flow control device for growing Verneuil crystals
US4242175A (en) * 1978-12-26 1980-12-30 Zumbrunnen Allen D Silicon refining process
US5367981A (en) * 1992-04-10 1994-11-29 Maruyama; Mitsuhiro Apparatus for manufacturing crystals through floating zone method
US20120049103A1 (en) * 2010-08-31 2012-03-01 Shirron Peter J Adr salt pill design and crystal growth process for hydrated magnetic salts
US8357211B2 (en) * 2010-08-31 2013-01-22 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration ADR salt pill design and crystal growth process for hydrated magnetic salts
US20210222320A1 (en) * 2016-07-28 2021-07-22 Crystal Systems Corporation Method of Producing a Single-Crystal

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ES258156A1 (es) 1960-08-16

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