US3801309A - Production of eutectic bodies by unidirectional solidification - Google Patents

Production of eutectic bodies by unidirectional solidification Download PDF

Info

Publication number
US3801309A
US3801309A US00196448A US3801309DA US3801309A US 3801309 A US3801309 A US 3801309A US 00196448 A US00196448 A US 00196448A US 3801309D A US3801309D A US 3801309DA US 3801309 A US3801309 A US 3801309A
Authority
US
United States
Prior art keywords
film
eutectic
seed
melt
composition
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
US00196448A
Other languages
English (en)
Inventor
A Mlavsky
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.)
Saint Gobain Ceramics and Plastics Inc
Original Assignee
Tyco Laboratories Inc
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 Tyco Laboratories Inc filed Critical Tyco Laboratories Inc
Application granted granted Critical
Publication of US3801309A publication Critical patent/US3801309A/en
Assigned to INDIAN HEAD NATIONAL BANK reassignment INDIAN HEAD NATIONAL BANK SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SAPHIKON, INC.
Assigned to SAPHIKON, INC., A CORP. OF NEW HAMPSHIRE reassignment SAPHIKON, INC., A CORP. OF NEW HAMPSHIRE ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: TYCO LABORATORIES, INC., A CORP. OF MA.
Assigned to SAPHIKON, INC., A COMPANY OF NH reassignment SAPHIKON, INC., A COMPANY OF NH RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: INDIAN HEAD NATIONAL BANK
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
    • C30B21/00—Unidirectional solidification of eutectic materials
    • C30B21/06—Unidirectional solidification of eutectic materials by pulling from a melt
    • 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
    • C30B15/34—Edge-defined film-fed crystal-growth using dies or slits

Definitions

  • the primary object of this invention is to provide a new and improved method of unidirectionally solidifying eutectic compositions so as to produce bodies that are characterized by unique crystallographic relationships between the constituent phases thereof.
  • Another important object of this invention is to provide a method of producing binary eutectic compositions as duplex single crystals.
  • Still another important object is to provide a method of producing binary eutectic compositions having microstructures that consist of substantially parallel alternating lamellae of each phase or long thin parallel rods of one phase embedded in a continuous matrix of the other phase.
  • a further object is to provide eutectic compositions having unique microstructures.
  • the foregoing objects are achieved by establishing a relatively thin molten film of the eutectic composition and growing and pulling a crystalline body from the thin film while simultaneously replenishing the film by feeding thereto additional melt under the influence of surface tension.
  • the process may be conducted on a continuous basis so as to produce bodies of indefinite length and the body may be grown to a predetermined arbitrary cross-sectional configuration.
  • FIG. 1 is a vertical sectional view of one form of crucible and die arrangement for practicing the invention
  • FIG. 2 is a fragmentary view of the apparatus of FIG. 1 showing a film of melt and a seed for effecting solidification and growth of a eutectic body;
  • FIG. 3 is a vertical sectional view of a second crucible and die arrangement
  • FIG. 4 is a view similar to FIG. 1 showing a die assem bly for growing a hollow eutectic body
  • FIG. 5 is a photomicrograph of a transverse section of a eutectic body comprising UP and NaCl grown according to this invention.
  • FIG. 6 is a photomicrograph of a transverse section of a eutectic body comprising LiF and CaF grown according to this invention.
  • the present inventions utilizes the so-called EFG process previously known for growing monocrystalline bodies of materials such as alumina.
  • EFG stand for edge-defined, filmfed growth and designates a process for growing crystalline bodies from a melt.
  • the essential features of the EFG process are described in US. Pat. No. 3,591,348, issued July 6, 1971 to Harold E. LaBelle, Jr. for METHOD OF GROWING CRYSTALLINE MATERIALS.
  • the shape of the crystalline body that is produced is determined by the external or edge configuration of a horizontal end surface of a forming member which for want of a better name is called a die, although it does not function in the same manner as a die.
  • a variety of complex shapes can be produced commencing with the simplest of seed geometries, namely, a round small diameter seed crystal.
  • the process involves growth on a seed from a liquid film or film material sandwiched between the growing body and the end surface of the die, with the liquid in the film being continuously replenished from a suitable reservoir of melt via one or more capillaries in the die member.
  • the film By appropriately controlling the pulling speed of the growing body and the temperature of the liquid film, the film can be made to spread (under the influence of the surface tension at its periphery) across the full expanse of the end surface of the die until it reaches the perimeter or perimeters thereof formed by intersection of that surface with the side surface or surfaces of the die.
  • the angle of intersection of the aforesaid surfaces of the die is such relative to the contact angle of the liquid film that the liquid s surface tension will prevent it from overrunning the edge or edges of the dies end surface.
  • the angle of intersection is a right angle which is simplest to achieve and thus most practical to have.
  • the growing body grows to the shape of the film which conforms to the edge configuration of the dies end surface.
  • a substantially monocrystalline body with any one of a variety of predetermined cross-sectional configurations, e.g. bodies with circular, square or rectangular crosssection.
  • the liquid film has no way of discriminating between an outside or inside edge of the dies end surface, it is possible to grow a monocrystalline body with a continuous hole by providing in that end surface a blind hole, i.e. a cavity of the same shape as the hole desired in the growing body, provided, however, that any such blind hole is made large enough so that surface tension will not cause melt film around the hole to fill in over the hole.
  • edgedefined, film-fed growth denotes the essential feature of the EFG process the shape of the growing crystalline body is defined by the edge configuration of the die and growth takes place from a film of liquid which is constantly replenished.
  • the term coherent eutectic denotes a eutectic composition having a high order of regularity of dispersal of one phase in another.
  • Eutectic compositions produced in accordance with this invention are characterized by crystallographic properties that are substantially more uniform than eutectic bodies of the same chemical composition produced by prior art unidirectional solidification techniques.
  • eutectic compositions produced as herein described may be used, for example, as structural materials for jet engines and to produce components for electrical and electronic devices and systems.
  • THe present invention may be used to unidirectionally solidify a wide variety of eutectic compositions, including, for example, Al-Al Ni, Al-CuAl Pb-Sn, Zn- Sn, Cd-Zn, Mg-Mg Al NiSb-lnSb, and Cu-Cr eutectic alloys, nickel-base super alloys (such as those commercially designated as PWA Nos.
  • eutectic compositions including, for example, Al-Al Ni, Al-CuAl Pb-Sn, Zn- Sn, Cd-Zn, Mg-Mg Al NiSb-lnSb, and Cu-Cr eutectic alloys, nickel-base super alloys (such as those commercially designated as PWA Nos.
  • the illustrated apparatus comprises a crucible 2 for holding a reservoir supply of a melt 4 of a eutectic composition which is to be directionally solidified in accordance with this invention.
  • the crucible is made of a material that will withstand the operating temperatures and will not react with the die assembly hereinafter described and will not react with or dissolve in the melt 4.
  • the crucible is mounted within a susceptor 6 by means of a plurality of short rods 8.
  • the susceptor is made of a material that will not evolve substances that will react with the crucible and preferably is spaced from the crucible if it is madeof a material that will react with the crucible or die assembly at the operating temperatures.
  • the top end of the susceptor is open but its bottom end is closed off by an end wall 10.
  • a die assembly 14 Mounted within the crucible is a die assembly 14 that comprises a disc 16 that is locked to the crucible by a removable collar 17.
  • the disc 16 functions as a heat shield to reduce radiative heat loss from the melt and also supports a die member in the form of a cylindrical, vertically-extending solid non-porous rod 18 which is securedly mounted within a centrally located hole in the disc.
  • Rod 18 extends a short distance above the disc and its bottom end terminates short of the bottom of the crucible.
  • Rod 18 has a flat, substantially horizontal top end surface 20 and several through holes in the form of axially-extending bores 22 that are uniformly spaced about the axis of the rod and are sized to function as capillaries for the melt 4.
  • Disc 16 and rod 18 are made of a material that will not react with the crucible and will not react or dissolve in the melt. Additionally, the rod 18 is made of a material that is wetted by the melt and the diameters of capillaries 22 are such as to cause melt to rise up and fully fill them so long as the bottom end of the rod is trapped by, i.e. submersed in, the melt.
  • the apparatus of FIG. 2 is mounted in a suitable induction heating furnace (not shown) that is adapted to envelope the crucible and the growing eutectic body in an inert atmosphere and includes a pulling mechanism that is adapted to position a seed crystal as hereinafter described and to pull the seed at a controlled rate as melt solidifies on the seed.
  • a suitable induction heating furnace (not shown) that is adapted to envelope the crucible and the growing eutectic body in an inert atmosphere and includes a pulling mechanism that is adapted to position a seed crystal as hereinafter described and to pull the seed at a controlled rate as melt solidifies on the seed.
  • One form of furnace that may be used in the practice of this invention is illustrated and described in U.S. Pat. No. 3,591,348 and also U.S. Pat. No. 3,471,266, issued 10/7/69 to Harold E. LaBelle, Jr. for GROWTH OF INORGANIC FILA- MENTS.
  • the susceptor 6 is mounted within the furnace
  • the seed may be a round filament, a flat ribbon or a crystalline body of other suitable shape.
  • the seed crystal serves as a nucleating medium for the melt and may also be used to establish a film of melt in the upper surface 20 of the die assembly.
  • the seed may be a single crystal of one of the components of the eutectic composition or may be a previously solidified body of substantially the same composition as the melt. The essential requirement of the seed is that it be wetted by the melt.
  • the seed With the upper surface 20 of rod 18 at a temperature of about -40C higher than the eutectic point temperature of the melt composition in the crucible, the seed is lowered into contact with surface 20 and held there long enough for its end to melt and form a liquid film 32 that connects with the melt in the capillaries 22 (see FIG. 2).
  • the capillaries are shown empty in FlGS. l-2 in order to render them more distinct to the reader and that before the end of the seed is melted to form film 32 the melt in each capillary has a concave meniscus with the edge of the meniscus being substantially flush with the surface 20.
  • the temperature gradient along the length of the seed is one factor influencing how much of the seed melts and forms film 32.
  • the seed 26 functions as a heat sink so that its temperature is lower at successively higher points therein.
  • the thermal gradients along the seed and vertically across the film 32 are affected by the power input to the induction heating coil of the furnace and the height and distance of the heating coil and susceptor 6 relative to the seed and the die assembly. In practice these parameters are adjusted so that the film 32 is maintained at a thickness in the order of 0.2 mm during growth of desired eutectic solid.
  • the pulling mechanism is actuated so as to pull the seed vertically away from the surface 20.
  • the initial pulling speed is set so that surface tension will cause the film 32 to adhere to the seed long enough for solidification to occur due to a drop in temperature at the seed-liquid film interface.
  • This drop in temperature occurs because of movement of the seed away from surface 20, i.e., because the solid-liquid interface advances vertically to a relatively cooler region. It is to be noted that radiative and conductive heat losses from the seed cause it to exhibit a decrease in temperature with an increase in distance from the surface 20. If it is desired that the eutectic solid have a constant cross-section conforming in shape and area to surface 20, it is necessary to have the film 32 fully cover surface 20. Accordingly, if the film initially established by melting the seed does not fully cover surface 20, the pulling speed must be set so that surface tension will cause the film to spread radially out to the edge of surface 20 as solidification progresses.
  • the initial pulling speed is set at the level at which solidification will occur on the seed across the full expanse of the film. If the initial film covers less than all of the surface 20, a pulling speed is used at the beginning of the solidification process which will cause the film to spread radially, and once the surface 20 is fully covered, the pulling speed is increased to a level at which the film is maintained at a suitable thickness and solidification will occur on the seed along the full expanse of the film. It is to be noted that the pulling speed and the temperature of the film control the film thickness which also controls the rate of film spreading. Increasing the temperature of surface 20 (and hence the average temperature of film 32) and increasing the pulling speed (but short of the speed at which the seed and the growth occurring thereon will pull clear of the film) each have the effect of increasing the film thickness.
  • liquid from film 32 will solidify on the seed at all points along the full horizontal expanse of the film, with the result that additional accretions of solid will form a longer and longer solid eutectic body.
  • the liquid consumed by solidification at the interface of the growing solid and the film 32 is replaced by additional melt which is supplied to surface 20 via capillaries 22 under the influence of surface tension.
  • the rate at which fresh melt is supplied to the surface 20 is determined by the number and size of the capillaries and, within limits, is always enough to maintain the film 32.
  • the process may be continued until the solid extension on the seed has grown to a desired length or until the supply of melt in the crucible has been depleted to the point where the bottom end of the capillaries are no longer trapped, whichever event occurs first. Furthermore, the growth process may be terminated at any time by increasing the pulling speed enough to cause the growing body to pull free of the melt film. Once growth has been terminated, the furnace is shut down and the seed with its newly acquired eutectic extension is removed for inspection and use.
  • the solidification process is relatively free of perturbations of the type that produce localized depletions of one phase in the other. Such areas of localized phase depletions are known to be sources of premature failure under stress.
  • FIG. 3 relates to a preferred modification of apparatus used in practicing the invention.
  • the die assembly 14A consists of the disc 16 and a rod 18A which is secured within a centrally located hole in the disc.
  • rod 18A extends a short distance above the disc.
  • the bottom end of rod 18A extends close to and may even engage the bottom of the crucible.
  • Rod 18A has a flat substantially horizontal top surface 20 which functions to support a film of melt 32.
  • rod 18A differs from rod 18 in that it is a po rous member characterized by a myriad of small interconnected open cells sized to function as capillaries whereby melt will rise in the rod by capillary action.
  • the cells are sized so that melt will rise to the top surface 20 by capillary action so long as the level of the melt in the crucible is high enough to trap the bottom end of the rod.
  • rod 18A is made of a material that is wetted by the melt but will not react with the melt or the crucible at the operating temperatures.
  • EXAMPLE I A crucible having the general appearance of the crucible 2 ofFlG. 2 and made of nickel is mounted on rods 8 in a susceptor 6 that is mounted in a furnace in the manner shown in HO. 1 of US. Pat. No. 3,471,266.
  • the rod 8 is made of alumina and the susceptor 6 is made of molybdenum. Disposed in the crucible is a die assembly constructed generally as shown in FIG. 1.
  • rod 18 is made of nickel and has four capillaries 22 of about 0.040 inch diameter spaced uniformly about its center axis.
  • the crucible has an internal diameter of about 1 inch and an internal depth of about 1.5 inches.
  • the rod 18 has an outside diameter of about Va inch and a rod length such that its upper end projects about 1/16 inch above the crucible.
  • the crucible is filled with a solid composition comprising 23% UP and 77% NaCl by weight.
  • An elongate seed crystal 26 consisting of UP is mounted in the seed holder of the crystal pulling mechanism associated with the furnace so that it is aligned with rod 18. The seed crystal is supported in axial alignment with rod 18.
  • the induction heating coil of the furnace is located so that its upper end is approximately even with the middle of the susceptor and its lower end at least even and preferably a little below the susceptor. Then the furnace enclosure is evacuated and filled with argon gas to a pressure of about one atmosphere which is maintained during the growth period, and the induction heating coil is energized and operated so that the charge in the crucible is brought to a fully molten condition and the surface 20 is brought to a temperature of about 700C. As the charge in the crucible is converted to the melt 4. columns of melt will rise in and till the capillaries 22. Each column of melt rises until its meniscus is substantially flush with the top surface 20 of rod 18.
  • the pulling mechanism is activated and operated so that the seed 26 is moved down into contact with the upper surface 20 and allowed to rest in that position long enough (e.g. about one minute) for the bottom end of the seed to melt and form a film 32 which fully covers surface 20 and connects with the melt in the capillaries.
  • the seed is withdrawn vertically at a rate of about 0.1 inch per minute.
  • surface tension causes film material to adhere to the seed and also cause additional melt to flow out of the capillaries and add to the total volume of film.
  • the liquid film material adhering to the seed experiences a temperature drop due to its movement away from the relatively hotter surface 20 and the fact that the seed functions as a heat sink.
  • FlG. 5 is a photomicrograph of a transverse microspecimen, magnified by a factor of 940, of a eutectic body produced by practicing the invention according to the procedure of the foregoing example.
  • the eutectic body was found to be of uniform morphology throughout its entire volume.
  • the eutectic body consists of substantially uniformly sized rods spaced substantially uniformly throughout a matrix phase.
  • the rod diameters are in the order of 0.0001 inches and the spacing between rods is in the order of 0.00015 inches.
  • the rods extend parallel to the direction of solidification.
  • the rods have been found to be of indefinite length, with the result that the body is characterized by a high aspect ratio, (i.e., the ratio of rod length to rod diameter).
  • EXAMPLE I A eutectic body consisting of 56% UP and 44% CaF is produced by using the same apparatus and following the same procedures as in Example I, except that the crucible is initially charged with UP and CaF in the above proportions, the furnace is operated so as to hold the top surface 20 of the die assembly at a temperature of about 775C, and the pulling speed of the crystal is maintained at about 0.1 inch per minute.
  • FIG. 6 is a photomicrograph similar to FIG. 5 ofa microspecimen, magnified by a factor of 940, of a LiF-CaF eutectic body produced in accordance with the procedure of Example II.
  • the product is a lamellar or plate-type eutectic, the LiF phase being in the form of plates of indefinite length dispersed through a CaF matrix.
  • the LiF-NaCl eutectic it has a coherent microstructure, the two phases having an exceptionally high degree of regularity with the parallel alternate lamellae extending parallel to the direction of solidification.
  • a crucible having the general appearance of the crucible 2 of FIG. 2 and made of alumina is mounted on rods 8 in a susceptor 6 that is mounted in a furnace of the type shown in FIG. 1 of U.S. Pat. No. 3,471,266, except that the pulling mechanism is constructed in accordance with the teachings of U.S. Pat. No. 3,552,931, issued Jan. 5, 1971 to Paul R. Doherty et al., for APPARATUS FOR IMPARTING TRANSLA- TIONAL AND ROTATIONAL MOTION, so that the seed crystal (and the growth that occurs thereon) will undergo rotational motion as it is being withdrawn.
  • the rods 8 are made of alumina and the susceptor 6 is made of molybdenum.
  • Disposed in the crucible is a die assembly constructed as shown in FIG. 2A and made of an alumina foam or sponge which consists of a myriad of small interconnected open cells having an average diameter in the order of 0.0002 inch.
  • the diameter and length of rod 18A and the depth and internal diameter of the crucible are the same as specified in Example I.
  • an aluminum-nickel ingot comprising 6.2 weight per cent nickel.
  • the ingot is prepared by inductively melting substantially pure aluminum and nickel in an argon atmosphere at 900C for 1 hour to assure complete mixing, and then cooling the melt.
  • An elongate aluminum seed crystal is mounted in the seed holder of the crystal pulling mechanism associated with the furnace. Then with the induction heating coil located as described in Example I, the furnace enclosure is evacuated and filled with argon to a pressure of about one atmosphere and the heating coil is energized. The furnace temperature is raised high enough to melt the ingot and then adjusted so as to hold the temperature of the upper surface of rod 18A at about 675C. The molten liquid in the crucible infiltrates the cells of rod 18A and rises up to its top surface by action of capillary rise.
  • the crystal pulling mechanism is operated to move the aluminum seed down into contact with the upper surface of rod 18A and held there long enough for its bottom end to melt and form a thin film that extends along surface 20. Then the pulling mechanism is operated to withdraw the seed vertically at a rate of about 2 centimeters per hour while the temperature of surface 20A is held steady at about 675C. As the seed is withdrawn, liquid film material solidifies on the seed and surface tension causes additional melt to flow up rod 18A to the film on surface 20A to replace the material lost by solidification. About 10 minutes after solidification is evident on the seed, the pulling mechanism is caused to rotate the seed at a rate of about 10 degrees per hour at the same time that it is being pulled.
  • An Al-Al Ni body grown according to this example has a eutectic microstructure consisting of a lamellar micromorphology.
  • the body has substantially parallel alternating lamellae of each phase with all of the lamellae extending spirally about the bodys longitudinal axis.
  • the lamellae are coextensive and substantially free of discontinuities.
  • a rod-like eutectic microstructure i.e., a micromorphology consisting of thin parallel rods of Al Ni embedded in a continuous matrix of Al, by increasing the pulling speed (and hence the solidification rate) to about 8-10 centimeters per hour. If the seed is rotated at an appropriate speed, the parallel rods of Al Ni will also extend spirally about the growth axis. If the seed is not rotated, the lamellae and rods will extend parallel to the growth axis.
  • eutectic alloys also may be grown with a twisted structure using a pulling procedure like that of Example III. It also is possible by solidification of the film-supporting surface of the die, e. g. by providing one or more blind holes or cavities 38 as shown in FIG. 4 that are too large in diameter to function as a capillary, to grow eutectic bodies having one or more through holes extending parallel to the axis of growth. In this case it is preferred to use a seed crystal in the form of a hollow tube 40 as shown or a solid body that has a cross section with a substantially smaller area than the upper surface 20 of the rod of the die assembly 14B.
  • the initial film that is formed may cover less than all of the surface 20 and must be made to spread out around the cavity 38 so as to fully cover the surface 20; hence the initial growth of solid will not conform to the desired shape but will grow to that shape as the film spreads out over surface 20.
  • the eutectic compositions may include trace amounts of impurities or minor amounts of selected elements introduced for reasons obvious to persons skilled in the art without departing from the present invention. Accordingly, the term essentially consisting of as used herein with respect to the eutectic composition is intended to allow for such additional impurities or selected elements.
  • Eutectic bodies produced according to this invention offer a number of advantages.
  • the most important advantage is a high degree of regularity of the phases with the phases being substantially free of discontinuities.
  • the individual rods will extend for substantially the full length of the body.
  • the ability to produce a body with one or more holes avoids the problem of irregular phase termination and particle breakout such as occurs when a hole is drilled in an alloy body.
  • Growing a body so that the phases are curved about the bodys longitudinal axis is advantageous when it is desired to machine a curved part.
  • the phases By properly controlling the speed at which the body is rotated as it is being grown, it is possible to have the phases oriented so that machining transverse to the direction of the phases can be avoided when the body is being machined into a finished part of predetermined size and shape. Furthermore, since the pulling rate is consistent with the rate of growth along the pulling axis (which in turn depends upon the temperature gradient across the film from which growth occurs), it is possible by controlling the rate of heat input and the rate of heat loss by radiation and conduction to control the rate of growth within close limits and to maintain the film thickness substantially constant. Also since the film is supported by the end surface of the die and its position with respect to the height of the heater coil is held fixed, the solidliquid interface is substantially planar at all times while a eutectic body is being grown.
  • eutectic bodies with any one of a variety of arbitrary cross-sectional configurations, e.g., a body having the general crosssectional shape of an air-foil with one or more holes extending lengthwise of the body. Still other advantages, in addition to those noted above, will be obvious to persons skilled in the art.
  • Method of producing polyphase eutectic bodies of uniform morphology comprising:
  • porous surface is part of a member consisting of a myriad of interconnected open cells, and further wherein said additional quantity of said mixture is supplied to said surface via said cells.
  • Method of producing a polyphase eutectic body having a coherent microstructure comprising:
  • Method according to claim 9 further including the step of rotating said body as it is withdrawn from said film.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)
US00196448A 1971-11-08 1971-11-08 Production of eutectic bodies by unidirectional solidification Expired - Lifetime US3801309A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US19644871A 1971-11-08 1971-11-08

Publications (1)

Publication Number Publication Date
US3801309A true US3801309A (en) 1974-04-02

Family

ID=22725462

Family Applications (1)

Application Number Title Priority Date Filing Date
US00196448A Expired - Lifetime US3801309A (en) 1971-11-08 1971-11-08 Production of eutectic bodies by unidirectional solidification

Country Status (7)

Country Link
US (1) US3801309A (xx)
JP (1) JPS4857830A (xx)
CA (1) CA976765A (xx)
DE (1) DE2254615C3 (xx)
FR (1) FR2159338B1 (xx)
GB (1) GB1382528A (xx)
NL (1) NL7215041A (xx)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3868228A (en) * 1971-06-01 1975-02-25 Tyco Laboratories Inc Method of growing crystalline bodies from the melt
US3915662A (en) * 1971-05-19 1975-10-28 Tyco Laboratories Inc Method of growing mono crystalline tubular bodies from the melt
US4323418A (en) * 1978-11-10 1982-04-06 Hitachi, Ltd. Method for growing a pipe-shaped single crystal
CN105568018A (zh) * 2015-07-22 2016-05-11 重庆电子工程职业学院 一种定向凝固镁合金装置及用该装置定向凝固镁合金方法
CN109518035A (zh) * 2019-01-10 2019-03-26 江西理工大学 无带状组织的定向凝固Cu-Cr合金的制备方法和应用
US11274379B2 (en) * 2020-02-26 2022-03-15 Ii-Vi Delaware, Inc. System for growing crystal sheets
US11326273B2 (en) * 2018-05-31 2022-05-10 Kyocera Corporation Device and method for producing tubular single crystal

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2635373C2 (de) * 1975-08-08 1982-04-15 PCUK-Produits Chimiques Ugine Kuhlmann, 92400 Courbevoie, Hauts-de-Seine Verfahren und Vorrichtung zur kontinuierlichen Züchtung von Einkristallen bestimmter Form
JPS5897464A (ja) * 1981-12-02 1983-06-09 Atsumi Ono 共晶複合材の連続鋳造法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3591348A (en) * 1968-01-24 1971-07-06 Tyco Laboratories Inc Method of growing crystalline materials

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3915662A (en) * 1971-05-19 1975-10-28 Tyco Laboratories Inc Method of growing mono crystalline tubular bodies from the melt
US3868228A (en) * 1971-06-01 1975-02-25 Tyco Laboratories Inc Method of growing crystalline bodies from the melt
US4323418A (en) * 1978-11-10 1982-04-06 Hitachi, Ltd. Method for growing a pipe-shaped single crystal
CN105568018A (zh) * 2015-07-22 2016-05-11 重庆电子工程职业学院 一种定向凝固镁合金装置及用该装置定向凝固镁合金方法
US11326273B2 (en) * 2018-05-31 2022-05-10 Kyocera Corporation Device and method for producing tubular single crystal
CN109518035A (zh) * 2019-01-10 2019-03-26 江西理工大学 无带状组织的定向凝固Cu-Cr合金的制备方法和应用
US11274379B2 (en) * 2020-02-26 2022-03-15 Ii-Vi Delaware, Inc. System for growing crystal sheets
US11761119B2 (en) 2020-02-26 2023-09-19 Ii-Vi Delaware, Inc. System for growing crystal sheets

Also Published As

Publication number Publication date
GB1382528A (en) 1975-02-05
DE2254615B2 (de) 1978-11-16
FR2159338A1 (xx) 1973-06-22
DE2254615C3 (de) 1979-07-12
DE2254615A1 (de) 1973-05-10
JPS4857830A (xx) 1973-08-14
FR2159338B1 (xx) 1976-04-23
CA976765A (en) 1975-10-28
NL7215041A (xx) 1973-05-10

Similar Documents

Publication Publication Date Title
US3591348A (en) Method of growing crystalline materials
US3846082A (en) Production of crystalline bodies of complex geometries
US3650703A (en) Method and apparatus for growing inorganic filaments, ribbon from the melt
US3608050A (en) Production of single crystal sapphire by carefully controlled cooling from a melt of alumina
Pollock Filamentary sapphire: Part 1 Growth and microstructural characterisation
DE69832846T2 (de) Verfahren und Vorrichtung zur Herstellung polykristalliner Halbleiter-blöcke
US3915662A (en) Method of growing mono crystalline tubular bodies from the melt
US3857436A (en) Method and apparatus for manufacturing monocrystalline articles
US3915761A (en) Unidirectionally solidified alloy articles
US5911822A (en) Method of manufacturing silicon monocrystal, and seed crystal used in the method
US3801309A (en) Production of eutectic bodies by unidirectional solidification
GB2112309A (en) Making a cast single crystal article
US5217565A (en) Contactless heater floating zone refining and crystal growth
EP1193332B1 (en) Method for producing silicon single crystal
US3434827A (en) Anisotropic monotectic alloys and process for making the same
US3915656A (en) Apparatus for growing crystalline bodies from the melt
US3701636A (en) Crystal growing apparatus
US5114528A (en) Edge-defined contact heater apparatus and method for floating zone crystal growth
CN1051207A (zh) 制造硅单晶设备
US3826625A (en) Method and apparatus for growing crystalline bodies from the melt using a porous die member
US3853489A (en) A non-wetting aid for growing crystalline bodies
US4838988A (en) Process for obtaining crystals of intermetallic compounds, in particular isolated monocrystals, by cooling alloys in the molten state
US3261722A (en) Process for preparing semiconductor ingots within a depression
Johnston et al. The influence of acceleration forces on dendritic growth and grain structure
US3584676A (en) Method for the manufacture of single crystals

Legal Events

Date Code Title Description
AS Assignment

Owner name: INDIAN HEAD NATIONAL BANK, NEW HAMPSHIRE

Free format text: SECURITY INTEREST;ASSIGNOR:SAPHIKON, INC.;REEL/FRAME:004637/0019

Effective date: 19860530

Owner name: INDIAN HEAD NATIONAL BANK, ONE INDIAN HEAD PLAZA,

Free format text: SECURITY INTEREST;ASSIGNOR:SAPHIKON, INC.;REEL/FRAME:004637/0019

Effective date: 19860530

AS Assignment

Owner name: SAPHIKON, INC., A CORP. OF NEW HAMPSHIRE, NEW HAMP

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:TYCO LABORATORIES, INC., A CORP. OF MA.;REEL/FRAME:004634/0027

Effective date: 19860530

Owner name: SAPHIKON, INC., 51 POWERS STREET, MILFORD, NEW HAM

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:TYCO LABORATORIES, INC., A CORP. OF MA.;REEL/FRAME:004634/0027

Effective date: 19860530

AS Assignment

Owner name: SAPHIKON, INC., A COMPANY OF NH,NEW HAMPSHIRE

Free format text: RELEASED BY SECURED PARTY;ASSIGNOR:INDIAN HEAD NATIONAL BANK;REEL/FRAME:004702/0047

Effective date: 19870327

Owner name: SAPHIKON, INC., 51 POWERS STREET, MILFORD, HILLSBO

Free format text: RELEASED BY SECURED PARTY;ASSIGNOR:INDIAN HEAD NATIONAL BANK;REEL/FRAME:004702/0047

Effective date: 19870327