US3243284A - Process for collecting metal whiskers - Google Patents

Process for collecting metal whiskers Download PDF

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Publication number
US3243284A
US3243284A US325645A US32564563A US3243284A US 3243284 A US3243284 A US 3243284A US 325645 A US325645 A US 325645A US 32564563 A US32564563 A US 32564563A US 3243284 A US3243284 A US 3243284A
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US
United States
Prior art keywords
whiskers
mercury
liquid
substrate
metal
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
US325645A
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English (en)
Inventor
Charles R Morelock
Fred E Luborsky
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.)
General Electric Co
Original Assignee
General Electric Co
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 NL280327D priority Critical patent/NL280327A/xx
Priority to BE619566D priority patent/BE619566A/xx
Application filed by General Electric Co filed Critical General Electric Co
Priority to US325645A priority patent/US3243284A/en
Priority to GB44787/64A priority patent/GB1077766A/en
Priority to SE13273/64A priority patent/SE307565B/xx
Priority to NL6413355A priority patent/NL6413355A/xx
Priority to BE655927D priority patent/BE655927A/xx
Priority to CH1493764A priority patent/CH431473A/de
Priority to FR995491A priority patent/FR1418394A/fr
Application granted granted Critical
Publication of US3243284A publication Critical patent/US3243284A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/062—Fibrous particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • 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
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • 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
    • Y10S75/00—Specialized metallurgical processes, compositions for use therein, consolidated metal powder compositions, and loose metal particulate mixtures
    • Y10S75/952—Producing fibers, filaments, or whiskers

Definitions

  • This invention relates to the production of sub-micron size metal whiskers and more particularly to an improved method for collecting sub-micron sized metal whiskers from their growth substrate.
  • whiskers grown by vapor phase deposition has become increasingly important, since such whiskers are of value as reinforcing agents in making high strength composites, for example.
  • whiskers produced of magnetic materials notably iron, nickel, cobalt and alloys of these metals with each other, are of great value in producing magnets having greater coercive forces than previously attainable.
  • the whiskers are of extremely small sizes, generally less than one micron, particularly when intended for magnetic use, difficulty is encountered in removing them from the substrate on which they are grown and in collecting them for subsequent processing.
  • FIG. 1 is a schematic illustrating the manner in which whiskers are removed from their growth substrate in a bath of mercury;
  • FIG. 2 is a schematic illustrating the manner in which the whiskers are removed from the mercury into a liquid non-reactive with the whiskers
  • FIG. 3 is a schematic illustrating one method for removing the whiskers from the non-reactive liquid.
  • the process of this invention comprises immersing a growth substrate which has the metal whiskers attached thereto in mercury, vibrating the substrate, or otherwise providing for relative motion between the substrate and the mercury, to free the whiskers therefrom, adding a liquid to the mercury which is non-reactive with respect to the whiskers and then mixing the added liquid and the mercury to transport the whiskers from the mercury into the added liquid and, finally, filtering the added liquid to remove the whiskers therefrom.
  • the process of the present invention has particular application with regard to the removal of metal whiskers, and particularly metal whiskers of sub-micron size, from their growth substrate so that they might be collected for further processing and use.
  • This process generally comprises vaporizing a source metal in an enclosed, continuously evacuated chamber and depositing the vaporized metal on a growth substrate which is maintained at carefully controlled temperatures. Gettering is effected simultaneously with evacuation so that the whiskers that are produced are freer of defects than whiskers previously produced by other techniques.
  • the whiskers that are produced by the Morelock process are generally less than one micron in size and are, therefore, comparatively difficult to remove from the substrate from which they have grown. A more complete description of the process can be obtained by referring to the cited copending application.
  • FIG. 1 indicates a vessel which contains a quantity of liquid mercury 11.
  • a growth substrate such as a metal sheet 12 from which whiskers 13 extend, the whiskers being greatly enlarged for purposes of illustration, is immersed in mercury 11.
  • the growth substrate 12 is vibrated by a vibrator 15 shown attached to the upper end thereof, so that relative motion is created between the growth substrate 12, the whiskers 13 and the mercury 11.
  • This physical vibration results in an unexpectedly complete freeing of the whiskers from the substrate and their passage into the mercury bath.
  • the whiskers rise to the surface and es sentially float on the top.
  • a second liquid 16 liquid other than mercury
  • This liquid need only be non-reactive with respect to the whiskers, that is, it should neither combine chemically with the whiskers nor should it contain a component such as oxygen that will cause oxidation thereof.
  • Organic liquids are particularly useful, particularly those such as toluene, benzene and the higher aromatic hydrocarbons which can be removed without leaving any film or residue on the particles.
  • deoxygenated water or water having a small amount of dichromate for example sodium or potassium dichromate added, can also be effectively used.
  • the combination is mixed, as by means of a mixer 17, so that the whiskers contained in the mercury Will contact the interface between the two liquids and pass into the liquid 16. Agitation or mixing for a reasonable time will ensure essentially complete withdrawal of the whiskers into the lighter of the two liquids.
  • the liquid 16 then containing the whiskers 13 can be poured off or decanted into a filtering vessel 20 which contains a filter member 21 that permits passage of liquid 16 therethrough into the bottom of filter 20.
  • Filter member 21 contains holes 22 through which liquid 16 passes. Obviously, these holes 22 are extremely small, since the particles that are filtered out are less than one micron in size.
  • a filter such as a glazed ceramic filter is outstandingly useful since the surface is very smooth and the particles do not tend toward becoming imbedded.
  • the whiskers 13 In addition to not becoming imbedded, the whiskers 13 generally become commonly aligned so that where some orientation is desired it can be achieved with less difiiculty.
  • a method for removing sub-micron size metal Whiskers from their growth substrate and collecting the same comprising, immersing the substrate and attached whisker in mercury, vibrating the substrate while immersed in the mercury to free the whiskers therefrom, removing the substrate from the mercury, adding a quantity of liquid non-reactive with respect to the whiskers and to the mercury and mixing the two together to collect the whiskers in the added liquid, removing the whisker bearing added liquid from the mercury, and filtering the whiskers from the removed liquid.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Catalysts (AREA)
US325645A 1961-06-29 1963-11-22 Process for collecting metal whiskers Expired - Lifetime US3243284A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
NL280327D NL280327A (pt-PT) 1963-11-22
BE619566D BE619566A (pt-PT) 1963-11-22 1962-06-28
US325645A US3243284A (en) 1963-11-22 1963-11-22 Process for collecting metal whiskers
GB44787/64A GB1077766A (en) 1963-11-22 1964-11-03 Process for collecting metal whiskers
SE13273/64A SE307565B (pt-PT) 1963-11-22 1964-11-04
NL6413355A NL6413355A (pt-PT) 1963-11-22 1964-11-17
BE655927D BE655927A (pt-PT) 1963-11-22 1964-11-18
CH1493764A CH431473A (de) 1961-06-29 1964-11-19 Verfahren zum Züchten von Einkristallen
FR995491A FR1418394A (fr) 1963-11-22 1964-11-19 Perfectionnements aux procédés pour recueillir les trichites

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US325645A US3243284A (en) 1963-11-22 1963-11-22 Process for collecting metal whiskers

Publications (1)

Publication Number Publication Date
US3243284A true US3243284A (en) 1966-03-29

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ID=23268781

Family Applications (1)

Application Number Title Priority Date Filing Date
US325645A Expired - Lifetime US3243284A (en) 1961-06-29 1963-11-22 Process for collecting metal whiskers

Country Status (5)

Country Link
US (1) US3243284A (pt-PT)
BE (2) BE619566A (pt-PT)
GB (1) GB1077766A (pt-PT)
NL (2) NL6413355A (pt-PT)
SE (1) SE307565B (pt-PT)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4249700A (en) * 1979-07-02 1981-02-10 Exxon Research & Engineering Co. Recovery of silicon carbide whiskers from coked, converted rice hulls by liquid-liquid separation
US4256571A (en) * 1979-10-09 1981-03-17 Silag, Inc. Recovery of silicon carbide whiskers from coked, converted rice hulls by selective flocculation-liquid extraction
US4746422A (en) * 1985-07-26 1988-05-24 Rutgers University Method for the separation of a mixture of plastic and contaminant
US4808136A (en) * 1985-12-19 1989-02-28 Patent Treuhand Gesellschaft Fur Elektrische Gluhlampen Mbh Mercury retention structure for introduction of measured amounts of mercury into a lamp and method of making the retention structure

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1957819A (en) * 1930-07-19 1934-05-08 Nat Lead Co Refining metal
US2383659A (en) * 1943-03-13 1945-08-28 American Smelting Refining Method of reclaiming magnesium from scrap
US2531547A (en) * 1946-09-09 1950-11-28 Phillips Petroleum Co Apparatus for washing oils with an immiscible wash liquid
US2686592A (en) * 1949-11-18 1954-08-17 Hugo S Miller Process for separating minerals
US2923648A (en) * 1956-09-26 1960-02-02 Du Pont Di-phase cleaning system
US2974104A (en) * 1955-04-08 1961-03-07 Gen Electric High-energy magnetic material
US3113018A (en) * 1960-05-19 1963-12-03 Patrick J Young Process for cleaning contaminated mercury

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1957819A (en) * 1930-07-19 1934-05-08 Nat Lead Co Refining metal
US2383659A (en) * 1943-03-13 1945-08-28 American Smelting Refining Method of reclaiming magnesium from scrap
US2531547A (en) * 1946-09-09 1950-11-28 Phillips Petroleum Co Apparatus for washing oils with an immiscible wash liquid
US2686592A (en) * 1949-11-18 1954-08-17 Hugo S Miller Process for separating minerals
US2974104A (en) * 1955-04-08 1961-03-07 Gen Electric High-energy magnetic material
US2923648A (en) * 1956-09-26 1960-02-02 Du Pont Di-phase cleaning system
US3113018A (en) * 1960-05-19 1963-12-03 Patrick J Young Process for cleaning contaminated mercury

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4249700A (en) * 1979-07-02 1981-02-10 Exxon Research & Engineering Co. Recovery of silicon carbide whiskers from coked, converted rice hulls by liquid-liquid separation
US4256571A (en) * 1979-10-09 1981-03-17 Silag, Inc. Recovery of silicon carbide whiskers from coked, converted rice hulls by selective flocculation-liquid extraction
US4746422A (en) * 1985-07-26 1988-05-24 Rutgers University Method for the separation of a mixture of plastic and contaminant
US4808136A (en) * 1985-12-19 1989-02-28 Patent Treuhand Gesellschaft Fur Elektrische Gluhlampen Mbh Mercury retention structure for introduction of measured amounts of mercury into a lamp and method of making the retention structure

Also Published As

Publication number Publication date
NL6413355A (pt-PT) 1965-05-24
BE655927A (pt-PT) 1965-03-16
GB1077766A (en) 1967-08-02
BE619566A (pt-PT) 1962-10-15
NL280327A (pt-PT)
SE307565B (pt-PT) 1969-01-13

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