US3709678A - Process for the preparation of metals or alloys - Google Patents

Process for the preparation of metals or alloys Download PDF

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Publication number
US3709678A
US3709678A US00016520A US3709678DA US3709678A US 3709678 A US3709678 A US 3709678A US 00016520 A US00016520 A US 00016520A US 3709678D A US3709678D A US 3709678DA US 3709678 A US3709678 A US 3709678A
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US
United States
Prior art keywords
vessel
reaction
preparation
metal
slag
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Expired - Lifetime
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US00016520A
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English (en)
Inventor
J Gallay
M Gallay
J Helary
La Graviere M De
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GRAVIERE M DE
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GRAVIERE M DE
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/22—Furnaces without an endless core
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/06—Dry methods smelting of sulfides or formation of mattes by carbides or the like
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0213—Obtaining thorium, uranium, or other actinides obtaining uranium by dry processes
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency
    • 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
    • Y10S75/959—Thermit-type reaction of solid materials only to yield molten metal

Definitions

  • crucible must be chemically inert with respect to the constituents which take part in the reaction;
  • the crucible in the case of highly exothermic reactions, the crucible must be constructed of a material which has high resistance to thermal shock and a high melting point;
  • the cost price of the crucible is low or that it can be used again.
  • the crucible must be leak-tight and this is a function which can often be achieved only with difficulty in the case of ceramic crucibles which are formed of a number of assembled parts.
  • the aim of this invention is to provide an improvement over the processes of the prior art, especially insofar as the practical requirements referred-to above are complied with in a more effective manner.
  • the invention proposes a process for the preparation of a metal or alloy by pyrometallurgical or metallothermic reaction in the presence of a slag, this process being characterized in that the reactants are placed in a furnace constituted by a vertical metallic vessel which is transparent to electromagnetic fields and by a winding placed around the vessel in coaxial relation thereto and intended to be supplied with highfrequency electric current, that high-frequency electric currents are induced in the reaction mass through the vessel and are of sufficient intensity to start the reaction while the vessel is cooled so as to maintain a solid layer of slag in contact therewith, that said current and said cooling are then regulated so as to maintain the reaction mass in the molten state for a sufficient period of time to cause settling of the metal or alloy and that the metal or alloy together with the slag are permitted to solidify in situ.
  • the molten reaction mass is in contact not with a different substance but with its own slag which is maintained in the solid state by the cold wall of the vessel whilst heating is carried out by Joule effect within the midst of the reactants and slag and not by heat transmission through the vessel wall. In consequence, the main causes of contamination are removed and the yield is improved.
  • the vessel can be used again a large number of times without intermediate maintenance or cleaning, which is a very appreciable advantage when the preparation process is carried out in a glove box.
  • the invention proposes a device for carrying out the process which has been outlined in the foregoing.
  • Said device comprises a vessel having a vertical axis whose side wall is constituted by tubular metal segments adapted to carry a circulation of cooling fluid and a multitum inductor coil which is coaxial with the vessel and placed around the wall, said device being especially characterized in that said side wall is delimited by an external cylindrical surface and by an internal surface which is throttled towards the base.
  • FIGURE is a very diagrammatic perspective view of the device and which is partially broken away.
  • the device which is illustrated in the FIGURE can be considered as being constituted by a vessel A provided with ancillary components and by an indicator B which is associated with a high-frequency current generator (not shown).
  • the vessel A comprises a side wall as delimited by an external cylindrical surface and by an internal surface forming a space which is throttled towards the bottom in accordance with an arrangement which is comparable with that of a conventional crucible.
  • the openings of the wall are intended to be closed by means of a base 4 and if necessary by a cover (not shown).
  • the side wall 2 is constituted by a large number of identical segments 6, each segment being delimited by a portion of the external cylindrical surface, by a portion of the internal surface, by flat top and bottom faces and by lateral faces corresponding to planes which pass through the axis of the vessel.
  • at least the lateral faces 9 are coated with a layer of insulating ceramic material which is applied by the spraygun process, for example. After assembly, the segments thus constitute a side wall which is highly permeable to the electromagnetic field.
  • the total potential difference produced by induction through the side wall is subdivided in a large number of elements (this would not be the case if provision were made for only a single slot) and there is practically no danger of breakdown resulting from discharge into the reaction mass between two adjacent segments.
  • the base 4 is constituted by a cylindrical box which is also provided with an insulating lining and shaped in such a manner as to engage in a tight fit within the bottom opening of the side wall 2 in order to prevent leakage. It is apparent that the base 4 could correspond to the side wall and thus be made up of a series of sectors which are insulated from each other.
  • the side wall 2 and the base 4 are both equipped with a cooling system.
  • Each segment 6 of the cold wall is provided with an inlet 8 for the admission of a liquid coolant at one end of the segment and with an outlet 10 for the discharge of coolant at the other end.
  • All the inlets 8 are connected by means of flexible insulating joints 12 to an admission mainfold 14.
  • all the outlets are connected to a manifold 18 by means of flexible insulating joints 16.
  • the cooling system of the base 4 is provided with an inlet 20 for the admission of liquid and with an outlet 22 for the discharge of said liquid.
  • the inductor l3 consists of a multi-turn winding 24 which is placed in proximity to the side wall 2 and coaxially with this latter.
  • the turns of said winding are fixed in position relative to each other by means of spacer members of insulating material, only one spacer member 26 being shown in the FIGURE.
  • Means are provided for maintaining the segments applied against each other throughout the duration of the reaction.
  • Said means can consist especially of a strip of insulating material which is wound tightly around the side wall. It would also be possible to clamp the top and bottom of the side wall by means of an insulating collar.
  • the base 4 having been placed in position, the reactants are intimately mixed and introduced into the vessel 2.
  • the cooling system of the side wall 2, of the base 4 and of the inductor coil is put into operation and the inductor coil B is energized. Heating is continued until start-up of the reaction.
  • the reaction will start first only in the central portion of the charge.
  • the electric power supplied to the inductor B can then be reduced to a very substantial extent and the reaction develops at a rate which can be controlled to a certain extent by regulating the power of the HF heating generator.
  • reaction mass conversion of some constituents to the liquid state frequently results in an increase in electrical conductivity of the reaction mass and this also makes it possible to reduce the intensity of the current supplied to the inductor coil.
  • the reaction takes place without any contact between the reaction mass and either the side wall or the base of the vessel since said mass remains separated from these latter by a thin layer of slag. Any contamination by the metal constituting the segments 6 (usually copper) or by the insulating product with which said segments are coated is thus prevented.
  • thermocouple is employed as a sensitive element and is immersed in the reaction mass.
  • the supply of current to the inductor coil is cut off and cooling is maintained for the period of time which is necessary to solidify the mass as constituted by an ingot surrounded by a skin of solidified slag.
  • Demolding will be carried out in some cases by removing the base and then displacing the ingot upwards, in some cases by separating the segments or in other cases by opening the wall which is designed in two disconnectable parts. Removal of the mold is facilitated by the presence of the solidified layer of slag which adheres only weakly to the metal walls of the vessel.
  • Tests have been carried out in a device comprising a highfrequency generator having a rating of 40 kVA and an output frequency of 400 kc/s.
  • the side wall of the vessel was constituted by segments having copper walls coated with alumina by the Schooping or spraygun process.
  • Quantities varying between and 600 g of uranium were employed in the tests.
  • the uranium recovered in the ingot represented between 98.6 and 99.7 percent of the uranium which was present in the tetrafluoride.
  • the weight of waste material to be recovered was limited to that of the calcium fluoride which had formed. Quantitative analysis resulted in determination of the following impurities:
  • the charges consisted of g of lanthanum and the yield was 90 percent.
  • the process and the device according to the invention are wholly suitable for the purpose of obtaining metals which are very costly, have a high degree of purity and/or by means of reactions which need not be exothermic. This is particularly the case of metals which must have a sufficient degree of purity to permit their use in nuclear reactions and of very costly metals such as plutonium and highly enriched uranium. It is also worthy of note that the invention can very readily be adapted to application in a glove box and in a controlled atmosphere and therefrom to the preparation of either toxic or radioactive metals or or alloys.
  • a process for the preparation of a metal or alloy by pyrometallurgical or metallothermic reduction of a chemical compound of said metal or alloy in the presence of a slag comprising the steps of preparing a reaction mixture from said compound and a chemical reducing agent, placing the reaction mixture in a vertical metallic vessel transparent to electromagnetic fields and in direct contact with the mixture, inducing highfrequency electric currents in said mixture through the vessel for directly heating the mixture until the metallothermic reaction starts, and simultaneously positively cooling the vessel to maintain a solid layer of slag in contact therewith, regulating said current and said cooling to maintain the reaction mass in the molten state, maintaining said current and cooling until substantially all the metal or alloy has settled and then allowing the metal or alloy together with the slag to cool and to solidify in situ.
  • a proce% according to claim 1 for the preparation of plutonium or uranium by calciothermic reduction from PuF or U1 including the step of preparing the reaction mixture by intimately mixing a powdered metal fluoride and granular calcium.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Electromagnetism (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Physics & Mathematics (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
US00016520A 1969-03-13 1970-03-04 Process for the preparation of metals or alloys Expired - Lifetime US3709678A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR6907180A FR2036418A5 (ru) 1969-03-13 1969-03-13

Publications (1)

Publication Number Publication Date
US3709678A true US3709678A (en) 1973-01-09

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Application Number Title Priority Date Filing Date
US00016520A Expired - Lifetime US3709678A (en) 1969-03-13 1970-03-04 Process for the preparation of metals or alloys

Country Status (10)

Country Link
US (1) US3709678A (ru)
BE (1) BE746865A (ru)
CH (1) CH520781A (ru)
ES (1) ES377467A1 (ru)
FR (1) FR2036418A5 (ru)
GB (1) GB1279386A (ru)
IL (1) IL33997A (ru)
LU (1) LU60473A1 (ru)
RO (1) RO61504A (ru)
SE (1) SE366064B (ru)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4252564A (en) * 1979-08-21 1981-02-24 The United States Of America As Represented By The United States Department Of Energy Method for cleaning bomb-reduced uranium derbies
US4432093A (en) * 1980-12-23 1984-02-14 SAPHYMO-STEL-Ste. d'Applications de la Physique Moderne et de l'Electronique Melting device by direct induction in a cold cage with supplementary electromagnetic confinement of the load
JPS62213682A (ja) * 1986-03-13 1987-09-19 テクノジニア　ソシエテ　アノニム 耐火材の製造方法
US4873698A (en) * 1987-10-06 1989-10-10 Commissariat A L'energie Atomique Induction furnace crucible
US5058127A (en) * 1989-05-19 1991-10-15 Compagnie Europeenne Du Zirconium Cezus Bottom discharge cold crucible
EP0467230A1 (de) * 1990-07-16 1992-01-22 Forschungszentrum Jülich Gmbh Kalt-Schmelz-Tiegel
US5257281A (en) * 1990-01-31 1993-10-26 Inductotherm Corp. Induction heating apparatus and method
US5272720A (en) * 1990-01-31 1993-12-21 Inductotherm Corp. Induction heating apparatus and method
US5283805A (en) * 1991-10-16 1994-02-01 Shinko Denki Kabushiki Kaisha Segmented cold-wall induction melting crucible
US5550353A (en) * 1990-01-31 1996-08-27 Inductotherm Corp. Induction heating coil assembly for prevent of circulating current in induction heating lines for continuous-cast products
US5668827A (en) * 1994-08-18 1997-09-16 Ald Vacuum Technologies Gmbh Crucible for induction melting
US5991328A (en) * 1996-07-23 1999-11-23 Ald Vacuum Technologies Gmbh Crucible for the inductive melting or superheating of metals, alloys, or other electrically conductive materials
US20130182740A1 (en) * 2010-09-15 2013-07-18 Korea Hydro & Nuclear Power Co., Ltd Cold crucible induction melter integrating induction coil and melting furnace
US20130223471A1 (en) * 2011-09-26 2013-08-29 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved inner surface and cold crucible induction melter having the same
US20130235896A1 (en) * 2011-09-26 2013-09-12 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved outer surface and cold crucible induction melter having the same
US20140369375A1 (en) * 2012-01-23 2014-12-18 Apple Inc. Boat and coil designs
JP2017198444A (ja) * 2017-05-08 2017-11-02 アップル インコーポレイテッド ボート及びコイルの設計
ES2648969A1 (es) * 2016-07-05 2018-01-09 Fco. Javier Porras Vila Horno industrial para fabricar metales y cerámicas de elevada dureza
US20220181076A1 (en) * 2020-12-08 2022-06-09 Ford Global Technologies, Llc Inductor temperature sensor

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3940029C2 (de) * 1989-12-04 1994-04-14 Leybold Ag Tiegel für die induktive Erwärmung

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1904664A (en) * 1929-09-14 1933-04-18 Neuhauss Heinrich Lining a furnace by freezing
US2877109A (en) * 1945-04-12 1959-03-10 Frank H Spedding Process for separating uranium fission products
US2899298A (en) * 1959-08-11 Process of producing shaped plutonium
US2899297A (en) * 1959-08-11 magel
US2977220A (en) * 1944-09-28 1961-03-28 Wood Cissie Process of producing uranium
US3549353A (en) * 1966-01-28 1970-12-22 Int Standard Electric Corp Method and apparatus for melting reactive materials

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1893992A (en) * 1929-02-05 1933-01-10 Electro Metallurg Co Production of metals and alloys by reduction
US1961621A (en) * 1929-07-19 1934-06-05 Ajax Electrothermic Corp Induction electric furnace
BE569633A (ru) * 1957-08-16
GB915693A (en) * 1959-12-08 1963-01-16 Alscope Explorations Ltd Improvements in the manufacture of alloys of refractory metals
FR1292863A (fr) * 1961-06-26 1962-05-04 Gen Electric Co Ltd Perfectionnements apportés à la fusion par induction
FR1385400A (fr) * 1963-08-29 1965-01-15 Commissariat Energie Atomique Perfectionnement au procédé d'élaboration de l'uranium métallique par calciothermie
FR1492063A (fr) * 1966-04-05 1967-08-18 Commissariat Energie Atomique Perfectionnement aux fours électriques haute fréquence pour la fabrication en continu de réfractaires électrofondus

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2899298A (en) * 1959-08-11 Process of producing shaped plutonium
US2899297A (en) * 1959-08-11 magel
US1904664A (en) * 1929-09-14 1933-04-18 Neuhauss Heinrich Lining a furnace by freezing
US2977220A (en) * 1944-09-28 1961-03-28 Wood Cissie Process of producing uranium
US2877109A (en) * 1945-04-12 1959-03-10 Frank H Spedding Process for separating uranium fission products
US3549353A (en) * 1966-01-28 1970-12-22 Int Standard Electric Corp Method and apparatus for melting reactive materials

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4252564A (en) * 1979-08-21 1981-02-24 The United States Of America As Represented By The United States Department Of Energy Method for cleaning bomb-reduced uranium derbies
US4432093A (en) * 1980-12-23 1984-02-14 SAPHYMO-STEL-Ste. d'Applications de la Physique Moderne et de l'Electronique Melting device by direct induction in a cold cage with supplementary electromagnetic confinement of the load
JPS62213682A (ja) * 1986-03-13 1987-09-19 テクノジニア　ソシエテ　アノニム 耐火材の製造方法
JP2682823B2 (ja) 1986-03-13 1997-11-26 テクノジニア ソシエテ アノニム 耐火材の製造方法
US4873698A (en) * 1987-10-06 1989-10-10 Commissariat A L'energie Atomique Induction furnace crucible
US5058127A (en) * 1989-05-19 1991-10-15 Compagnie Europeenne Du Zirconium Cezus Bottom discharge cold crucible
US5257281A (en) * 1990-01-31 1993-10-26 Inductotherm Corp. Induction heating apparatus and method
US5272720A (en) * 1990-01-31 1993-12-21 Inductotherm Corp. Induction heating apparatus and method
US5550353A (en) * 1990-01-31 1996-08-27 Inductotherm Corp. Induction heating coil assembly for prevent of circulating current in induction heating lines for continuous-cast products
EP0467230A1 (de) * 1990-07-16 1992-01-22 Forschungszentrum Jülich Gmbh Kalt-Schmelz-Tiegel
US5283805A (en) * 1991-10-16 1994-02-01 Shinko Denki Kabushiki Kaisha Segmented cold-wall induction melting crucible
US5668827A (en) * 1994-08-18 1997-09-16 Ald Vacuum Technologies Gmbh Crucible for induction melting
US5991328A (en) * 1996-07-23 1999-11-23 Ald Vacuum Technologies Gmbh Crucible for the inductive melting or superheating of metals, alloys, or other electrically conductive materials
US20130182740A1 (en) * 2010-09-15 2013-07-18 Korea Hydro & Nuclear Power Co., Ltd Cold crucible induction melter integrating induction coil and melting furnace
US9288847B2 (en) * 2010-09-15 2016-03-15 Korea Hydro & Nuclear Power Co., Ltd Cold crucible induction melter integrating induction coil and melting furnace
US9265095B2 (en) * 2011-09-26 2016-02-16 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved inner surface and cold crucible induction melter having the same
US20130223471A1 (en) * 2011-09-26 2013-08-29 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved inner surface and cold crucible induction melter having the same
US20130235896A1 (en) * 2011-09-26 2013-09-12 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved outer surface and cold crucible induction melter having the same
US9265096B2 (en) * 2011-09-26 2016-02-16 Korea Hydro & Nuclear Power Co., Ltd. Metal sector having curved outer surface and cold crucible induction melter having the same
US20140369375A1 (en) * 2012-01-23 2014-12-18 Apple Inc. Boat and coil designs
JP2015513655A (ja) * 2012-01-23 2015-05-14 アップル インコーポレイテッド ボート及びコイルの設計
CN104540618A (zh) * 2012-01-23 2015-04-22 苹果公司 舟皿和线圈设计
US9544949B2 (en) * 2012-01-23 2017-01-10 Apple Inc. Boat and coil designs
ES2648969A1 (es) * 2016-07-05 2018-01-09 Fco. Javier Porras Vila Horno industrial para fabricar metales y cerámicas de elevada dureza
JP2017198444A (ja) * 2017-05-08 2017-11-02 アップル インコーポレイテッド ボート及びコイルの設計
US20220181076A1 (en) * 2020-12-08 2022-06-09 Ford Global Technologies, Llc Inductor temperature sensor
US11915858B2 (en) * 2020-12-08 2024-02-27 Ford Global Technologies, Llc Inductor temperature sensor

Also Published As

Publication number Publication date
BE746865A (fr) 1970-08-17
CH520781A (fr) 1972-03-31
SE366064B (ru) 1974-04-08
LU60473A1 (ru) 1970-05-05
IL33997A (en) 1973-01-30
DE2011795A1 (de) 1972-02-17
RO61504A (ru) 1977-06-15
FR2036418A5 (ru) 1970-12-24
DE2011795B2 (de) 1973-01-25
IL33997A0 (en) 1970-08-19
GB1279386A (en) 1972-06-28
ES377467A1 (es) 1973-04-01

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