US1671213A - Process of precipitaing metals on an incandescent body - Google Patents

Process of precipitaing metals on an incandescent body Download PDF

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Publication number
US1671213A
US1671213A US94253A US9425326A US1671213A US 1671213 A US1671213 A US 1671213A US 94253 A US94253 A US 94253A US 9425326 A US9425326 A US 9425326A US 1671213 A US1671213 A US 1671213A
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United States
Prior art keywords
metals
incandescent body
precipitating
precipitaing
heated
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Expired - Lifetime
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US94253A
Inventor
Anton Eduard Van Arkel
Boer Jan Hendrik De
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Koninklijke Philips NV
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Philips Gloeilampenfabrieken NV
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    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/14—Obtaining zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
    • C23C16/14—Deposition of only one other metal element
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01K—ELECTRIC INCANDESCENT LAMPS
    • H01K3/00—Apparatus or processes adapted to the manufacture, installing, removal, or maintenance of incandescent lamps or parts thereof
    • H01K3/02—Manufacture of incandescent bodies

Definitions

  • This invention relates to a process of precipitating chemical compounds on an 1ncandescent body and refers more particularly to a process of precipitating metals of 5 the first. undergroup of the fourth column of the periodic system on such a body.
  • the process of precipitating the said metals on an incandescent body consists in heating this body in an W atmosphere containing one or more iodides of the metals to be precipitated.
  • the invention will be more clearly understood by referring to an example.
  • the figure represents perspectively by way of example an apparatus suitable for carrying out the process.
  • the apparatus consists of a vessel 1 in which a wire 2 -made, for example, of tungsten, serves as incandescent body.
  • This tungsten wire is electrically connected, for example, by small screws to leading-in wires 3 and 4 which are hermetically sealed to the narrowed upper end of the vessel.
  • the tungsten wire can be heated to the suitable temperature by an electric current.
  • the vessel is provided with a side-tube 5 which can be connected to a pump and which per-- mits to remove from the vessel 1 the air present therein or other gases having a detrimental influence during the reaction.
  • zirconium iodide is now introduced into the vessel 1 and if the latter is heated to such a temperature, that the zirconium iodide has a sufiiciently high vapour pressure, which temperature lies between about 400 and 600 (3.
  • the zirconium iodide vapour will be decomposed by heating the tungsten wire to incandescence and metallic zirconium will deposit on the wire.
  • Good results are obtained by heating the tungsten wire to a starting from hafnium iodide, the vapour which is conducted along the wire 2 which f now is heated to beyond 1600 C.
  • the filament is heated to a very high. temperature it may occur that the metal precipitated alloys with the tungsten wire, this may occur, for example, when precipitating thorium.
  • the maximal temperature to which the filament can be heated is there: fore not always determined by the melting temperature of the metal precipitated, but, if the case may be, by the melting temperature of the alloy formed.
  • the apparatus for carrying out the process should not be made of glass but of suitable metals, for example, of chrome iron.
  • a process of precipitating the metals of the first undergroup of the fourth column of the periodic system on an incandescent body characterized in that this body is heated in an-atmosphere containing at least one iodide of the metals to be precipitated.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Powder Metallurgy (AREA)

Description

May 29, 1928. 1,671,213
A. E. VAN ARKEL ET AL PROCESS OF PRECIPITATING METALS 0N ANINCANDESCENT BODY Filed March 12, 1926 Patented May 29, 1928.
UNITED ANTON EDUABD VAN ARKEL AND JAN HENDRIX DE BOER, F EINDHOVEN, NETHER- LANDS, ASSIGNORS TO N. V. PHILIPS GLOEILAMPENFABRIEKEN, OF EINDHOVEN,-
NETHERLANDS.
PROCESS OF PRECIPITATING METALS ON AN INCANDESCENT BODY.
Application filed March 12, 1926, Serial No. 94,253, and in the Netherlands March 14, 1925.
This invention relates to a process of precipitating chemical compounds on an 1ncandescent body and refers more particularly to a process of precipitating metals of 5 the first. undergroup of the fourth column of the periodic system on such a body.
According to the invention, the process of precipitating the said metals on an incandescent body consists in heating this body in an W atmosphere containing one or more iodides of the metals to be precipitated.
It has already been proposed to precipitate zirconium and titanium on a metal wire by heating the latter in an atmosphere of zirconium chloride or titanium chloride respectively and hydrogen. It has been found,
however, that it is-impossible to precipitate in this manner metallic zirconium or titanium on the metal wire. In these attempts to isolate metallic zirconium or titanium impurities of the hydrogen will presumably have given rise to the isolation of certain zirconium or titanium compounds, for example, nitrides.
Particularly favourable results are obtained with the processaccording to the invention if an incandescent body is heated in an atmosphere containing hafnium iodide so that hafnium is precipitated on said body as the temperature to which the incandescent body can be heated and which depends on the melting point of the metal to be precipitated, can be higher in the case of precipitating hafnium than when precipitating the other metals of the first undergroup o 'the 'fourth column of the periodic system,
since the melting point of hafnium-is higher than that of the other metals of the said undergroup.
The invention will be more clearly understood by referring to an example. The figure represents perspectively by way of example an apparatus suitable for carrying out the process.
The apparatus consists of a vessel 1 in which a wire 2 -made, for example, of tungsten, serves as incandescent body. This tungsten wire is electrically connected, for example, by small screws to leading-in wires 3 and 4 which are hermetically sealed to the narrowed upper end of the vessel. Thus the tungsten wire can be heated to the suitable temperature by an electric current. The vessel is provided with a side-tube 5 which can be connected to a pump and which per-- mits to remove from the vessel 1 the air present therein or other gases having a detrimental influence during the reaction. If zirconium iodide is now introduced into the vessel 1 and if the latter is heated to such a temperature, that the zirconium iodide has a sufiiciently high vapour pressure, which temperature lies between about 400 and 600 (3., the zirconium iodide vapour will be decomposed by heating the tungsten wire to incandescence and metallic zirconium will deposit on the wire. Good results are obtained by heating the tungsten wire to a starting from hafnium iodide, the vapour which is conducted along the wire 2 which f now is heated to beyond 1600 C.
If the filament is heated to a very high. temperature it may occur that the metal precipitated alloys with the tungsten wire, this may occur, for example, when precipitating thorium. The maximal temperature to which the filament can be heated, is there: fore not always determined by the melting temperature of the metal precipitated, but, if the case may be, by the melting temperature of the alloy formed.
In connection with the high temperatures to which the iodides have to be heated in order to evaporate to a sufiicient extent,--it is advisable in some cases that the apparatus for carrying out the process, should not be made of glass but of suitable metals, for example, of chrome iron.
The present application is a continuation in part of application Ser. No. 52,350, filed August 25, 1925.
What we claim is 1. A process of precipitating the metals of the first undergroup of the fourth column of the periodic system on an incandescent body, characterized in that this body is heated in an-atmosphere containing at least one iodide of the metals to be precipitated.
2. A process according to claim 1, characterized in that hafnium is precipitated on the body by heating the latter in an atmosphere of hafnium iodide. i
In testimony whereof we aflix our signatures, at the city of Eindhoven, this 17th day of February, 1926.
ANTON EDUARD VAN ARKEL. JAN HENDRIK DE BOER.
US94253A 1925-03-14 1926-03-12 Process of precipitaing metals on an incandescent body Expired - Lifetime US1671213A (en)

Applications Claiming Priority (1)

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NL29635A NL16957C (en) 1925-03-14 1925-03-14

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2522679A (en) * 1945-02-17 1950-09-19 William J Kroll Method of producing titanium alloys
US2604395A (en) * 1945-11-19 1952-07-22 Fansteel Metallurgical Corp Method of producing metallic bodies
US2694653A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694654A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694652A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2711955A (en) * 1951-10-12 1955-06-28 Jordan James Fernando Halide cracking-ingotting process
US2714564A (en) * 1948-04-12 1955-08-02 Chilean Nitrate Sales Corp Production of metallic titanium
US2717915A (en) * 1952-11-13 1955-09-13 Zalman M Shapiro Apparatus for production of purified metals
US2732292A (en) * 1956-01-24 Process of heating particulate metal
US2739566A (en) * 1953-06-24 1956-03-27 Zalman M Shapiro Apparatus for the production of coatings of purified metals
US2743173A (en) * 1945-05-28 1956-04-24 Derge Gerhard Method of preparing metal and apparatus therefor
US2768074A (en) * 1949-09-24 1956-10-23 Nat Res Corp Method of producing metals by decomposition of halides
US2785972A (en) * 1945-06-12 1957-03-19 Jr Charles H Prescott Preparation of uranium metal
US2868636A (en) * 1945-06-12 1959-01-13 Jr Charles H Prescott Process of preparing uranium metal
US3000726A (en) * 1945-11-14 1961-09-19 Frank H Speeding Production of metals
US3042494A (en) * 1955-11-02 1962-07-03 Siemens Ag Method for producing highest-purity silicon for electric semiconductor devices
US3330251A (en) * 1955-11-02 1967-07-11 Siemens Ag Apparatus for producing highest-purity silicon for electric semiconductor devices
US3419357A (en) * 1966-02-10 1968-12-31 Philips Corp Processes for manufacturing iodine of very high purity
WO2013152805A1 (en) 2012-04-13 2013-10-17 European Space Agency Method and system for production and additive manufacturing of metals and alloys

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2732292A (en) * 1956-01-24 Process of heating particulate metal
US2522679A (en) * 1945-02-17 1950-09-19 William J Kroll Method of producing titanium alloys
US2743173A (en) * 1945-05-28 1956-04-24 Derge Gerhard Method of preparing metal and apparatus therefor
US2785972A (en) * 1945-06-12 1957-03-19 Jr Charles H Prescott Preparation of uranium metal
US2868636A (en) * 1945-06-12 1959-01-13 Jr Charles H Prescott Process of preparing uranium metal
US3000726A (en) * 1945-11-14 1961-09-19 Frank H Speeding Production of metals
US2604395A (en) * 1945-11-19 1952-07-22 Fansteel Metallurgical Corp Method of producing metallic bodies
US2694653A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694654A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694652A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2714564A (en) * 1948-04-12 1955-08-02 Chilean Nitrate Sales Corp Production of metallic titanium
US2768074A (en) * 1949-09-24 1956-10-23 Nat Res Corp Method of producing metals by decomposition of halides
US2711955A (en) * 1951-10-12 1955-06-28 Jordan James Fernando Halide cracking-ingotting process
US2717915A (en) * 1952-11-13 1955-09-13 Zalman M Shapiro Apparatus for production of purified metals
US2739566A (en) * 1953-06-24 1956-03-27 Zalman M Shapiro Apparatus for the production of coatings of purified metals
US3042494A (en) * 1955-11-02 1962-07-03 Siemens Ag Method for producing highest-purity silicon for electric semiconductor devices
US3330251A (en) * 1955-11-02 1967-07-11 Siemens Ag Apparatus for producing highest-purity silicon for electric semiconductor devices
US3419357A (en) * 1966-02-10 1968-12-31 Philips Corp Processes for manufacturing iodine of very high purity
WO2013152805A1 (en) 2012-04-13 2013-10-17 European Space Agency Method and system for production and additive manufacturing of metals and alloys

Also Published As

Publication number Publication date
GB249067A (en) 1927-01-06
NL16957C (en) 1927-07-26

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