US3668017A - Tungsten boride-containing articles and production thereof - Google Patents

Tungsten boride-containing articles and production thereof Download PDF

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Publication number
US3668017A
US3668017A US882713A US3668017DA US3668017A US 3668017 A US3668017 A US 3668017A US 882713 A US882713 A US 882713A US 3668017D A US3668017D A US 3668017DA US 3668017 A US3668017 A US 3668017A
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US
United States
Prior art keywords
tungsten
boron
tungsten boride
boride
core
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
US882713A
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English (en)
Inventor
Daniel Paul Henri Mandineau
Michele Yvonne Christia Mourey
Georges Philippe Henri Pizzini
Jacques Constant Poulain
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.)
Safran Aircraft Engines SAS
Ecole Nationale Superieure des Mines
Original Assignee
SNECMA SAS
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.)
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Publication date
Application filed by SNECMA SAS filed Critical SNECMA SAS
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Publication of US3668017A publication Critical patent/US3668017A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00Stock material or miscellaneous articles
    • Y10S428/922Static electricity metal bleed-off metallic stock
    • Y10S428/9335Product by special process
    • Y10S428/941Solid state alloying, e.g. diffusion, to disappearance of an original layer

Definitions

  • the present invention is concerned with articles containing or consisting essentially of tungsten boride and with processes for their preparation.
  • the present invention also comprises, therefore, articles containing or consisting essentially of one or more tungsten borides in which the tungsten boride W B constitutes at least 80% of the tungsten boride content and tungsten tetraboride WB constitutes less than 15% of the tungsten boride content.
  • complex materials containing tungsten borides are usually prepared by depositing boron on a suitably heated tungsten core. As the boron is deposited on the tungsten, tungsten borides are formed leading to conversion of all or part of the tungsten and of all or part of the boron which is deposited. When the boron deposit is rather thick, a composite material is obtained comprising a core of tungsten boride which can, in the appropriate circumstances, still contain an inner core of unconverted tungsten, and an outer layer of boron. However the mechanical properties of such a composite material are better when all the tungsten is converted into tungsten boride.
  • the articles according to the invention do not contain any unconverted tungsten.
  • the outer layer of boron which may be present in the articles according to the invention, preferably consists of amorphous boron.
  • amorphous used in this specification does not imply that the boron atoms are in a non-crystalline state and entriely disorganised, but that the boron crystallites are sufficiently small for the material to appear to be amorphous when examined by X-rays.
  • the articles according to the invention are prepared by suitably controlling the conditions under which the deposi tion of the boron on a core of tungsten is effected.
  • Filamentary or threadlike articles are preferably prepared.
  • the deposition of boron arises from the thermal decomposition and the chemical reaction of a boron halide, such as boron trichloride, mixed with hydrogen.
  • the process is carried out, for example, on a 12.7 micron tungsten filament which is electrically heated by Joule effect, the ends of the filament being subject to a potential difference sufficient to heat the filament to a temperature such that amorphous boron having crystallites of well defined dimensions, is obtained.
  • the parameters of the process are as follows: (a) total gaseous mass supply, (b) mass fraction of the reactants, (c) temperature of the filament, (d) speed of transport of the filament, (e) diameter of the reactor, (f) length of the reactor, (g) sequence of the reactors, and (h) running system chosen.
  • the control of the overall tungsten boride content and of the proportion of W B and WB, in the overall tungsten boride content, in the filamentary material obtained is effected by precisely regulating the temperature and the time for which the filament is heated to a high temperature in order to effect boron deposition.
  • the starting material is a tungsten filament 12.7 microns in diameter
  • complete conversion of the tungsten into tungsten borides, of which at least is W B is obtained by heating the filament in the presence of the gaseous mixture Whose decomposition leads to boron deposition, to a temperature of from 1050 to 1150 C. for a period of about 1 minute.
  • the boron deposit changes from the amorphous state previously defined to the crystalline state, it produces a detectable electrical instability in the heating of the substrate by Joule etfect.
  • the operative can use the detection of such electrical instability to prevent this allotropic variation.
  • the electrical intensity used is suitably fixed at 3% below the experimentally determined value at which the instability phenomenon occurs with the same reactor and operating parameters.
  • the electrical intensity is preferably regulated by means of an apparatus capable of maintaining the chosen value to within better than 1%.
  • a process for the production of an article containing at least one tungsten boride which comprises the step of heating an article consisting of a core of tungsten having around said core a layer of boron to a temperature of from about 1050 to about 1150 C. under conditions as close as possible to, but not the same as those indicated by electrical instability in the heating of the tungsten, which cause the structure of the deposited boron to change from amorphous to crystalline for a time sufiicient to convert at least a part of the tungsten to tung- References Cited UNITED STATES PATENTS 3,226,248 12/1965 Talley 117-933 RALPH S. KENDALL, Primary Examiner C. WESTON, Assistant Examiner US. Cl. X.R.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Chemical Vapour Deposition (AREA)
US882713A 1968-12-10 1969-12-05 Tungsten boride-containing articles and production thereof Expired - Lifetime US3668017A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR177408 1968-12-10

Publications (1)

Publication Number Publication Date
US3668017A true US3668017A (en) 1972-06-06

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ID=8658080

Family Applications (1)

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US882713A Expired - Lifetime US3668017A (en) 1968-12-10 1969-12-05 Tungsten boride-containing articles and production thereof

Country Status (3)

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US (1) US3668017A (enrdf_load_stackoverflow)
FR (1) FR1594282A (enrdf_load_stackoverflow)
GB (1) GB1274696A (enrdf_load_stackoverflow)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4343865A (en) * 1981-06-24 1982-08-10 General Electric Company Hard metal body and method of making same
US4374901A (en) * 1981-12-21 1983-02-22 United Technologies Corporation Very fine diameter uniform wires
US4436775A (en) 1981-06-24 1984-03-13 General Electric Company Hard metal body and method of making same
WO2013022503A3 (en) * 2011-04-22 2013-05-10 The Regents Of The University Of California Compositional variations of tungsten tetraboride with transition metals and light elements
WO2017132286A1 (en) * 2016-01-25 2017-08-03 SuperMetalix, Inc. Binder compositions of tungsten tetraboride and abrasive methods thereof
CN115747820A (zh) * 2022-10-11 2023-03-07 东北电力大学 一种多孔硼化钨催化剂的制备方法及应用
US12344921B2 (en) 2017-02-06 2025-07-01 The Regents Of The University Of California Tungsten tetraboride composite matrix and uses thereof

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4407860A (en) * 1981-06-30 1983-10-04 International Business Machines Corporation Process for producing an improved quality electrolessly deposited nickel layer
NL8200903A (nl) * 1982-03-05 1983-10-03 Philips Nv Werkwijze voor het boreren van een naleveringskathode.

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4343865A (en) * 1981-06-24 1982-08-10 General Electric Company Hard metal body and method of making same
US4436775A (en) 1981-06-24 1984-03-13 General Electric Company Hard metal body and method of making same
US4374901A (en) * 1981-12-21 1983-02-22 United Technologies Corporation Very fine diameter uniform wires
WO2013022503A3 (en) * 2011-04-22 2013-05-10 The Regents Of The University Of California Compositional variations of tungsten tetraboride with transition metals and light elements
US10125412B2 (en) 2011-04-22 2018-11-13 The Regents Of The University Of California Compositional variations of tungsten tetraboride with transition metals and light elements
US10731236B2 (en) 2011-04-22 2020-08-04 The Regents Of The University Of California Compositional variations of tungsten tetraboride with transition metals and light elements
US11873544B2 (en) 2011-04-22 2024-01-16 The Regents Of The University Of California Compositional variations of tungsten tetraboride with transition metals and light elements
WO2017132286A1 (en) * 2016-01-25 2017-08-03 SuperMetalix, Inc. Binder compositions of tungsten tetraboride and abrasive methods thereof
US11033998B2 (en) 2016-01-25 2021-06-15 The Regents Of The University Of California Binder compositions of tungsten tetraboride and abrasive methods thereof
US11752593B2 (en) 2016-01-25 2023-09-12 The Regents Of The University Of California Binder compositions of tungsten tetraboride and abrasive methods thereof
US12344921B2 (en) 2017-02-06 2025-07-01 The Regents Of The University Of California Tungsten tetraboride composite matrix and uses thereof
CN115747820A (zh) * 2022-10-11 2023-03-07 东北电力大学 一种多孔硼化钨催化剂的制备方法及应用

Also Published As

Publication number Publication date
GB1274696A (en) 1972-05-17
FR1594282A (enrdf_load_stackoverflow) 1970-06-01

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