WO1981000977A1 - Process for producing dispersion strengthened precious metal alloys - Google Patents

Process for producing dispersion strengthened precious metal alloys Download PDF

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Publication number
WO1981000977A1
WO1981000977A1 PCT/US1980/001061 US8001061W WO8100977A1 WO 1981000977 A1 WO1981000977 A1 WO 1981000977A1 US 8001061 W US8001061 W US 8001061W WO 8100977 A1 WO8100977 A1 WO 8100977A1
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WO
WIPO (PCT)
Prior art keywords
process according
precious metal
yttria
powder
ranging
Prior art date
Application number
PCT/US1980/001061
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English (en)
French (fr)
Inventor
F Roehrig
Original Assignee
Owens Corning Fiberglass Corp
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 Owens Corning Fiberglass Corp filed Critical Owens Corning Fiberglass Corp
Publication of WO1981000977A1 publication Critical patent/WO1981000977A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0021—Matrix based on noble metals, Cu or alloys thereof

Definitions

  • This invention relates to a process for producing dispersion strengthened precious metal alloys.
  • the present invention can provide alloys containing platinum, palladium, rhodium and gold which are useful in the production of glass fibers.
  • the present invention provides a process for producing dispersion-strengthened precious metal alloys having creep resistance superior to known dispersi on- strengthened platinum alloys.
  • precious metal pov.der end cisp ⁇ rsoids ere mechanically alloyed together.
  • the mechanical alloying uses a high energy ball mill to achieve the intimate mechanical mixing of this process.
  • the oxide particles are forged into the precious metal matrix powder particle to form a composite povider particle.
  • FIG. 1 illustrates the internal arrangement in an attritor mill showing the impeller, grinding media and external cooling jacket. Impact events occur in the dynamic interstices of the media created by the impeller during stirring.
  • FIG. I shows an overall view of the attritor mill .
  • the stainless steel bearings or grinding media and the powder charge go into the cylin ⁇ rical container of the mill .
  • the high-energy impacts are effected by the rotating impeller.
  • FIG. 1 also illustrates the internal arrangement in the attritor mill, impact events occur in the dynamic interstices of the media created by the impeller during stirring.
  • Dispersion strengthened precious metals are known in the art and are commercially available.
  • One such material is that available from Johnson, Matt hey & Co. Limited, under their designation ZGS.
  • the above indicated ZGS material consists essentially of platinum in which the disperoid is zirconia; the latter is present in an amount of about 0.5% by volume.
  • the dispersion strengthened precious metals of this invention generally comprise a precious metal, or precious metal alloy, preferably platinum, as the dispersing medium, or matrix, and a disperse id of a metal oxide, metal carbide, metal suicide, metal nitride, metal sulfic'a or a metal boride which dispersoid is present in effective dispersion strengthening amounts. Usually such amounts will be between about C.l percent to about 5.0 percent by volume. Preferably the dispersoid will be an oxide.
  • metal compounds which may be employed as the dispersoid are compounds of metals of Group IIA, IIIA, 111 B (including non-hazardous metals of the Actinide and Lanthanide classes), I VB , VS , VI B and VI IB. More specifically exemplary of suitable metals a r e the following: Be, Hg, Ca, Ba, Y, La, Ti , Zr, Hf, Mo, W, Ce, Nd , Gd , and Th as well as Al .
  • VHP vacuum hot pressing
  • the samples can be consolidated by first coIo pressing at elevated pressures followed by sintering at elevated temperatures.
  • VHP generally is carried out at a temperature ranging from 1300 to 1700°C under a pressure ranging from 500 to 10,000 psi for a time ranging from 10 to 30 minutes.
  • the temperature ranges from 1400 to 1500°C under a pressure of 3,000 to 6,000 psi for a time of 15 to 25 minutes.
  • the cold pressing is carried cut at a pressure ranging from 2,000 to 10,000 psi for up to 5 minutes followed by sintering at a temperature ranging from 1200 to 1700°C for 2 to 6 hours.
  • yttria Approximately one kgm of -325 mesh (-44 micron) platinum sponge from Engl ⁇ hard was blended with an amount of yttria (Y 2 O 3 ) to give nominally 0.65 volume percent (0.15 weight percent) oxide loading in the final compact.
  • the yttria was 200-600 angstrom in size.
  • the platinum matrix starting powder for the experiment consisted of ⁇ / ery fine, near spherical particles or chained aggregates. Most of the particles below 2 microns appeared to be single crystals. Tne starting powder had a fairly high specific surface area.
  • the powder mixture was charged into the container of the attritor mill while it was running.
  • the grinding media had been previously loaded to give a volume ratio of media to powder of about 20:1.
  • the grinding media useo was s hardened 400 series stainless steel bearing nominally 3/8 inch (0.953 cm) diameter.
  • the impeller rotational speed was selected at 130 rpm .
  • Samples of powder were removed at various times to obtain information on the changes in particle morphology and specific surface area with milling time.
  • the first sample was taken after one hour of milling and indicated that flake generation was in progress.
  • the iron contamination in the milled powder was greatly reduced compared to the previous experiments and reflects the coating action that appeared to minimize wear debris generation curing milling.
  • the maximum iron contamination level in the powder was approximately 300 wppm.
  • the milled powder was consolidated by vacuum hot pressing and thermomechanically processing into sheet for creep testing, the details are to follow.
  • Example I produced a powder of relatively low iron contamination. Since this experiment resulted in small powder lots (nominally 20 gms) taken at various times during the milling experiment, each sample was individually consolidated by vacuum hot pressing (VHP) at 1,450°C under 5,G0C psi (34.5 MN/m 2 ) for twenty minutes. The resultant compacts were nominally 1 inch (2.54 cm) in diameter.
  • VHP vacuum hot pressing
  • thermomechanical processing (TMP) scheduled used on the compact consisted of several roll/anneal cycles.
  • the basic operation involved rolling a sheet specimen and cropping pieces after various rolling passes for microstructural characterization.
  • the procedure used was to roll the compact for a 10 percent reduction in area then anneal the rolled specimen for five minutes at nominally 1,040°C before further rolling.
  • Specimen D was the most responsive to the TMP cycles.
  • the grain structure was fairly elongated.
  • the lack of oxide clusters during optical metal 1 ographi c examination suggested that the milling action had worked the yttria into the platinum matrix.
  • a metallogrephic analysis of the same region showed the development of a moderate grain aspect ratio (grain length to thickness ratio in the viewing plane) , As the number of roll/anneal cycles increased, the grain aspect ratio (GAR) increased. At this stage a moderate GAR also h ⁇ been developed in a transverse direction. The significance of this observation is that the grains took on the shape of a pancake structure thin in a direction perpendicular to the sheet yet extended in the other two directions. Since a GAR seems to extend in two directions in the rolled sheet and the state of stress in a bushing tip plate is biaxial, this transverse GAR development may be v ery beneficial for good creep resistance in bushing applications.
  • the creep testing was cone in air using constant load machines, the elongation was measured by an LVDT connected to a multi-point recorder and a precision digital voltmeter. Specimen temperature was monitored with a calibrated Pt/Pt-Rh thermocouple attached so that the bead was adjacent to the g ⁇ ge section of the creep specimen.
  • the creep specimen was a flat plate type with a gage length of approximately 2.25 inch (5.72 cm) .
  • the tensile stress was applied parallel to the rolling direction (longitudinal direction) .
  • the general procedure was to hang the specimen in the furance to reach thermal equilibrium then start the rig timer upon application of the load. Periodic temperature and extension measurements were made either until the specimen failed or the test was terminated (specimen removal or furnace burn-out).
  • Creep results were obtained from specimens that we r e processed according to Example II except that these specimens were milled 10 hours and received the above thermomechani cal processing treatment of 10% reduction in area per pass with an intermediate anneal at nominally 1040°C for 5 minutes. The extent of deformation was nominally an 85% reduction in area.
  • the first specimen had a varied creep history that started by applying a tensile stress of 1,000 psi (6.89 Mn/m 2 ) at 2,400°F (1,316°C) .
  • the resultant secondary creep rate was toe lew to adequately measure; therefore, the temperature was increased to 2,600°F (1,427°C) and a secondary creep rate of 4.5x10 -6 h r -1 was Observed.
  • the stress was increased to 1,400 psi (9.65 Mn/m 2 ) and a new secondary creep rate of nominally 3x10 -5 h r -1 was recorded .
  • the ZGS material will have a stress rupture life of at least 48 hours when tested at 1400oC and 1000 psi in the rolling direction of the sheet.
  • the general microstructure of the crept specimen indicated that the grains were highly elongated in the rolling direction (creep stress direction also) end the grain bouncries were ragged. There appeared to be evidence of subgrains in the structure as well .
  • the microstructure observed in this specimen was typical of that of a good creep resistant material as evidenced by the exceptionally good creep properties.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
PCT/US1980/001061 1979-10-04 1980-08-18 Process for producing dispersion strengthened precious metal alloys WO1981000977A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US8172379A 1979-10-04 1979-10-04
US81723 2002-02-21

Publications (1)

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WO1981000977A1 true WO1981000977A1 (en) 1981-04-16

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ID=22165981

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Application Number Title Priority Date Filing Date
PCT/US1980/001061 WO1981000977A1 (en) 1979-10-04 1980-08-18 Process for producing dispersion strengthened precious metal alloys

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JP (1) JPS56501456A (enrdf_load_html_response)
CA (1) CA1178828A (enrdf_load_html_response)
GB (1) GB2075553A (enrdf_load_html_response)
SE (1) SE8103480L (enrdf_load_html_response)
WO (1) WO1981000977A1 (enrdf_load_html_response)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4518406A (en) * 1983-12-06 1985-05-21 Owens-Corning Fiberglas Corporation Drain bushing
US4536202A (en) * 1983-12-06 1985-08-20 Owens-Corning Fiberglas Corporation Drain bushing
EP0683240A3 (de) * 1994-05-19 1997-12-17 Schott Glaswerke Verfahren zur Herstellung von mit Yttriumoxid dispersionverfestigten Reinst-Platin-Werkstoffen, Halbzeugen und Blechen
EP1188844A1 (de) * 2000-09-18 2002-03-20 W.C. Heraeus GmbH & Co. KG Durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigter, goldfreier Platin-Werkstoff
EP1712646A4 (en) * 2004-10-08 2008-02-20 Tanaka Precious Metal Ind PLATINUM ALLOY MATERIAL COMPRISING DISPERSEED FORM OXIDE
US7867439B2 (en) * 2004-08-26 2011-01-11 Umicore Ag & Co., Kg Process for producing dispersoid-strengthened material

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101758227B (zh) * 2008-09-30 2011-10-26 王惠民 飞机玻璃座舱内电磁、雷达波屏蔽专用纳米铁粉
JP4965696B2 (ja) * 2010-10-21 2012-07-04 田中貴金属工業株式会社 酸化物分散強化型白金合金の製造方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3591362A (en) * 1968-03-01 1971-07-06 Int Nickel Co Composite metal powder
US3623849A (en) * 1969-08-25 1971-11-30 Int Nickel Co Sintered refractory articles of manufacture
US3640705A (en) * 1965-01-15 1972-02-08 Johnson Matthey Co Ltd Treatment of platinum group metals and alloys
US3738817A (en) * 1968-03-01 1973-06-12 Int Nickel Co Wrought dispersion strengthened metals by powder metallurgy
US4156053A (en) * 1976-09-07 1979-05-22 Special Metals Corporation Method of making oxide dispersion strengthened powder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3640705A (en) * 1965-01-15 1972-02-08 Johnson Matthey Co Ltd Treatment of platinum group metals and alloys
US3591362A (en) * 1968-03-01 1971-07-06 Int Nickel Co Composite metal powder
US3738817A (en) * 1968-03-01 1973-06-12 Int Nickel Co Wrought dispersion strengthened metals by powder metallurgy
US3623849A (en) * 1969-08-25 1971-11-30 Int Nickel Co Sintered refractory articles of manufacture
US4156053A (en) * 1976-09-07 1979-05-22 Special Metals Corporation Method of making oxide dispersion strengthened powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Platinum Metals Review, Volume 18, issued 1974, pages 46-56, Selman, G.L., et al: *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4518406A (en) * 1983-12-06 1985-05-21 Owens-Corning Fiberglas Corporation Drain bushing
US4536202A (en) * 1983-12-06 1985-08-20 Owens-Corning Fiberglas Corporation Drain bushing
EP0683240A3 (de) * 1994-05-19 1997-12-17 Schott Glaswerke Verfahren zur Herstellung von mit Yttriumoxid dispersionverfestigten Reinst-Platin-Werkstoffen, Halbzeugen und Blechen
EP1188844A1 (de) * 2000-09-18 2002-03-20 W.C. Heraeus GmbH & Co. KG Durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigter, goldfreier Platin-Werkstoff
US6663728B2 (en) 2000-09-18 2003-12-16 W.C. Heraeus Gmbh & Co. Kg Gold-free platinum material dispersion-strengthened by small, finely dispersed particles of base metal oxide
KR100491671B1 (ko) * 2000-09-18 2005-05-27 베.체. 헤레우스 게엠베하 운트 코. 카게 작고 미세하게 분산된 비금속 산화물 입자에 의해 분산강화된 금 미함유 백금 재료 및 그 제조 방법
US7867439B2 (en) * 2004-08-26 2011-01-11 Umicore Ag & Co., Kg Process for producing dispersoid-strengthened material
EP1712646A4 (en) * 2004-10-08 2008-02-20 Tanaka Precious Metal Ind PLATINUM ALLOY MATERIAL COMPRISING DISPERSEED FORM OXIDE

Also Published As

Publication number Publication date
CA1178828A (en) 1984-12-04
JPS56501456A (enrdf_load_html_response) 1981-10-08
SE8103480L (sv) 1981-06-03
GB2075553A (en) 1981-11-18

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