WO1981001013A1 - Thermomechanical processing of dispersion-strengthened precious metal alloys - Google Patents
Thermomechanical processing of dispersion-strengthened precious metal alloys Download PDFInfo
- Publication number
- WO1981001013A1 WO1981001013A1 PCT/US1980/001062 US8001062W WO8101013A1 WO 1981001013 A1 WO1981001013 A1 WO 1981001013A1 US 8001062 W US8001062 W US 8001062W WO 8101013 A1 WO8101013 A1 WO 8101013A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- process according
- dispersion
- precious metal
- yttria
- carried out
- Prior art date
Links
- 229910000923 precious metal alloy Inorganic materials 0.000 title claims abstract description 14
- 238000012545 processing Methods 0.000 title claims description 10
- 230000000930 thermomechanical effect Effects 0.000 title claims description 9
- 238000000034 method Methods 0.000 claims abstract description 23
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000005551 mechanical alloying Methods 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 238000005728 strengthening Methods 0.000 claims description 3
- 229910001260 Pt alloy Inorganic materials 0.000 claims 2
- 238000005275 alloying Methods 0.000 claims 1
- 238000000713 high-energy ball milling Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000003801 milling Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000011109 contamination Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- WLNBMPZUVDTASE-HXIISURNSA-N (2r,3r,4s,5r)-2-amino-3,4,5,6-tetrahydroxyhexanal;sulfuric acid Chemical compound [O-]S([O-])(=O)=O.O=C[C@H]([NH3+])[C@@H](O)[C@H](O)[C@H](O)CO.O=C[C@H]([NH3+])[C@@H](O)[C@H](O)[C@H](O)CO WLNBMPZUVDTASE-HXIISURNSA-N 0.000 description 1
- -1 Ce Na Inorganic materials 0.000 description 1
- 229910018967 Pt—Rh Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 235000012771 pancakes Nutrition 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
Definitions
- TECHNICAL FIELD This i nv ⁇ ntion rel ates to thermomechani cal processing of di spersi on- 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.
- Structural components such as these at elevated temperatures under constant loads experience continuous dimensional changes or creep during their lives. This creep behavior depends upon the interaction between the external conditions (load, temperature) and the microstructure of the component.
- increased resistance to creep of material systems has been accomplished by using a dispersion of very small, hard particles (called dispersoids) to strengthen the microstructure of the component.
- dispersoids very small, hard particles
- These systems have become to be known as d ispersi on- strengthened metals and alloys and the dispersoids used are usually oxides.
- a recent development in dispersion-strengthening is mechanical alloying which uses a high energy ball mill to achieve the intimate mechanical mixing typical of the process. An attritor mill or vibratory mill also can be used.
- the present invention provides for the thermomechani cal processing of dispersion-strengthened precious metal alloys.
- the invention is comprised of a series of mechanical deformation and annealing cycles to help develop a creep resistant microstructure. Specifically, I achieve this by rolling and annealing a powder compact of dispersion-strengthened precious metal.
- the material may be cross-rolled as well as longitudinally rolled or just longitudinally rolled.
- FIGURE 1 is a schematic drawing of the rolling operation.
- the proceoure used to thermomechanically process the compact was to roll the compact for a 10 percent reduction in area then anneal the rolled specimen.
- the reduction in area is carried out under a pressure that elongates the rolled specimen without substantially widening it.
- the annealing is carried out for a period of time and at a temperature sufficient to develop a specimen with a minimum creep rate.
- the annealing is carried out for five minutes at at 1,900°F (1,040°C) before further rolling.
- the total extent of deformation ranges from 50 to 20 percent reduction in area and generally is approximately an 85 percent reduction in area.
- This roll/anneal cycle was selected to help develop a creep resistance microstructure.
- Dispersion-strengthened precious m ⁇ tals are known in the art and are commercially available.
- One such material is that available from Johnson, Matthey & Co.
- 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 mftals of this invention generally comprise a precious metal, or precious metal alloy, preferably platinum, as the dispersing medium, or matrix, and a dispersoid of a metal oxide, metal carbide, metal silicide, metal nitride, metal sulfide or a metal boride which dispersoid is present in effective dispersion-strengthening amounts. Usually such amounts will be between about 0.1 percent to about 5.0 percent by volume.
- the dispersoid will be an oxide.
- Exemplary of metal compounds which may be employed as the dispersoid are compounds of metals of Group IIA, IIIA, 111 E (including non-hazardous metals of the Actinid ⁇ and Lanthanide classes) , I VB , VB , VI B and VI IB. More specifically exemplary of suitable metals are the following: Be, Kg, Ca, Ba, Y, La, Ti , Zr, Hf M o W, Ce Na , Ga , and Th as Well as Al .
- VHP vacuum hot pressing
- the samples can be consolidated by first cold 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
- the cold pressing is carried out at a pressure ranging from 2,000 to 10,000 psi for up to 5 minutes followed by sintering at a temperature ranging from 120G to 1700°C for 2 to 6 hours.
- EXAMPLE I Approximately one kgm of -325 mesh (-44 micron) platinum sponge from Englehard was blended with an amount of yttria (Y 2 0 3 ) to give nominally 0.65 volume percent (0.15 weight percent) oxide loading in the final compact.
- the yttria was nominally 200-600 angstrom in size.
- the platinum matrix starting powder for the experiment consisted of v ery fine, near spherical particles or chained aggregates. Most of the particles below 2 microns appeared to be single crystals. The starting powder had a fairly high specific surface area.
- the pov-der 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 20:1.
- the grinding media used was a hardened 400 series stainless steel bearing nominally 3/8 inch (0.953 cm) diameter.
- the impeller rotational speec 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 experiment was continued for 71 hours then terminated, and the powder was removed for further processing .
- the maximum iron contamination level in the powder was approximately 300 wppm.
- the milled powder was consolidated by vacuum hot pressing and thermomechani cal ly 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 60 gms) taken at various times during the milling experiment, each sample was individually consolidated by vacuum hot pressing (VHP) ⁇ t 1,450°C under 5, 000 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) 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. After the 10th rolling pass, the grain structure was fairly elongated. The lack of oxide clusters during optical metal lographic examination suggested that the milling action had worked the yttria into the platinum matrix. A metal 1 ographic analysis of the same region showed the development of a moderate grain aspect ratio
- Creep results were obtained from specimens that were processed according to Example II except that these specimens w e r e milled 10 hours and received the above thermomechanical processing treatment of 10% reduction in area per pass with an intermediate anneal at nominally 1040oC 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 2,400oF (1,316°C). The resultant secondary creep rate was too low to adequately measure; therefore, the temperature was increased to
- the ZGS material will have a stress rupture life of at least 48 hours when tested at 1400 oC 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) and the grain boundries 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)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (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)
- Reinforced Plastic Materials (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US8172279A | 1979-10-04 | 1979-10-04 | |
| US81722 | 1979-10-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1981001013A1 true WO1981001013A1 (en) | 1981-04-16 |
Family
ID=22165974
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US1980/001062 WO1981001013A1 (en) | 1979-10-04 | 1980-08-18 | Thermomechanical processing of dispersion-strengthened precious metal alloys |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JPS56501457A (enrdf_load_html_response) |
| CA (1) | CA1178459A (enrdf_load_html_response) |
| GB (1) | GB2075552A (enrdf_load_html_response) |
| SE (1) | SE8103481L (enrdf_load_html_response) |
| WO (1) | WO1981001013A1 (enrdf_load_html_response) |
Cited By (8)
| 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 |
| EP0320877A3 (en) * | 1987-12-18 | 1989-11-02 | Ppg Industries, Inc. | Lamination of oxide dispersion strengthened patinum and alloys |
| EP1188844A1 (de) * | 2000-09-18 | 2002-03-20 | W.C. Heraeus GmbH & Co. KG | Durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigter, goldfreier Platin-Werkstoff |
| US20160289808A1 (en) * | 2013-12-06 | 2016-10-06 | Heraeus Deutschland GmbH & Co. KG | Method for processing a dispersion-hardened platinum composition |
| EP3971311A1 (de) | 2020-09-17 | 2022-03-23 | Heraeus Deutschland GmbH & Co. KG | Verbesserte, dispersionsgehärtete edelmetalllegierung |
| EP3978884A1 (de) | 2020-10-02 | 2022-04-06 | Heraeus Deutschland GmbH & Co. KG | Draht mit platin-zusammensetzung zur kontaktierung von temperatursensoren |
| EP4492048A1 (de) | 2023-07-12 | 2025-01-15 | Heraeus Precious Metals GmbH & Co. KG | Verfahren zur messung einer elektrischen grösse zur bestimmung der zeitdauer einer dispersionshärtung eines metallhaltigen formkörpers |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1134492A (en) * | 1964-03-11 | 1968-11-27 | Johnson Matthey Co Ltd | Methods of improving the mechanical properties of metals and their alloys |
| CA801702A (en) * | 1968-12-17 | W. Fraser Robert | Working cycle for dispersion strengthened materials | |
| 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 |
-
1980
- 1980-08-18 GB GB8112099A patent/GB2075552A/en not_active Withdrawn
- 1980-08-18 WO PCT/US1980/001062 patent/WO1981001013A1/en unknown
- 1980-08-18 JP JP50222980A patent/JPS56501457A/ja active Pending
- 1980-09-16 CA CA000360277A patent/CA1178459A/en not_active Expired
-
1981
- 1981-06-03 SE SE8103481A patent/SE8103481L/ not_active Application Discontinuation
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA801702A (en) * | 1968-12-17 | W. Fraser Robert | Working cycle for dispersion strengthened materials | |
| GB1134492A (en) * | 1964-03-11 | 1968-11-27 | Johnson Matthey Co Ltd | Methods of improving the mechanical properties of metals and their alloys |
| 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 |
Cited By (13)
| 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 |
| EP0320877A3 (en) * | 1987-12-18 | 1989-11-02 | Ppg Industries, Inc. | Lamination of oxide dispersion strengthened patinum and alloys |
| 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 |
| US20160289808A1 (en) * | 2013-12-06 | 2016-10-06 | Heraeus Deutschland GmbH & Co. KG | Method for processing a dispersion-hardened platinum composition |
| EP3077556B1 (de) | 2013-12-06 | 2019-06-19 | Heraeus Deutschland GmbH & Co. KG | Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung |
| EP3971311A1 (de) | 2020-09-17 | 2022-03-23 | Heraeus Deutschland GmbH & Co. KG | Verbesserte, dispersionsgehärtete edelmetalllegierung |
| US11781208B2 (en) | 2020-09-17 | 2023-10-10 | Heraeus Deutschland GmbH & Co. KG | Dispersion-hardened precious-metal alloy |
| EP3978884A1 (de) | 2020-10-02 | 2022-04-06 | Heraeus Deutschland GmbH & Co. KG | Draht mit platin-zusammensetzung zur kontaktierung von temperatursensoren |
| US12024763B2 (en) | 2020-10-02 | 2024-07-02 | Heraeus Deutschland GmbH & Co. KG | Wire with platinum composition for contacting temperature sensors |
| EP4492048A1 (de) | 2023-07-12 | 2025-01-15 | Heraeus Precious Metals GmbH & Co. KG | Verfahren zur messung einer elektrischen grösse zur bestimmung der zeitdauer einer dispersionshärtung eines metallhaltigen formkörpers |
Also Published As
| Publication number | Publication date |
|---|---|
| CA1178459A (en) | 1984-11-27 |
| SE8103481L (sv) | 1981-06-03 |
| GB2075552A (en) | 1981-11-18 |
| JPS56501457A (enrdf_load_html_response) | 1981-10-08 |
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