WO2004022801A1 - Method of forming non-sag molybdenum-lanthana alloys - Google Patents
Method of forming non-sag molybdenum-lanthana alloys Download PDFInfo
- Publication number
- WO2004022801A1 WO2004022801A1 PCT/US2003/027439 US0327439W WO2004022801A1 WO 2004022801 A1 WO2004022801 A1 WO 2004022801A1 US 0327439 W US0327439 W US 0327439W WO 2004022801 A1 WO2004022801 A1 WO 2004022801A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- lanthana
- molybdenum
- weight percent
- sintered body
- alloy
- Prior art date
Links
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 39
- 239000000956 alloy Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001953 recrystallisation Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims 5
- 239000000463 material Substances 0.000 description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 3
- 229910001182 Mo alloy Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
- B22F3/162—Machining, working after consolidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- 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
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
-
- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
Definitions
- This invention relates generally to methods for forming dispersion-strengthened alloys of molybdenum. More particularly, this invention relates to methods of forming molybdenum-lanthana alloys having non-sag microstructures .
- Molybdenum alloys which have been dispersion-strengthened with particles of lanthanum oxide (lanthana) , La 2 0 3 , are desirable for use in high temperature applications because of their high melting point and good mechanical properties at high temperatures, in particular, resistance to sag and creep.
- the alloys are formed by combining molybdenum powder with from about 0.1 to about 5 weight percent (wt.%) of lanthanum oxide powder or an equivalent amount of a lanthanum oxide precursor, such as La(0H) 3 or La(N0 3 ) , which is then converted to the oxide by heating.
- the size of the lanthanum oxide particles dispersed in the molybdenum matrix is generally preferred to be less than about 1 ⁇ m, however, the particles may be as large 5-10 ⁇ .
- the sintered body is deformed by mechanical working, e.g., rolling, swaging, drawing, or hammering, and then is then recrystallized to generate the desired microstructure .
- the preferred microstructure consists of large, interlocking grains which are elongated in the direction of the applied mechanical work.
- the recrystallization behavior of the alloy is affected by the prior amount of deformation. When the undeformed or fully recrystallized alloy is being cold worked, the density of dislocations within the alloy increases. This occurs first at the grain boundaries and then progresses further into the bulk of the grains as the amount of cold work increases.
- Prior art methods have employed high degrees of deformation (>60%) in order to achieve hi ' gh-temperature strength and creep-resistance.
- Japanese Patent Publication 59-177345 (1984) describes a molybdenum-lanthana alloy for structural purposes.
- the alloy has a high secondary recrystallization temperature and high high-temperature strength.
- the alloy contains 1 to 5 wt.% lanthana (La 2 0 3 ) particles having an average size of not more than 3 ⁇ m which are uniformly dispersed in molybdenum.
- the material is preferably worked from the sinter by a working factor of at least 60% and then heated above the secondary recrystallization temperature.
- One disadvantage with the prior art methods is that the dimensions of the feed material must be substantially greater than the dimensions of the finally recrystallized material in order to impart the required high degree of deformation. This leads to less flexibility in the manufacturing process.
- Another disadvantage is that the large amount of stored energy in the material caused by the high degree of deformation can lead to spontaneous grain growth in the material during recrystallization. This may make it more difficult to control grain size in the finally recrystallized material.
- a non-sag microstructure can be obtained in a molybdenum-lanthana alloy using a degree of deformation of from about 7% to about 18%.
- the degree of deformation refers to the percentage reduction in at least one dimension of the feed material, e.g., sheet thickness.
- the degree of deformation is from about 12% to about 17%.
- the alloy may be deformed directly from the as-sintered state to its finished form and then finally recrystallized or, preferably, the alloy can worked from the as-sintered state to a near-finished form, recrystallized, and then deformed to its finished form and finally recrystallized.
- the recrystallization of the alloy in its near-finished form is conducted at a temperature of from about 1150°C to about 1400°C.
- the final recrystallization is preferably conducted at about 1900°C.
- the amount of lanthana in the alloy ranges from 0.4 wt.% to about 1.0 wt.%, more preferably, from about 0.6 wt.% to about 0.7 wt.%.
- the grain size after final recrystallization is larger because the predominant mechanism occurring during the heat treatment is the annihilation of dislocations at the neighboring grain boundaries causing some grain boundaries to disappear. This is generally referred to as strain-induced grain boundary migration.
- the grains tend to exhibit less elongation than grains resulting from methods which use high degrees of deformation.
- the aspect ratio for the grains produced by the method of this invention is no more than 4:1.
- the degree of reformation needed to produce the non-sag microstructure is about 18% or less, the feed material need not be much larger than the finished product and there is a greater potential to control grain size in the finished material because of the lower amount of stored energy in the material prior to final recrystallization.
- the method of this invention is more flexible for manufacturers of refractory metal products.
- Fig. 1A is a photomicrograph of the microstructure of the molybdenum-lanthana alloy of Example 1 after recrystallization and rolling to 0.15 cm thickness.
- Fig. IB is a photomicrograph of non-sag microstructure of the molybdenum-lanthana alloy of Example 1 after final recrystallization .
- Fig. 2A is a photomicrograph of the microstructure of the molybdenum-lanthana alloy of Example 2 after recrystallization and rolling to 0.10 cm thickness.
- Fig. 2B is a photomicrograph of non-sag microstructure of the molybdenum-lanthana alloy of Example 2 after final recrystallization .
- Pure molybdenum metal powder with grain size of 3.5 ⁇ m was mixed with 0.7 weight percent (wt.%) of La(0H) 3 powder having a grain size of 0.65 ⁇ m.
- the mixture was isostatically pressed at 240 MPa to form a pressed slab with dimensions of 64 cm x 38 cm x 5 cm.
- the slab was subsequently rolled at varying temperatures; starting at 980°C, followed by 785°C, and finally at ambient temperature to a thickness of 0.17 cm.
- the sheet was then recrystallized at 1400°C and then rolled at ambient temperature to the thickness of 0.15 cm, (about 12% deformation) .
- the microstructure of the recrystallized and rolled sheet is shown in Fig. 1A.
- the rolled sheet was subjected to a final recrystallization anneal at 1900°C to produce the non-sag microstructure which is shown in Fig. IB.
- Pure molybdenum metal powder with grain size of 3.5 ⁇ m was mixed with 0.7 wt.% La(0H) 3 powder with a grain size of 0.65 ⁇ m.
- the mixture was isostatically pressed at 240 MPa to form a pressed slab with dimensions of 64 cm x 38 cm x 5 cm.
- the slab was subsequently rolled at varying temperatures; starting at 980°C, followed by 785°C, and finally at ambient temperature to a thickness of 0.12 cm.
- the sheet was then recrystallized at 1150°C. Subsequently it was rolled at ambient temperature to the thickness of 0.10 cm (about 17% deformation) .
- the microstructure of the recrystallized and rolled sheet is shown in Fig. 2A.
- the sheet material exhibited the non-sag microstructure shown in Fig. 2B.
- the sag resistance of 0.5 in. x 5.6 in. samples of the non-sag molybdenum-lanthana sheet material from Examples 1 and 2 was measured according to the following procedure. The samples were supported at opposite ends and a 10 g weight placed on the sample at the center point between the supports. The distance between the supports was 4.2 inches. At the start of the test, the distance between the reference plate and the 0.15-cm-thick sample was 0.5 in. at the point directly below the 10-g load. The corresponding distance for the 0.10-cm-thick sample was 0.4375 in. at the start of the test. Sag was measured as the amount of deflection of the sample toward the reference plate after heating the sample at 1900°C for 1 hour.
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- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Powder Metallurgy (AREA)
- Polyurethanes Or Polyureas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/526,480 US20060073063A1 (en) | 2002-09-04 | 2003-09-04 | Method of forming non-sag molybdenum-lanthana alloys |
DE60312012T DE60312012T2 (en) | 2002-09-04 | 2003-09-04 | METHOD FOR THE PRODUCTION OF SAG-RESISTANT MOLYBDEN-LANTHANOXIDE ALLOYS |
EP03794565A EP1546422B1 (en) | 2002-09-04 | 2003-09-04 | Method of forming sag-resistant molybdenum-lanthana alloys |
AU2003263051A AU2003263051A1 (en) | 2002-09-04 | 2003-09-04 | Method of forming non-sag molybdenum-lanthana alloys |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US40808702P | 2002-09-04 | 2002-09-04 | |
US60/408,087 | 2002-09-04 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004022801A1 true WO2004022801A1 (en) | 2004-03-18 |
Family
ID=31978560
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2003/027439 WO2004022801A1 (en) | 2002-09-04 | 2003-09-04 | Method of forming non-sag molybdenum-lanthana alloys |
Country Status (6)
Country | Link |
---|---|
US (1) | US20060073063A1 (en) |
EP (1) | EP1546422B1 (en) |
AT (1) | ATE354683T1 (en) |
AU (1) | AU2003263051A1 (en) |
DE (1) | DE60312012T2 (en) |
WO (1) | WO2004022801A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004095501A3 (en) * | 2003-04-23 | 2005-04-21 | Starck H C Inc | Molybdenum alloy x-ray targets having uniform grain structure |
CN102626845A (en) * | 2012-03-27 | 2012-08-08 | 苏州先端稀有金属有限公司 | Molybdenum lanthanum alloy tray processing method |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110100356A1 (en) * | 2009-10-13 | 2011-05-05 | Wayne Thomas Bliesner | Reversible hydride thermal energy storage cell optimized for solar applications |
KR20180016693A (en) * | 2016-08-05 | 2018-02-19 | 삼성디스플레이 주식회사 | Linear evaporation source and deposition apparatus including the same |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3785801A (en) * | 1968-03-01 | 1974-01-15 | Int Nickel Co | Consolidated composite materials by powder metallurgy |
US4950327A (en) * | 1987-01-28 | 1990-08-21 | Schwarzkopf Development Corporation | Creep-resistant alloy of high-melting metal and process for producing the same |
US5134039A (en) * | 1988-04-11 | 1992-07-28 | Leach & Garner Company | Metal articles having a plurality of ultrafine particles dispersed therein |
US5435829A (en) * | 1992-10-29 | 1995-07-25 | H. C. Starck Gmbh & Co. Kg | Molybdenum powder mixture for TZM |
US5835841A (en) * | 1992-10-21 | 1998-11-10 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Composite material and production thereof |
US5868876A (en) * | 1996-05-17 | 1999-02-09 | The United States Of America As Represented By The United States Department Of Energy | High-strength, creep-resistant molybdenum alloy and process for producing the same |
US6102979A (en) * | 1998-08-28 | 2000-08-15 | The United States Of America As Represented By The United States Department Of Energy | Oxide strengthened molybdenum-rhenium alloy |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3467774D1 (en) * | 1983-02-10 | 1988-01-07 | Toshiba Kk | Molybdenum board and process of manufacturing the same |
AT389326B (en) * | 1987-11-09 | 1989-11-27 | Plansee Metallwerk | METHOD FOR PRODUCING SEMI-FINISHED PRODUCTS FROM Sintered Refractory Metal Alloys |
AT392432B (en) * | 1989-05-03 | 1991-03-25 | Plansee Metallwerk | METHOD FOR THE PRODUCTION OF WARM-CRAWL-RESISTANT SEMI-FINISHED PRODUCTS OR MOLDED PARTS FROM HIGH-MELTING METALS |
-
2003
- 2003-09-04 US US10/526,480 patent/US20060073063A1/en not_active Abandoned
- 2003-09-04 AU AU2003263051A patent/AU2003263051A1/en not_active Abandoned
- 2003-09-04 DE DE60312012T patent/DE60312012T2/en not_active Expired - Lifetime
- 2003-09-04 WO PCT/US2003/027439 patent/WO2004022801A1/en active IP Right Grant
- 2003-09-04 AT AT03794565T patent/ATE354683T1/en not_active IP Right Cessation
- 2003-09-04 EP EP03794565A patent/EP1546422B1/en not_active Expired - Fee Related
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3785801A (en) * | 1968-03-01 | 1974-01-15 | Int Nickel Co | Consolidated composite materials by powder metallurgy |
US4950327A (en) * | 1987-01-28 | 1990-08-21 | Schwarzkopf Development Corporation | Creep-resistant alloy of high-melting metal and process for producing the same |
US5134039A (en) * | 1988-04-11 | 1992-07-28 | Leach & Garner Company | Metal articles having a plurality of ultrafine particles dispersed therein |
US5835841A (en) * | 1992-10-21 | 1998-11-10 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Composite material and production thereof |
US5435829A (en) * | 1992-10-29 | 1995-07-25 | H. C. Starck Gmbh & Co. Kg | Molybdenum powder mixture for TZM |
US5868876A (en) * | 1996-05-17 | 1999-02-09 | The United States Of America As Represented By The United States Department Of Energy | High-strength, creep-resistant molybdenum alloy and process for producing the same |
US6102979A (en) * | 1998-08-28 | 2000-08-15 | The United States Of America As Represented By The United States Department Of Energy | Oxide strengthened molybdenum-rhenium alloy |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004095501A3 (en) * | 2003-04-23 | 2005-04-21 | Starck H C Inc | Molybdenum alloy x-ray targets having uniform grain structure |
CN102626845A (en) * | 2012-03-27 | 2012-08-08 | 苏州先端稀有金属有限公司 | Molybdenum lanthanum alloy tray processing method |
Also Published As
Publication number | Publication date |
---|---|
US20060073063A1 (en) | 2006-04-06 |
DE60312012D1 (en) | 2007-04-05 |
ATE354683T1 (en) | 2007-03-15 |
EP1546422A1 (en) | 2005-06-29 |
AU2003263051A1 (en) | 2004-03-29 |
EP1546422B1 (en) | 2007-02-21 |
EP1546422A4 (en) | 2006-04-05 |
DE60312012T2 (en) | 2007-08-09 |
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