US20040206429A1 - Large diameter tungsten-lanthana rod - Google Patents

Large diameter tungsten-lanthana rod Download PDF

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US20040206429A1
US20040206429A1 US10/767,052 US76705204A US2004206429A1 US 20040206429 A1 US20040206429 A1 US 20040206429A1 US 76705204 A US76705204 A US 76705204A US 2004206429 A1 US2004206429 A1 US 2004206429A1
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rod
lanthana
diameter
tungsten
rolling
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Ricky Morgan
Thomas Dixon
Harry Martin
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    • 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
    • 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
    • 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
    • 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
    • B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
    • B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
    • 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
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • This invention is related to tungsten rod and methods of forming tungsten rod. More particularly, it is related to large-diameter tungsten-lanthana rod with an elongated grain structure.
  • Tungsten-lanthana alloys are well-known. A description of these alloys, their methods of making, and uses can be found in U.S. Pat. Nos. 5,590,386, 5,742,891, 4,923,673, 3,159,908 and 3,086,103.
  • tungsten-lanthana alloys are used to manufacture rocket nozzles. Rocket nozzles require high strength along the nozzle's longitudinal axis because of the high temperatures and internal combustive forces generated during its operation. In order to provide this high strength, the tungsten-lanthana rod from which the nozzle is machined should have a microstructure in which the tungsten grains are elongated in a direction substantially parallel to the longitudinal axis of the rod. Current methods of forging and extrusion for forming large-diameter tungsten rods (>0.625 in. dia.) achieve acceptable mechanical properties but have been ineffective at producing a longitudinal grain elongation.
  • FIG. 1 is a micrograph of the longitudinally elongated grain structure of a rolled tungsten-lanthana rod subjected to a reduction in cross-sectional area of about 40%.
  • FIG. 2 is a micrograph of the longitudinally elongated grain structure of a rolled tungsten-lanthana rod subjected to a reduction in cross-sectional area of about 70%.
  • a rolling process has been developed to produce large-diameter tungsten-lanthana rod with grain elongation substantially parallel to the longitudinal axis of the rod.
  • large diameter means that the rod has a diameter greater than 0.625 inches as worked. Acceptable mechanical properties were achieved with at least about a 40% reduction in cross-sectional area (RIA).
  • RIA cross-sectional area
  • the diameter of the worked rod ranges from greater than 0.625 inches to 2.250 inches and the lanthana contents range from 0.3 wt. % to 2.5 wt. %.
  • the parallel-elongated structure was achieved by rolling bars of tungsten-lanthana at temperatures greater than 1400° C.
  • rolling temperatures must be greater than 1400° C. and less than 1700° C.
  • Rod reheating can occur at any point up to a maximum of four rolling passes.
  • Starting bar diameters of greater than 1.5 inches require an in-process stress relief at a point between 25 and 45% reduction in area.
  • a pressed and sintered bar of tungsten containing 1.3 wt. % lanthana (LT8103-008) and measuring 2.374 inches in diameter by 23.5 inches in length was rolled at 1500° C. on a two-high rod rolling mill to 1.850 inches in diameter by 38 inches in length (a reduction-in-area of 39.27%) and stress relieved at 1400° C. for 1 ⁇ 2 hour.
  • the rolling schedule is given in Table 1.
  • the material was then tested for tensile properties, density, and hardness. The test results are provided in Table 0.4. Microstructures showed grain elongation parallel to the longitudinal axis of the rod. TABLE 1 1500° C. Nominal. Nominal Groove Soak Diameter Diameter Pass Dia.
  • a pressed and sintered bar of tungsten containing 1.3 wt. % lanthana (LT8103-004) and measuring-1.400 inches in diameter by 33 inches in length was reduced by a two-high rod rolling method to 0.733 inches in diameter by 50 inches in length at 1500° C.
  • the rod wasthen finish swaged to 0.682 in diameter by 56 inches in length at 1300° C.; a total reduction-in-area of 76%.
  • the rolling schedule is provided in Table 2.
  • the measured mechanical properties are given in Table 4.
  • FIGS. 1 and 2 show the microstructures of the rolled rods after about 40% RIA and about 70% RIA, respectively. Greater elongation is observed at the higher RIA.
  • Grain elongation was parallel to the longitudinal axis of the rod. Grains are elongated from left to right in the micrographs. The black specks in the micrographs are the lanthana particles. TABLE 2 1500° C. Nominal. Nominal Groove Soak Diameter Diameter Pass Dia. Time Before After RIA cumulative No.
  • the mechanical properties compare favorably with the values measured for forged materials.
  • the ultimate tensile strength (UTS) for forged materials ranges from 65 to 89 ksi; the yield strength (YS) from 53 to 82 ksi; elongation from 12 to 32%; and hardness from 41 to 42 Rockwell C.
  • the results in Table 4 demonstrate that the large-diameter tungsten-lanthana rod of this invention has a UTS of from about 70 to about 85 ksi, a YS of from about 60 to about 80 ksi and a hardness of from about 40 to about 43 Rockwell C.
  • the large-diameter rod of this invention possesses both the grain structure and mechanical properties desired for rocket nozzle applications.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Forging (AREA)

Abstract

A large-diameter tungsten-lanthana rod having an elongated grain structure substantially parallel to the longitudinal axis of the rod is described. The large diameter rod is produced by rolling at a temperature greater than 1400° C. and less than 1700° C. to achieve at least about a 40% reduction in cross-sectional area. The high strength of the longitudinally elongated grain structure is desirable for applications such as rocket nozzles.

Description

    TECHNICAL FIELD
  • This invention is related to tungsten rod and methods of forming tungsten rod. More particularly, it is related to large-diameter tungsten-lanthana rod with an elongated grain structure. [0001]
    • BACKGROUND OF THE INVENTION
  • Tungsten-lanthana alloys are well-known. A description of these alloys, their methods of making, and uses can be found in U.S. Pat. Nos. 5,590,386, 5,742,891, 4,923,673, 3,159,908 and 3,086,103. [0002]
  • In addition to the uses referenced above, tungsten-lanthana alloys are used to manufacture rocket nozzles. Rocket nozzles require high strength along the nozzle's longitudinal axis because of the high temperatures and internal combustive forces generated during its operation. In order to provide this high strength, the tungsten-lanthana rod from which the nozzle is machined should have a microstructure in which the tungsten grains are elongated in a direction substantially parallel to the longitudinal axis of the rod. Current methods of forging and extrusion for forming large-diameter tungsten rods (>0.625 in. dia.) achieve acceptable mechanical properties but have been ineffective at producing a longitudinal grain elongation. [0003]
    • SUMMARY OF THE INVENTION
  • It is an object of the invention to obviate the disadvantages of the prior art. [0004]
  • It is another object of the invention to provide a large diameter tungsten-lanthana rod having a grain structure which is elongated in a direction substantially parallel to the longitudinal axis of the rod. [0005]
  • It is still another object of the invention to provide a large-diameter tungsten-lanthana rod having mechanical properties desirable for rocket nozzle applications. [0006]
  • These and other objects and advantages of the invention have been achieved by rolling large-diameter tungsten-lanthana rod at a temperature greater than 1400° C. and less than 1700° C. to achieve a reduction in the cross-sectional area of at least about 40%. These rolling parameters yield a large-diameter rod-having an elongated grain structure which is substantially parallel to the longitudinal axis of the rod. The as-worked rod has mechanical properties desirable for rocket nozzle applications.[0007]
    • BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 is a micrograph of the longitudinally elongated grain structure of a rolled tungsten-lanthana rod subjected to a reduction in cross-sectional area of about 40%. [0008]
  • FIG. 2 is a micrograph of the longitudinally elongated grain structure of a rolled tungsten-lanthana rod subjected to a reduction in cross-sectional area of about 70%.[0009]
    • DETAILED DESCRIPTION OF THE INVENTION
  • For a better understanding of the present invention, together with other and further objects, advantages and capabilities thereof, reference is made to the following disclosure and appended claims taken in conjunction with the above-described drawings. [0010]
  • A rolling process has been developed to produce large-diameter tungsten-lanthana rod with grain elongation substantially parallel to the longitudinal axis of the rod. As used herein, large diameter means that the rod has a diameter greater than 0.625 inches as worked. Acceptable mechanical properties were achieved with at least about a 40% reduction in cross-sectional area (RIA). Preferably, the diameter of the worked rod ranges from greater than 0.625 inches to 2.250 inches and the lanthana contents range from 0.3 wt. % to 2.5 wt. %. [0011]
  • The parallel-elongated structure was achieved by rolling bars of tungsten-lanthana at temperatures greater than 1400° C. In particular, rolling temperatures must be greater than 1400° C. and less than 1700° C. Rod reheating can occur at any point up to a maximum of four rolling passes. Starting bar diameters of greater than 1.5 inches require an in-process stress relief at a point between 25 and 45% reduction in area. [0012]
  • The following non-limiting examples are presented. [0013]
    • EXAMPLE 1
  • A pressed and sintered bar of tungsten containing 1.3 wt. % lanthana (LT8103-008) and measuring 2.374 inches in diameter by 23.5 inches in length was rolled at 1500° C. on a two-high rod rolling mill to 1.850 inches in diameter by 38 inches in length (a reduction-in-area of 39.27%) and stress relieved at 1400° C. for ½ hour. The rolling schedule is given in Table 1. The material was then tested for tensile properties, density, and hardness. The test results are provided in Table 0.4. Microstructures showed grain elongation parallel to the longitudinal axis of the rod. [0014]
    TABLE 1
    1500° C. Nominal. Nominal
    Groove Soak Diameter Diameter
    Pass Dia. Time Before After RIA cumulative
    No. (in.) (min.) (in.) (in.) (%) RIA (%)
    1 2.393 15 — — — —
    2 2.393 5 — — — —
    3 2.146 5 — 2.325 — 4.1
    4 2.146 5 2.325 — — —
    5 2.020 5 — — — —
    6 2.020 5 — 2.085 — 22.9
    7 1.875 15 2.085 1.985 9.4 30.1
    8 1.875 5 1.985 1.850 13.1 39.3
    • EXAMPLE 2
  • A pressed and sintered bar of tungsten containing 1.3 wt. % lanthana (LT8103-004) and measuring-1.400 inches in diameter by 33 inches in length was reduced by a two-high rod rolling method to 0.733 inches in diameter by 50 inches in length at 1500° C. The rod wasthen finish swaged to 0.682 in diameter by 56 inches in length at 1300° C.; a total reduction-in-area of 76%. The rolling schedule is provided in Table 2. The measured mechanical properties are given in Table 4. FIGS. 1 and 2 show the microstructures of the rolled rods after about 40% RIA and about 70% RIA, respectively. Greater elongation is observed at the higher RIA. Grain elongation was parallel to the longitudinal axis of the rod. Grains are elongated from left to right in the micrographs. The black specks in the micrographs are the lanthana particles. [0015]
    TABLE 2
    1500° C. Nominal. Nominal
    Groove Soak Diameter Diameter
    Pass Dia. Time Before After RIA cumulative
    No. (in.) (min.) (in.) (in.) (%) RIA (%)
    1 1.320 15 1.400 — — —
    2 1.320 5 — — — —
    3 1.219 5 — — — 4.1
    4 1.219 5 — 1.290 — 15.1
    5 1.125 5 1.290 1.195 14.2 27.1
    6 1.125 5 1.195 1.178 2.8 29.2
    7 1.040 5 1.178 1.091 14.2 39.3
    8 1.040 5 1.091 1.084 1.3 40.0
    9 0.969 5 1.084 1.015 12.3 47.4
    10 0.969 5 1.015 1.002 2.5 48.8
    11 0.906 5 1.002 0.940 12.0 54.9
    12 0.906 5 0.940 0.930 2.1 55.9
    13 0.850 5 0.930 0.855 15.5 62.7
    14 0.850 5 0.855 0.855 0.0 62.7
    15 0.797 5 0.855 0.795 13.5 67.8
    16 0.797 15 0.795 0.805 0.0 67.8
    17 0.750 5 0.805 — — —
    18 0.750 5 — 0.733 — 72.6
    • EXAMPLE 3
  • Another bar of tungsten-1.3 wt. % lanthana (LT8103-009) measuring 2.41 inches in diameter was reduced by a two-high rod rolling method to a 2.050 inch diameter at 1400° C., a 27.6% reduction in area. At this point, the bar was rolled on a different set of rolls at 1400° C. to 2.025 inches in diameter for a total reduction in area of 29.4%. At this point, the rod split prematurely due to the 1400° C. rolling temperature. After stress relieving the rod at 1500° C. for 30 minutes, the rod was rolled successfully to a 1.265 inch diameter at 1500° C. for a total reduction in area of 72.4%. The rod was then stress relieved at 1400° C. for 30 minutes. The actual rolling schedule is provided in Table 3. Density, hardness and tensile properties are given in Table 4. As expected, grain elongation was parallel to the longitudinal axis of the rod. [0016]
    TABLE 3
    Nominal. Nominal
    Groove Diameter Diameter
    Dia. 1500° C. Soak Before After cumulative
    Pass No. (in.) Time (min.) (in.) (in.) RIA (%) RIA (%)
    1 2.393 15 (1400° C.)  — — — —
    2 2.393 5 (1400° C.) — — — —
    3 2.146 5 (1400° C.) — 2.325 — 6.9
    4 2.146 5 (1400° C.) 2.325 — — —
    5 2.020 5 (1400° C.) — — — —
    6 2.020 5 (1400° C.) — 2.050 — 27.6
    7 1.875 15 (1400° C.)  2.050 — — —
    8 1.875 5 (1400° C.) — 2.025 2.4 29.4
    9 1.718 5 (1400° C.) 2.025 1.850 16.5 41.1
    10 1.718 15 1.850 1.733 2.5 48.3
    11 1.718 5 — — — —
    12 1.578 5 — — — —
    13 1.578 5 — 1.580 — 57.0
    14 1.445 5 1.580 — — —
    15 1.445 5 — 1.422-1.425 — 65.1
    16 1.320 5 1.423 — — —
    17 1.320 5 — 1.310-1.325 — 70.1
    18 2.002 5 1.317 1.281 5.4 71.7
    19 2.020 5 1.281 1.265-1.266 2.4 72.4
  • [0017]
    TABLE 4
    Sample
    Direction Density Hardness UTS YS
    Sample (longitudinal) (g/cc) Rockwell C (ksi) (ksi) Elongation %
    LT8103-004
    As rolled Edge 18.76 42.7 — — —
    Center 18.72 43 85.4 79.4 26
    Stress Edge — 42.8 — — —
    relieved Center — 42.9 80, 74† 71, 66† 27, 27†
    (1500° C.,
    ½ hour)
    Stress Edge — 42.6 — — —
    relieved Center — 42.5 77, 79† 69, 72† 25, 28†
    (1600° C.,
    ½ hour)
    LT8103-008
    Stress Edge 18.76 40 71, 73† 67, 61† 32, 35†
    relieved Center 18.6 39.7 73, 74† 61, 62† 28, 30†
    (1400° C.,
    ½ hour)
    LT8103-009
    Stress Edge 18.72 41 77, 78† 62, 64† 32, 34†
    relieved Center 18.64 41.3 81 59 56
    (1400° C.,
    ½ hour)
  • The mechanical properties compare favorably with the values measured for forged materials. In particular, the ultimate tensile strength (UTS) for forged materials ranges from 65 to 89 ksi; the yield strength (YS) from 53 to 82 ksi; elongation from 12 to 32%; and hardness from 41 to 42 Rockwell C. The results in Table 4 demonstrate that the large-diameter tungsten-lanthana rod of this invention has a UTS of from about 70 to about 85 ksi, a YS of from about 60 to about 80 ksi and a hardness of from about 40 to about 43 Rockwell C. Thus, the large-diameter rod of this invention possesses both the grain structure and mechanical properties desired for rocket nozzle applications. [0018]
  • While there has been shown and described what are at the present considered the preferred embodiments of the invention, it will be obvious to those skilled in the art that various changes and modifications may be made therein without departing from the scope of the invention as defined by the appended claims. [0019]

Claims (8)

1-7. (canceled).
8. A method of making a large-diameter tungsten-lanthana rod comprising rolling a tungsten-lanthana rod at a temperature greater than 1400° C. and less than 1700° C. until at least about a 40% reduction in the cross-sectional area of the rod is achieved.
9. The method of claim 8 wherein the rolling is performed by multiple passes.
10. The method of claim 8 wherein at least about a 70% reduction in cross-sectional area is achieved.
11. The method of claim 8 wherein the rod after rolling has a UTS of from about 70 to about 85 ksi, a YS of from about 60 to about 80 ksi and a hardness of from about 40 to about 43 Rockwell C.
12. The method of claim 11 wherein the tungsten-lanthana rod contains from 0.3 to 2.5 weight percent lanthana.
13. The method of claim 8 wherein the rod is stress relieved at a point between 25 and 45% reduction in cross-sectional area.
14. The method of claim 8 wherein the rod is stress relieved after rolling.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11043352B1 (en) 2019-12-20 2021-06-22 Varex Imaging Corporation Aligned grain structure targets, systems, and methods of forming

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* Cited by examiner, † Cited by third party
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CN107190195A (en) * 2017-05-04 2017-09-22 鹤山市沃得钨钼实业有限公司 A kind of W-REO alloys crucible and its manufacture method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3086103A (en) * 1961-03-28 1963-04-16 Union Carbide Corp Refractory electrode-inert gas shielded-arc working
US3159908A (en) * 1963-02-26 1964-12-08 Du Pont Dispersion hardened metal product and process
US4923673A (en) * 1988-10-17 1990-05-08 Gesellschaft Fur Wolfram-Industrie Mbh Method for producing alloyed tungsten rods
US4950327A (en) * 1987-01-28 1990-08-21 Schwarzkopf Development Corporation Creep-resistant alloy of high-melting metal and process for producing the same
US5051139A (en) * 1989-05-03 1991-09-24 Schwarzkopf Development Corporation Process for the manufacture of semi-finished products or preformed parts made of refractory metals and resistant to thermal creep
US5590386A (en) * 1995-07-26 1996-12-31 Osram Sylvania Inc. Method of making an alloy of tungsten and lanthana
US5604321A (en) * 1995-07-26 1997-02-18 Osram Sylvania Inc. Tungsten-lanthana alloy wire for a vibration resistant lamp filament

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3086103A (en) * 1961-03-28 1963-04-16 Union Carbide Corp Refractory electrode-inert gas shielded-arc working
US3159908A (en) * 1963-02-26 1964-12-08 Du Pont Dispersion hardened metal product and process
US4950327A (en) * 1987-01-28 1990-08-21 Schwarzkopf Development Corporation Creep-resistant alloy of high-melting metal and process for producing the same
US4923673A (en) * 1988-10-17 1990-05-08 Gesellschaft Fur Wolfram-Industrie Mbh Method for producing alloyed tungsten rods
US5051139A (en) * 1989-05-03 1991-09-24 Schwarzkopf Development Corporation Process for the manufacture of semi-finished products or preformed parts made of refractory metals and resistant to thermal creep
US5590386A (en) * 1995-07-26 1996-12-31 Osram Sylvania Inc. Method of making an alloy of tungsten and lanthana
US5604321A (en) * 1995-07-26 1997-02-18 Osram Sylvania Inc. Tungsten-lanthana alloy wire for a vibration resistant lamp filament
US5742891A (en) * 1995-07-26 1998-04-21 Osram Sylvania Inc. Tungsten-lanthana alloy wire for a vibration resistant lamp filament

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11043352B1 (en) 2019-12-20 2021-06-22 Varex Imaging Corporation Aligned grain structure targets, systems, and methods of forming

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