US20040166017A1 - Age-hardening copper-base alloy and processing - Google Patents

Age-hardening copper-base alloy and processing Download PDF

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Publication number
US20040166017A1
US20040166017A1 US10/657,005 US65700503A US2004166017A1 US 20040166017 A1 US20040166017 A1 US 20040166017A1 US 65700503 A US65700503 A US 65700503A US 2004166017 A1 US2004166017 A1 US 2004166017A1
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alloy
copper
hours
reduction
electrical conductivity
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Inventor
Ronald Caron
Peter Robinson
Derek Tyler
Andreas Boegel
Doris Humpenoder-Bogel
Hans-Achim Kuhn
Joerg Seeger
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Wieland Werke AG
GBC Metals LLC
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Wieland Werke AG
Olin Corp
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Priority to TW092125248A priority patent/TW200422410A/zh
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Publication of US20040166017A1 publication Critical patent/US20040166017A1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Definitions

  • This invention relates to an age-hardening copper-base alloy and a processing method to make commercially useful products from that alloy. More particularly, a copper alloy containing from 0.35% to 5%, by weight, titanium is wrought to finish gauge by a process that includes an in-process solution anneal and at least one age anneal. The resultant product has an electrical conductivity in excess of 50% IACS and a yield strength in excess of 105 ksi.
  • compositions are in weight percent and all mechanical and electrical testing was performed at room temperature (nominally 22° C.), unless otherwise specified.
  • the word “about” implies ⁇ 10% and the word “base” as in copper-base, means the alloy contains at least 50%, by weight, of the specified base element.
  • the terms “rolling” or “rolled” are intended to encompass drawing or drawn or any other form of cold reduction, for example, as used in the manufacture and processing of wire, rod or tubing.
  • Target values for these properties and the relative importance of the properties are dependent on the intended application of products manufactured from the subject copper alloys.
  • the following property descriptions are generic for many intended applications, but the target values are specific for under the hood automotive applications.
  • the yield strength is the stress at which a material exhibits a specified deviation, typically an offset of 0.2%, from proportionality of stress and strain. This is indicative of the stress at which plastic deformation becomes dominant with respect to elastic deformation. It is desirable for copper alloys utilized as connectors to have a yield strength of at least 105 ksi, that is at least approximately 724 MPa.
  • Copper based electrical connectors must maintain above a threshold contact force on a mating member for prolonged times for good electrical connection. Stress relaxation reduces the contact force to below the threshold leading to an open circuit. It is desirable for a copper alloy for connector applications to maintain at least 95% of the initial stress when exposed to a temperature of 105° C. for 1000 hours and to maintain at least 85% of the initial stress when exposed to a temperature of 150° C. for 1000 hours.
  • the modulus of elasticity also known as Young's modulus, is a measure of the rigidity or stiffness of a metal and is the ratio of stress to corresponding strain in the elastic region. Since the modulus of elasticity is a measure of the stiffness of a material, a high modulus, on the order of 140 Gpa (20 ⁇ 10 3 ksi) is desirable.
  • MBR minimum bend radius
  • Bend formability may be expressed as, MBR/t, where t is the thickness of the metal strip.
  • MBR/t is a ratio of the minimum radius of curvature of a mandrel about which the metallic strip can be bent without failure to the thickness of the strip.
  • the “mandrel” test is specified in ASTM (American Society for Testing and Materials) designation E290-92, entitled Standard Test Method for Semi - Guided Bend Test for Ductility of Metallic Materials , and is incorporated by reference in its entirety herein.
  • the MBR/t prefferably isotropic, a similar value in the “good way”, bend axis perpendicular to the rolling direction of the metallic strip, as well as the “bad way”, bend axis parallel to the rolling direction of the metallic strip. It is desirable for the MBR/t to be about 1.5 or less for a 90° bend and about 2 or less for a 180° bend.
  • the bend formability for a 90° bend may be evaluated utilizing a block having a V-shaped recess and a punch with a working surface having a desired radius.
  • a strip of the copper alloy in the temper to be tested is disposed between the block and the punch and when the punch is driven down into the recess, the desired bend is formed in the strip.
  • V-block method related to the V-block method is the 180° “form punch” method in which a punch with a cylindrical working surface is used to shape a strip of copper alloy into a 180° bend.
  • both methods give quantifiable bendability results and either method may be utilized to determine relative bendability.
  • the ultimate tensile strength is a ratio of the maximum load a strip withstands before failure during a tensile test divided by the initial cross-sectional area of the strip. It is desirable for the ultimate tensile strength to be about 110 ksi, that is approximately 760 MPa.
  • Electrical conductivity is expressed in % IACS (International Annealed Copper Standard) in which unalloyed copper is defined as having an electrical conductivity of 100% IACS at 20° C.
  • Copper-base alloys containing titanium are disclosed in U.S. Pat. Nos. 4,601,879 and 4,612,167, among others.
  • The, 4,601,879 patent discloses a copper-base alloy containing 0.25% to 3.0% of nickel, 0.25% to 3.0% of tin and 0.12% to 1.5% of titanium.
  • Exemplary alloys have an electrical conductivity of between 48.5% and 51.4% IACS and a yield strength of between 82.5 ksi and 84 ksi.
  • the 4,612,167 patent discloses a copper alloy containing 0.8% to 4.0% of nickel and 0.2% to 4.0% of titanium. Exemplary alloys have an electrical conductivity of 51% IACS and a yield strength of 96.2 ksi to 98.5 ksi. Both the 4,601,879 patent and the 4,612,167 patent are incorporated by reference in their entireties herein.
  • AMAX Copper, Inc. (Greenwich, Conn.) has commercialized copper-nickel-titanium alloys having nominal compositions of Cu-2% Ni-1% Ti and Cu-5% Ni-2.5% Ti.
  • the reported properties for the Cu-2% Ni-1% Ti alloy are yield strength 64-80 ksi; ultimate tensile strength 73-95 ksi; elongation 9%; and electrical conductivity 50-60% IACS.
  • the reported properties for the Cu-5% Ni-2.5% Ti alloy are yield strength 90-100 ksi; ultimate tensile strength 108 ksi UTS; elongation 10%; and electrical conductivity 40-53% IACS.
  • an age-hardening copper-base alloy and methods to process this alloy to form a commercially useful product for any application requiring high yield strength and moderately high electrical conductivity.
  • Typical forms for the product include strip, plate, wire, foil, tube, powder or cast form.
  • the alloys when processed according to the methods of the invention achieve a yield strength of at least 105 ksi and an electrical conductivity of 50% IACS making the alloys particularly suited for use in electrical connectors and interconnections.
  • the alloys consisting essentially of, by weight, from 0.35% to 5% titanium, from 0.001% to 10% of X, where X is selected from Ni, Fe, Sn, P, Al, Zn, Si, Pb, Be, Mn, Mg, Bi, S, Te, Se, Ag, As, Sb, Zr, B, Cr and Co and combinations thereof and the balance is copper and inevitable impurities.
  • the alloy has an electrical conductivity of at least 50% IACS and a yield strength of at least 105 ksi.
  • the alloy consists essentially of from 0.35% to 2.5% titanium, from 0.5% to 5.0% nickel, from 0.5% to 0.8% of iron, cobalt and mixtures thereof, from 0.01% to 1.0% magnesium, up to 1% of Cr, Zr, Ag and combinations thereof and the balance is copper and inevitable impurities.
  • FIG. 1 illustrates in flow chart format a first method for processing the copper alloys of the invention.
  • FIG. 2 illustrates in flow chart format a second method for processing the copper alloys of the invention.
  • FIG. 3 illustrates in flow chart format a third method for processing the copper alloys of the invention.
  • Copper alloys having a combination of strength and electrical conductivity, as well as good formability and a resistance to stress relaxation are in demand for many electrical current carrying applications.
  • Two exemplary applications are under-the-hood automotive applications and multimedia applications (such as computers, DVD players, CD readers and the like).
  • the alloy compositions when processed by the methods of this invention surprisingly provide an optimum combination of properties for meeting the needs for both automotive and multimedia applications, as well as other electrical and electronic applications.
  • the alloys can provide moderately high strength along with high conductivity and moderately high conductivity along with very high strength.
  • the alloys of the present invention have compositions containing Cu—Ti—X, where X is selected from Ni, Fe, Sn, P, Al, Zn, Si, Pb, Bi, S, Te, Se, Be, Mn, Mg, Ag, As, Sb, Zr, B, Cr and Co and combinations thereof.
  • X is selected from Ni, Fe, Sn, P, Al, Zn, Si, Pb, Bi, S, Te, Se, Be, Mn, Mg, Ag, As, Sb, Zr, B, Cr and Co and combinations thereof.
  • the titanium content is from 0.35% to 5% and the sum total of the “X” elements is from 0.001% to 10%.
  • Oxygen, sulfur and carbon may be present in the alloys of the invention in amounts typically found in either electrolytic (cathode) copper or remelted copper or copper alloy scrap. Typically, the amount of each of these elements will be in the range of from about 2 ppm to about 50 ppm and preferably, each is present in an amount of less than 20 ppm.
  • additions that influence the properties of the alloy may also be included.
  • Such additions include those that improve the free machinability of the alloy, such as bismuth, lead, tellurium, sulfur and selenium. When added to enhance free machinability, these additions may be present in an amount of up to 2%. Preferably, the total of free machinability additions is between about 0.8% and 1.5%.
  • Typical impurities found in copper alloys may be present in an amount of up to about 1%, in total.
  • such impurities include magnesium, aluminum, silver, silicon, cadmium, bismuth, manganese, cobalt, germanium, arsenic, gold, platinum, palladium, hafnium, zirconium, indium, antimony, chromium, vanadium, and beryllium.
  • Each impurity should be present in an amount of less than 0.35%, and preferably in an amount of less than 0.1%.
  • the titanium content is from 0.35% to 2.5% and in a most preferred embodiment, the titanium content is from 0.8% to 1.4%
  • “X” should preferably be effective to cause titanium to precipitate from solution during an age anneal.
  • Suitable elements for “X” to enhance such precipitation include Ni, Fe, Sn, P, Al, Si, S, Mg, Cr, Co and combinations of these elements.
  • One preferred addition is nickel.
  • a combination of Ni and Ti provides precipitates of CuNiTi and the presence of Fe and Ti provides precipitates of Fe 2 Ti.
  • Another preferred addition is magnesium.
  • An addition of Mg increases stress relaxation resistance and softening resistance in finished gauge and temper products.
  • the Mg also provides softening resistance during in-process aging annealing heat treatments.
  • One preferred alloy in accordance with the invention that has an improved combination of yield strength, electrical conductivity, stress relaxation resistance, along with modest levels of bendability consists essentially of
  • the optional elements comprise up to 1% of one or more of Cr, Zr and Ag.
  • the alloy composition and processing provide a yield strength of at least about 115 ksi and preferably a yield strength of at least about 120 ksi.
  • the conductivity is up to about 40% IACS.
  • the composition and processing provide a yield strength of more than about 105 ksi, and preferably up to about 115 ksi.
  • the electrical conductivity of the alloy is preferably from about 45% to about 55% IACS.
  • the composition and processing provide a yield strength of from about 80 ksi to about 100 ksi and the electrical conductivity is between about 55% and about 65% IACS.
  • FIG. 1 illustrates in flow chart format, a process in accordance with a first embodiment of the invention.
  • the alloy of the invention is melted and cast 10 in accordance with conventional practice.
  • the cast alloy is hot rolled 12 at from about 750° C. to about 1,000° C.
  • the alloy is then cold rolled 14 to a reduction in cross-sectional area transverse to the rolling direction (“reduction in area”) of from about 50% to about 99%.
  • the alloy may then be solutionized 16 at a solution annealing temperature of from about 850 to about 1,000° C. for from about 10 seconds to about one hour, followed by a quench 18 or rapid cool to ambient temperature to obtain equiaxed grains with an average grain size of about 5 and 20 ⁇ m.
  • the alloy may be first cold rolled 20 up to about 80% reduction in area, preferably about 30% to about 80% reduction in area.
  • the first cold roll 20 is followed by a first anneal 22 at a temperature of from about 400° C. to about 650° C. and preferably from about 450° C. to about 600° C. for from about 1 minute to about 10 hours and preferably from about 1 to about 8 hours.
  • the alloy is then second cold rolled 24 from about a 10% to about a 50% reduction in area to finished gauge.
  • the second cold roll may be followed by a second anneal 26 at about 150° C. to about 600° C. and preferably from about 200° C. to about 500° C. for from about 15 seconds to about 10 hours.
  • the alloy is processed to finished gauge without using an in-process solutionizing heat treatment. That is, it can be processed to finish using cycles of lower temperature annealing treatments and intervening cold work. This alternative process is especially useful for making a product with higher electrical conductivity levels.
  • FIG. 2 illustrates in flow chart representation an alternative process of the invention.
  • the alloy of the invention is melted and cast 10 in accordance with conventional practice.
  • the cast alloy is hot rolled 12 at from about 750° C. to about 1,000° C. and then quenched or quickly cooled. After milling to remove oxide, the hot rolled alloy is then cold rolled 14 to a reduction in area of from about 50% to about 99%.
  • the alloy may then be first annealed 28 at an annealing temperature of from about 400° C. to about 650° C. for from about 15 secs. to about 10 hours.
  • the cold rolling and first annealing steps may optionally be repeated, if desired
  • the alloy is then cold rolled 30 from about 40% to about 80% reduction in area followed by a second anneal 32 at from about 400° C. to about 650° C. and preferably from about 450° C. to about 600° C. for from about 1 to about 10 hours.
  • the alloy is then cold rolled 34 from about a 10% to about a 50% reduction in area to finished gauge. This may optionally be followed by a third anneal 26 at about 150° C. to about 600° C. and preferably from about 200° C. to about 500° C. for from about 15 seconds to about 10 hours.
  • a second alternative preferred embodiment of the process of this invention employs an alloy in the preferred composition ranges.
  • This process is capable of making the alloy of this invention with nominal properties of about 110 ksi YS and about 50% IACS conductivity.
  • the alloy is melted and cast 10 in accordance with conventional practice.
  • the cast alloy is hot rolled 12 at from about 750° C. to about 1,000° C. After milling to remove oxide the hot rolled alloy is then cold rolled 14 to a reduction in area of from about 50% to about 99%.
  • the alloy is then solutionized 16 at a temperature of from about 950° C. to about 1,000° C. for from about 15 seconds to about 1 hour.
  • the alloy is next cold rolled 20 to from about a 40% to about a 60% reduction in area and then first annealed 28 at about 400° C. to about 650° C. and preferably 450° C. to about 600° C. for from about 1 to about 10 hours and preferably from about 1 to about 3 hours.
  • the first anneal 28 is followed by cold rolling 30 from about a 40% to about a 60% reduction in area.
  • the alloy is then second annealed 32 at a lower temperature than the first anneal 28.
  • the second anneal is at a temperature of from about 375° C. to about 550° C. for from about 1 to about 3 hrs.
  • the doubly annealed alloy is then cold rolled 34 at least about 30% reduction in area to a finished gauge where it may be annealed a third time 26 at a temperature of from about 150° C. to about 600° C. and preferably from about 200° C. to about 500° C. for from about 1 to about 3 hours.
  • the alloys were cold rolled to 0.050′′.
  • the alloys were then solutionized at a temperature of 1000° C. for from 20 to 60 seconds, with the exception of alloy J346 which was solutionized at 950° C. for 60 seconds.
  • the alloys were cold rolled 50% to 0.025′′ and age annealed at 550° C. for 3 hours
  • the alloys were then cold rolled 50% to 0.0125′′ gauge and relief annealed at 275° C. for 2 hours and the properties reported in Table 2 measured.
  • the alloys of Table 1 were processed as in Example 1 up through the homogenization heat treatment at hot rolled plate gauge.
  • the alloys were processed to finish gauge without an in-process solutionizing heat treatment.
  • the alloys were cold rolled to 0.100′′ and given a first aging anneal at 550° C. for 3 hours.
  • the alloys were then cold rolled 70% to 0.030′′ and subjected to a second aging anneal at 525° C. for 3 hours.
  • the alloys were then cold rolled 50% to 0.015′′ gauge and relief annealed 275° C. for 2 hrs in which condition the properties recited in Table 3 were measured.
  • alloys other than J477 were then solution heat treated at 1,000° C. for 25 seconds followed by a water quench to yield a controlled, fine, recrystallized grain size in the range 12-24 ⁇ m in diameter. Alloy J477 was solution heat treated at 950° C./25 secs+WQ, yielding a grain size of 9 ⁇ m.
  • the alloys of Table 4 were processed to finish gauge without using an in-process solutionizing heat treatment. After trimming and milling to remove the oxide coating, the alloys in the as hot rolled condition were cold rolled to 0.050′′ gauge and given a first aging anneal at a temperature and time as shown in Table 6 effective to maximize electrical conductivity. The alloys were then cold rolled 50% to 0.025′′ gauge and subjected to a second aging anneal at a temperature and time as shown in Table 6 selected to maximize the conductivity without unduly softening the matrix. The specific aging anneals applied to each alloy are noted in Table 6.
  • the alloys were then cold rolled 50% to 0.0125′′ gauge and relief annealed at 275° C. for 2 hrs. at which condition the properties in Table 7 were measured. Using this process, the alloys with Fe and Mg additions provide lower, but still good, strength with higher electrical conductivity and good stress relaxation resistance.
  • Comparing baseline alloy J694 to zirconium containing alloy J698 demonstrates that a small amount of zirconium increases the yield strength without affecting electrical conductivity.
  • a comparison of alloy J694 with silver containing alloy J699 demonstrates that a small amount of silver increases both the yield strength and the electrical conductivity.
  • a comparison of alloy J694 with chromium containing alloy J700 demonstrates that an addition of a small amount of chromium increases the yield strength slightly with a slight penalty in electrical conductivity.

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JP2005539140A (ja) 2005-12-22
CN1688732B (zh) 2010-05-26
JP4590264B2 (ja) 2010-12-01
CA2497819A1 (fr) 2004-03-25
EP1537249A4 (fr) 2007-07-11
TW200422410A (en) 2004-11-01
EP1537249A2 (fr) 2005-06-08
CN1688732A (zh) 2005-10-26
AU2003272276A1 (en) 2004-04-30
WO2004024964A2 (fr) 2004-03-25
JP2010275640A (ja) 2010-12-09
AU2003272276A8 (en) 2004-04-30
KR20050050654A (ko) 2005-05-31
WO2004024964A3 (fr) 2004-07-01
MXPA05002640A (es) 2005-07-19
EP1537249B1 (fr) 2014-12-24

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