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EP0282204A1 - Shaped body formed of copper-beryllium alloy and method of manufacturing same - Google Patents

Shaped body formed of copper-beryllium alloy and method of manufacturing same Download PDF

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Publication number
EP0282204A1
EP0282204A1 EP88301618A EP88301618A EP0282204A1 EP 0282204 A1 EP0282204 A1 EP 0282204A1 EP 88301618 A EP88301618 A EP 88301618A EP 88301618 A EP88301618 A EP 88301618A EP 0282204 A1 EP0282204 A1 EP 0282204A1
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Prior art keywords
alloy
rolled sheet
formability
cold rolling
aging
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EP88301618A
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German (de)
French (fr)
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EP0282204B1 (en
Inventor
Yosuke Matsui
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NGK Insulators Ltd
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NGK Insulators Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing 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

  • the present invention relates to technology for manufacturing a shaped body which comprises Be-Cu alloy material.
  • Be-Cu alloy is widely used as an excellent raw material with high mechanical strength and electrical conductivity.
  • a Be-Cu alloy material having a suf­ficient formability to withstand severe working conditions.
  • the first mode is to subject the rolled sheet of the Be-Cu alloy to a subsequent age hardening, and deliver the material to customers as a so-called mill hardened material.
  • the material is then subjected to various works, including bending into the desired configuration of a parts body in the factory of the customer. In many cases, the shaped parts body so obtained is incorporated into the products as it is.
  • the second mode is to deliver to customers the rolled sheet of the Be-Cu alloy which is then subjected to various works into the desired configuration of a parts body in the factory of the customer, and subsequently to an age hardening in the factory of either the customer or the raw material supplier, to form a complete parts body with a desired strength.
  • the cold rolling to be effected after the solution treatment is a parameter dominantly influential on the characteristics of the material, and is intended to improve the product strength, to prevent the deformation of the material after the aging, and to promote the age precipitation.
  • the material already subjected to the age hardening as a mill hardened material
  • the material with a higher post aging strength has a decreased elongation, an inferior formability and markedly degraded freedom degree of bending.
  • the preservation of the desired formability of Be-Cu alloy could be achieved only with the sacrifice of the fundamental feature of the alloy, i.e. the excellent high strength.
  • An object of the present invention is to improve the Be-Cu alloy material, with an originally degraded formability as a result of the cold rolling with the reduction of 20% or more, such that the material is capable of withstanding a bending with a smaller radius of curvature during the shaping into the desired configuration of a parts body, and to readily realize the maximum post aging strength of the Be-Cu alloy which has already been shaped into the desired configuration.
  • a solution treatment is carried out with respect to a rolled Be-Cu alloy sheet including 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu.
  • This sheet is subjected to a cold rolling with a reduc­tion of 20% or more, and the cold rolled sheet is subjected to an annealing at a temperature of 250 to 550°C to recover the formability of the Be-Cu alloy material.
  • the so-obtained material is subjected to necessary works, including bending into a predetermined configuration of the parts body, and then to an aging at a temperature of 350-500°C, thereby to realize the maximum post aging strength.
  • the cold rolling carried out after the solution treatment is followed by an annealing at a predetermined temperature thereby to release part of the work strain and to recover the formability, and the so-obtained Be-Cu alloy material with an improved formability is then shaped into the desired configura­tion of the parts body and subjected to an age hardening, whereby it becomes possible to produce products with a desired high strength.
  • Be-Cu alloy which includes 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu.
  • the amount of Be has been defined as ranging from 0.2 to 0.8 wt%.
  • the amount of Ni and/or Co has been defined as ranging from 0.3 to 4.0 wt%.
  • the rolled sheet of Be-Cu alloy with the above-mentioned composition is subjected to a cold rolling, following the solution treatment, with the reduction of 20% or more.
  • a cold rolling following the solution treatment, with the reduction of 20% or more.
  • the present invention defines the temperature range of 250 to 550°C due to the reason that the temperature below 250°C does not result in a sufficient recovery of the formability, on one hand, while the temperature above 550°C results in an excessively aged state whereby a sufficiently high strength cannot be achieved through the age hardening after the shaping into the desired configuration, on the other hand.
  • the present invention defines the temperature range of 350 to 500°C due to the reason that the temperature below 350°C does not induce the precipitation hardening, on one hand, and the tempera­ture above 500°C, though effective to improve the electrical conductivity, results in an excessively aged state whereby a sufficient strength cannot be achieved, on the other hand.
  • R/t value The formability as mentioned in Table 1 has been determined with respect to rolled sheets of Be-Cu alloy prior to the age hardening step, and is expressed as R/t value, where R is a safety bending radius determined by whether or not cracks are formed in the bent portion of the sheet after it has been bent by 180° about an axis in parallel with the rolling direction, and t is the thickness of the sheet by which the safety bending radius is divided.
  • R is a safety bending radius determined by whether or not cracks are formed in the bent portion of the sheet after it has been bent by 180° about an axis in parallel with the rolling direction
  • t the thickness of the sheet by which the safety bending radius is divided.
  • a smaller R/t value indicates that the sheet is capable of withstanding a more severe work conditions including bending with a smaller bending radius.
  • the annealing has been carried out at a higher temperature so that the precipitation nuclei became coarse accompanying decrease in the post aging 0.2% yield strength.
  • the annealing has been carried out under a lower temperature so that is was not possible to achieve a sufficient recovery of the formability after the annealing.
  • the comparative sample (21) exhibits an excessively aged state as a result of aging under a higher temperature, while the comparative sample (22) is in a non-aged state due to the aging treatment under a lower temperature; for both of these samples the post aging 0.2% yield strength has decreased.
  • the cold rolling following the solution treatment is carried out with a higher value such as to improve the post aging strength and to prevent post aging deformations in an effective manner. Also, the degradation of the formability, which has hitherto been considered inevitable, can be prevented positively by the annealing at a predetermined temperature.
  • the solution treatment can be carried out with respect to the sheet of a greater thickness.
  • the solution treatment can be effected with respect to the sheet of 1.0 mm thickness.
  • the shape of the sheet can be properly corrected and also the aging precipita­tion can be more or less prompted, so that it is possible to prevent undesirable shrinkage arising during the aging after the material has been worked into the configuration of the parts body.

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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)
  • Conductive Materials (AREA)
  • Metal Rolling (AREA)
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Abstract

In manufacturing shaped parts of various products, such as relays and connectors, of Cu-Be alloy material, the aim is improved formability to withstand severe working conditions. Known processes include a solution treatment of a rolled sheet of Cu-Be alloy material followed by a cold rolling with a relatively low reduction; this suffers from degradation of the formability of the material. Also, mill-hardened Cu-Be alloy material subjected to an age hardening is dis­advantageous in that desired formability of the alloy cannot be achieved without sacrifice of strength.
The invention enables the recovery of the formability of the material by subjecting a rolled sheet of the Cu-Be alloy containing 0.2-0.8 wt% Be and 0.3-4.0 wt% Ni and/or Co to a solution treatement and cold rolling of 20% reduction or more, followed by annealing at 250-550°C. A high post aging strength of the material shaped into the desired configuration is then achieved by subjecting the shaped material to aging at 350-500°C.

Description

  • The present invention relates to technology for manufacturing a shaped body which comprises Be-Cu alloy material.
  • For manufacturing various products such as relays and connectors, Be-Cu alloy is widely used as an excellent raw material with high mechanical strength and electrical conductivity. In view of the recent progressive needs for products of small size, there is the demand for a Be-Cu alloy material having a suf­ficient formability to withstand severe working conditions.
  • It has been a conventional practice to produce a rolled sheet of Be-Cu alloy to be worked into a shaped parts body with a predetermined configuration, by casting and hot rolling the raw material, subjecting the hot rolled material repeatedly to cold rolling and annealing, and then to a subsequent solution treatment followed by a further cold rolling. Moreover, the above-mentioned rolled sheet of Be-Cu alloy is worked into the desired configuration of a parts body in either one of the following modes.
  • The first mode is to subject the rolled sheet of the Be-Cu alloy to a subsequent age hardening, and deliver the material to customers as a so-called mill hardened material. The material is then subjected to various works, including bending into the desired configuration of a parts body in the factory of the customer. In many cases, the shaped parts body so obtained is incorporated into the products as it is.
  • The second mode is to deliver to customers the rolled sheet of the Be-Cu alloy which is then subjected to various works into the desired configuration of a parts body in the factory of the customer, and subsequently to an age hardening in the factory of either the customer or the raw material supplier, to form a complete parts body with a desired strength.
  • In both modes, the cold rolling to be effected after the solution treatment is a parameter dominantly influential on the characteristics of the material, and is intended to improve the product strength, to prevent the deformation of the material after the aging, and to promote the age precipitation.
  • In effecting the cold rolling subsequently after the solution treatment, an excessively high reduction results in a degradation in 90° bending characteristic of the rolled sheet when bent about an axis that is in parallel with the rolling direction; hence, even when the rolled sheet is shaped into the configuration of a parts body prior to the age hardening, a sufficient freedom degree of the shaping cannot be achieved. Consequently, for a material exhibiting an outstanding tendency of work hardening, the cold rolling is usually carried out with the reduction of no greater than 60%. In other words, it has been considered necessary to increase the number of repetition of the cold rolling and the annealing prior to the solution treatment, and this results in difficulties in lowering the manufacturing cost.
  • On the other hand, for the material already subjected to the age hardening as a mill hardened material, the material with a higher post aging strength has a decreased elongation, an inferior formability and markedly degraded freedom degree of bending. Thus, the preservation of the desired formability of Be-Cu alloy could be achieved only with the sacrifice of the fundamental feature of the alloy, i.e. the excellent high strength.
  • An object of the present invention is to improve the Be-Cu alloy material, with an originally degraded formability as a result of the cold rolling with the reduction of 20% or more, such that the material is capable of withstanding a bending with a smaller radius of curvature during the shaping into the desired configuration of a parts body, and to readily realize the maximum post aging strength of the Be-Cu alloy which has already been shaped into the desired configuration.
  • According to the present invention, a solution treatment is carried out with respect to a rolled Be-Cu alloy sheet including 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu. This sheet is subjected to a cold rolling with a reduc­tion of 20% or more, and the cold rolled sheet is subjected to an annealing at a temperature of 250 to 550°C to recover the formability of the Be-Cu alloy material. The so-obtained material is subjected to necessary works, including bending into a predetermined configuration of the parts body, and then to an aging at a temperature of 350-500°C, thereby to realize the maximum post aging strength.
  • There is shown in the sole Figure a flow chart of the production steps wherein the present invention is compared with the above-mentioned prior art. Conven­tionally, either the cold rolled sheet obtained after the solution treatment of the Be-Cu alloy is directly subjected to shaping into the desired configuration and to a subsequent age hardening, or the mill hardened material obtained after the advance age hardening is subjected to shaping into the configuration of the product. As mentioned hereinbefore, such production steps accompany a variety of problems.
  • In contrast to the above, according to the present invention, the cold rolling carried out after the solution treatment is followed by an annealing at a predetermined temperature thereby to release part of the work strain and to recover the formability, and the so-obtained Be-Cu alloy material with an improved formability is then shaped into the desired configura­tion of the parts body and subjected to an age hardening, whereby it becomes possible to produce products with a desired high strength.
  • According to the present invention, as mentioned hereinbefore, use is made of Be-Cu alloy which includes 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu. These limitations on each of the components are based on the following reasons.
  • First of all, it has been found that with the amount of Be of less than 0.2 wt% a sufficient precipitation hardening cannot be achieved, while when the amount of Be exceeds 0.8 wt% an improvement in the strength in conformity with the increased amount cannot be recognized; hence, the amount of Be has been defined as ranging from 0.2 to 0.8 wt%.
  • Secondly, it has also been found that with the amount of Ni and/or Co of less than 0.3 wt% a sufficient precipitation hardening cannot be achieved, while when the amount of Ni and/or Co exceeds 4.0 wt% the form­ability degrades; hence, the amount of Ni and/or Co has been defined as ranging from 0.3 to 4.0 wt%.
  • According to the present invention, the rolled sheet of Be-Cu alloy with the above-mentioned composition is subjected to a cold rolling, following the solution treatment, with the reduction of 20% or more. This is due to recognition that, with a reduction of less than 20%, the formability does not undergo a significant degradation and does not require the recovery by the annealing, while a higher reduction makes it possible to reduce the number of repetition of the cold rolling and annealing in advance of the solution treatment.
  • Moreover, for effecting the annealing between the cold rolling step following the solution treatment and the working step for shaping the material into the desired configuration of the parts body, the present invention defines the temperature range of 250 to 550°C due to the reason that the temperature below 250°C does not result in a sufficient recovery of the formability, on one hand, while the temperature above 550°C results in an excessively aged state whereby a sufficiently high strength cannot be achieved through the age hardening after the shaping into the desired configuration, on the other hand.
  • Furthermore, for effecting age hardening following the shaping into the desired parts body configuration, the present invention defines the temperature range of 350 to 500°C due to the reason that the temperature below 350°C does not induce the precipitation hardening, on one hand, and the tempera­ture above 500°C, though effective to improve the electrical conductivity, results in an excessively aged state whereby a sufficient strength cannot be achieved, on the other hand.
  • EXAMPLES
  • There is shown, in the following Table 1, the compositions, production conditions and mechanical properties of samples (1) to (16) of the present invention and comparative samples (17) to (24).
    Figure imgb0001
    Figure imgb0002
  • The samples (1) to (24) listed in Table 1 have been produced in a known manner up to the solution treatment step in the process shown in the Figure, and subsequently under respectively different process conditions.
  • The formability as mentioned in Table 1 has been determined with respect to rolled sheets of Be-Cu alloy prior to the age hardening step, and is expressed as R/t value, where R is a safety bending radius determined by whether or not cracks are formed in the bent portion of the sheet after it has been bent by 180° about an axis in parallel with the rolling direction, and t is the thickness of the sheet by which the safety bending radius is divided. Here, a smaller R/t value indicates that the sheet is capable of withstanding a more severe work conditions including bending with a smaller bending radius.
  • As Table 1 clearly shows, all the samples (1) to (16) of the present invention exhibit excellent form­ability and strength (post aging 0.2% yield strength obtained in accordance with JIS Z2241). On the other hand, the comparative samples (17), (19) and (21) are of the same composition as the samples (5) to (8) of the present invention, while the comparative samples (18), (20) and (22) are of the same composition as the samples (10) and (11) of the present invention.
  • With respect to the comparative samples (17) and (18), the cold rolling has been carried out with a smaller reduction. It is apparent that, with the reduction of 15%, an excellent formability can be achieved though the post aging 0.2% yield strength becomes much lower as compared with the corresponding samples of the present invention having the same composition.
  • With respect to the comparative sample (19), the annealing has been carried out at a higher temperature so that the precipitation nuclei became coarse accompanying decrease in the post aging 0.2% yield strength. As to the comparative sample (20), the annealing has been carried out under a lower temperature so that is was not possible to achieve a sufficient recovery of the formability after the annealing.
  • The comparative sample (21) exhibits an excessively aged state as a result of aging under a higher temperature, while the comparative sample (22) is in a non-aged state due to the aging treatment under a lower temperature; for both of these samples the post aging 0.2% yield strength has decreased.
  • Furthermore, a sufficient strength could not be achieved for the comparative samples (23) and (24) due to insufficient content of Be or Co, respectively.
  • Another samples have been prepared to have the same composition as the samples (10) and (11) of the present invention, and these samples were subjected to cold rolling with the variable reduction of 20 to 90%, to a subsequent annealing at the temperature of 400°C followed by the measurement of the formability, and then to an aging at the temperature of 400°C followed by the measurement of the 0.2% yield strength. The result is as shown in the following Table 2.
    Figure imgb0003
  • As is apparent from Table 2, a higher reduction of the cold rolling results in a degradation of the formability which, in accordance with the present invention, can be recovered to a practically high R/t value by effecting the annealing.
  • It will be appreciated that, in accordance with the present invention, the cold rolling following the solution treatment is carried out with a higher value such as to improve the post aging strength and to prevent post aging deformations in an effective manner. Also, the degradation of the formability, which has hitherto been considered inevitable, can be prevented positively by the annealing at a predetermined temperature.
  • Furthermore, with the higher reduction of the cold rolling following the solution treatment, the solution treatment can be carried out with respect to the sheet of a greater thickness. As an example, in case of the reduction of 80% and the final product thickness of 0.2 mm, the solution treatment can be effected with respect to the sheet of 1.0 mm thickness. Hence, it is possible to reduce the number of repetition of the cold rolling and the annealing in advance of the solution treatment, as compared with the cold rolling in the conventional process with a lower reduction, and to thereby achieve a substantial economical advantage.
  • Moreover, when the annealing is effected with respect to a constrained sheet, the shape of the sheet can be properly corrected and also the aging precipita­tion can be more or less prompted, so that it is possible to prevent undesirable shrinkage arising during the aging after the material has been worked into the configuration of the parts body.

Claims (2)

1. A shaped body comprising a Be-Cu alloy material with a predetermined configuration, said shaped parts body being produced by a process which comprises the steps of:
      preparing a rolled sheet of Be-Cu alloy which includes 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu;
      subjecting said rolled sheet to a solution treatment;
      cold rolling said rolled sheet with a reduction of 20% or more;
      subjecting the cold rolled sheet to an annealing at a temperature of 250 to 550°C to form a Be-Cu alloy raw material;
      working, including bending, the so-obtained alloy raw material into a predetermined parts body configuration; and
      aging the worked alloy material at a temperature of 350 to 500°C.
2. A method of manufacturing a shaped body comprising a Be-Cu alloy material with a pre­determined configuration, the method comprising the steps of:
      preparing a rolled sheet of Be-Cu alloy which includes 0.2 to 0.8 wt% Be, 0.3 to 4.0 wt% Ni and/or Co, the balance consisting essentially of Cu;
      subjecting said rolled sheet to a solution treatment;
      cold rolling said rolled sheet with a reduction of 20% or more;
      subjecting the cold rolled sheet to an annealing at a temperature of 250 to 550°C to form a Be-Cu alloy raw material;
      working, including bending, the so-obtained alloy raw material into a predetermined parts body configuration; and
      aging the worked alloy material at a temperature of 350 to 500°C.
EP88301618A 1987-03-12 1988-02-25 Shaped body formed of copper-beryllium alloy and method of manufacturing same Expired - Lifetime EP0282204B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP55147/87 1987-03-12
JP5514787A JPS63223151A (en) 1987-03-12 1987-03-12 Formed body for parts composed of berylium-copper alloy material and its production

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EP0282204A1 true EP0282204A1 (en) 1988-09-14
EP0282204B1 EP0282204B1 (en) 1993-09-22

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0500377A1 (en) * 1991-02-21 1992-08-26 Ngk Insulators, Ltd. Production of copper-beryllium alloys and copper-beryllium alloys produced thereby
EP0681035A3 (en) * 1994-04-25 1996-03-06 Olin Corp Process for improving the bend formability of copper alloys.
EP0841407A1 (en) * 1996-10-28 1998-05-13 BRUSH WELLMAN Inc. Copper-nickel-beryllium alloy
EP0854200A1 (en) * 1996-10-28 1998-07-22 BRUSH WELLMAN Inc. Copper-beryllium alloy
US5824167A (en) * 1994-01-06 1998-10-20 Ngk Insulators, Ltd. Beryllium-copper alloy excellent in strength, workability and heat resistance and method for producing the same
WO1999007902A1 (en) * 1997-08-04 1999-02-18 Integran Technologies Inc. Metallurgical method for processing nickel- and iron-based superalloys

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DE102006018896B3 (en) * 2006-04-24 2007-12-13 Infineon Technologies Ag Local selective change of breaking strength and elongation in region of bending groove of electrical terminal clamp, includes strong cold deformation of the electrical terminal clamp by annealing under variable recrystallization temperature
JP5480688B2 (en) * 2010-03-26 2014-04-23 株式会社神戸製鋼所 Aluminum alloy plate for PP cap and method for producing the same
EP3208664B1 (en) * 2016-02-19 2023-08-16 Omega SA Timepiece mechanism or clock without magnetic signature

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WO1980001169A1 (en) * 1978-12-11 1980-06-12 Kawecki Berylco Ind Treatment of shaped beryllium-copper alloys
US4394185A (en) * 1982-03-30 1983-07-19 Cabot Berylco, Inc. Processing for copper beryllium alloys
FR2554830A1 (en) * 1983-11-10 1985-05-17 Brush Wellman THERMOMECHANICAL TREATMENT OF COPPER-BERYLLIUM ALLOYS
WO1986005522A1 (en) * 1985-03-18 1986-09-25 Woodard Dudley H Controlling distortion in processed copper beryllium alloys

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WO1980001169A1 (en) * 1978-12-11 1980-06-12 Kawecki Berylco Ind Treatment of shaped beryllium-copper alloys
US4394185A (en) * 1982-03-30 1983-07-19 Cabot Berylco, Inc. Processing for copper beryllium alloys
FR2554830A1 (en) * 1983-11-10 1985-05-17 Brush Wellman THERMOMECHANICAL TREATMENT OF COPPER-BERYLLIUM ALLOYS
WO1986005522A1 (en) * 1985-03-18 1986-09-25 Woodard Dudley H Controlling distortion in processed copper beryllium alloys

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Title
PATENT ABSTRACTS OF JAPAN, vol. 6, no. 49 (C-96)[927], 31st March 1982; & JP-A-56 163 248 (NIPPON GAISHI K.K.) 15-12-1981 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0500377A1 (en) * 1991-02-21 1992-08-26 Ngk Insulators, Ltd. Production of copper-beryllium alloys and copper-beryllium alloys produced thereby
US5354388A (en) * 1991-02-21 1994-10-11 Ngk Insulators, Ltd. Production of beryllium-copper alloys and beryllium copper alloys produced thereby
US5565045A (en) * 1992-11-04 1996-10-15 Olin Corporation Copper base alloys having improved bend formability
US5601665A (en) * 1992-11-04 1997-02-11 Olin Corporation Process for improving the bend formability of copper alloys
US5824167A (en) * 1994-01-06 1998-10-20 Ngk Insulators, Ltd. Beryllium-copper alloy excellent in strength, workability and heat resistance and method for producing the same
EP0681035A3 (en) * 1994-04-25 1996-03-06 Olin Corp Process for improving the bend formability of copper alloys.
EP0841407A1 (en) * 1996-10-28 1998-05-13 BRUSH WELLMAN Inc. Copper-nickel-beryllium alloy
EP0854200A1 (en) * 1996-10-28 1998-07-22 BRUSH WELLMAN Inc. Copper-beryllium alloy
US5993574A (en) * 1996-10-28 1999-11-30 Brush Wellman, Inc. Lean, high conductivity, relaxation-resistant beryllium-nickel-copper alloys
US6001196A (en) * 1996-10-28 1999-12-14 Brush Wellman, Inc. Lean, high conductivity, relaxation-resistant beryllium-nickel-copper alloys
WO1999007902A1 (en) * 1997-08-04 1999-02-18 Integran Technologies Inc. Metallurgical method for processing nickel- and iron-based superalloys

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JPS63223151A (en) 1988-09-16
JPH0123526B2 (en) 1989-05-02
DE3884239T2 (en) 1994-03-31
EP0282204B1 (en) 1993-09-22
DE3884239D1 (en) 1993-10-28

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