US20070062619A1 - Copper alloy and process for producing the same - Google Patents

Copper alloy and process for producing the same Download PDF

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US20070062619A1
US20070062619A1 US11/518,194 US51819406A US2007062619A1 US 20070062619 A1 US20070062619 A1 US 20070062619A1 US 51819406 A US51819406 A US 51819406A US 2007062619 A1 US2007062619 A1 US 2007062619A1
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alloy
diameter
precipitates
copper alloy
inclusions
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Yasuhiro Maehara
Mitsuharu Yonemura
Keiji Nakajima
Tsuneaki Nagamichi
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Nippon Steel Corp
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Individual
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Priority claimed from JP2004234868A external-priority patent/JP2005290543A/ja
Priority claimed from JP2004234891A external-priority patent/JP2005307334A/ja
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Assigned to SUMITOMO METAL INDUSTRIES, LTD. reassignment SUMITOMO METAL INDUSTRIES, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MAEHARA, YASUHIRO, NAGAMICHI, TSUNEAKI, NAKAJIMA, KEIJI, YONEMURA, MITSUHARU
Publication of US20070062619A1 publication Critical patent/US20070062619A1/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
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/10—Alloys based on copper with silicon as the next major constituent
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/02—Contact members
    • H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the present invention relates to a copper alloy, which can be produced at low cost and has excellent mechanical and electrical properties.
  • This invention also relates to a process for producing the said copper alloy.
  • This copper alloy is suitable for electrical and electronic parts, safety tools, and the like.
  • Examples of the electric and electronic parts include connectors for personal computers, semiconductor plugs, optical pickups, coaxial connectors, IC checker pins and the like in the electronics field; cellular phone parts (connector, battery terminal, antenna part), submarine relay casings, exchanger connectors and the like in the communication field; and various electric parts such as relays, various switches, micromotors, diaphragms, and various terminals in the automotive field; medical connectors, industrial connectors and the like in the medical and analytical instrument field; and air conditioners, home appliance relays, game machine optical pickups, card media connectors and the like in the electric home appliance field.
  • Examples of the safety tools include excavating rods and tools such as spanner, chain block, hammer, driver, cutting pliers, and nippers, which are used where a possible spark explosion hazard may take place, for example, in an ammunition chamber, a coal mine, or the like.
  • a Cu—Be alloy has been known as a copper alloy that is used for the above mentioned electric and electronic parts. This alloy is strengthened by age precipitation of the Be, and contains a substantial amount of Be. This alloy has been extensively used as a spring material or the like because it is excellent in both tensile strength and electric conductivity. However, Be oxide is generated in the production process of Cu—Be alloy and also in the process of forming to various parts.
  • Be is an environmentally harmful material as is Pb and Cd.
  • the substantial amount of Be in the conventional Cu—Be alloy necessitates a treatment process for the Be oxide in the production and working of the copper alloy.
  • the treatment process leads to an increase in the production cost. It also causes a problem in the recycling process of the electric and electronic parts.
  • the Cu—Be alloy is a problematic material from the environmental point of view. Therefore, a material, which is excellent in both tensile strength and electric conductivity and in which the content of environmentally harmful elements such as Be is as low as possible, is desired.
  • Corson alloy in which Ni 2 Si is precipitated, is proposed in Patent Document 1.
  • This alloy has a relatively good balance of tensile strength and electric conductivity among alloys free from environmentally harmful elements such as Be, and has a electric conductivity of about 40% at a tensile strength of 750 to 820 MPa.
  • this alloy has limitations in enhancing strength and electric conductivity, and this still leaves a problem from the point of product variations as described below.
  • This alloy has age hardenability due to the precipitation of Ni 2 Si. If the electric conductivity is enhanced by reducing the contents of Ni and Si, the tensile strength is significantly reduced. On the other hand, even if the contents of Ni and Si are increased in order to raise the precipitation quantity of Ni 2 Si, the electric conductivity is seriously reduced, although the rise of tensile strength is limited. Therefore, the balance between tensile strength and electric conductivity of the Corson alloys is disrupted in an area with high tensile strength and in an area with high electric conductivity, consequently narrowing the product variations. This is explained as follows.
  • the electric resistance (or electric conductivity that is the inverse thereof of an alloy is determined by electron scattering, and fluctuates depending on the kinds of elements dissolved in the alloy. Since the Ni dissolved in the alloy noticeably raises the electric resistance (noticeably reduces the electric conductivity), the electric conductivity reduces in the above-mentioned Corson alloy if Ni is increased. On the other hand, the tensile strength of the copper alloy is obtained due to an age hardening effect. The tensile strength is improved more as the quantity of precipitates grows larger, or as the precipitates are dispersed more finely.
  • the Corson alloy has limitations in enhancing the strength from the point of the precipitation quantity and from the point of the dispersing state, since the precipitated particle is made up of Ni 2 Si only.
  • Patent Document 2 discloses a copper alloy with a satisfactory wire bonding property, which contains elements such as Cr and Zr and has a regulated surface hardness and surface roughness. As described in an embodiment thereof, this alloy is produced based on hot rolling and solution treatment.
  • the hot rolling needs a surface treatment for preventing hot cracking or removing scales, which result in a reduction in yield. Further, frequent heating in the atmosphere facilitates oxidation of active additive elements such as Si, Mg and Al. Therefore, the generated coarse internal oxides problematically s cause deterioration of characteristics of the final product. Further, the hot rolling and solution treatment need an enormous amount of energy.
  • the copper alloy described in Patent Document 2 thus has problems in view of an addition in production cost and energy saving because this alloy is based on the hot working and solution treatment, Furthermore, deterioration of product characteristics (bending workability, fatigue characteristic and the like besides tensile strength and electric conductivity), which is result of generation of coarse oxides and the like.
  • the safety tool materials have required mechanical properties, for example, strength and wear resistance matching those of tool steel. It is also required to avoid generating sparks which could cause an explosion. In other words, excellent spark generation resistance is necessary for the safety tool materials. Therefore, a copper alloy with high thermal conductivity, particularly, a Cu—Be alloy aimed at strengthening by age precipitation of Be has been extensively used. Although the Cu—Be alloy is an environmentally problematic material, as described above, it has been heavily used as the safety tool material based on the following.
  • FIG. 1 is a graph showing the relationship between electric conductivity [IACS (%)] and thermal conductivity [TC (W/m.K)] of a copper alloy. As shown in FIG. 1 , both are almost in a 1:1-relation. Enhancing of the electric conductivity [IACS (%)] means enhancing of the thermal conductivity [TC (W/m.K)], in other words, enhancing of the electric conductivity inproves the spark generation resistance. Sparks are generated by the application of a sudden force by an impact blow or the like during the use of a tool due to a specified component in the alloy being burnt by the heat generated by an impact or the like.
  • Non-Patent Document 1 steel tends to cause a local temperature rise due to its thermal conductivity which can be as low as 1 ⁇ 5 or less of that of Cu. Since the steel contains C, a reaction “C+O 2 ⁇ CO 2 ” takes place, generating sparks. In fact, it is known that pure iron containing no C generates no sparks. Other metals which tend to generate sparks are Ti and Ti alloy. The thermal conductivity of Ti is as extremely low, as low as 1/20 of that of Cu, and therefore the reaction “Ti+O 2 ⁇ TiO 2 ” takes place. Data shown in Non-Patent Document 2 are summarized in FIG. 1 .
  • the electric conductivity [IACS (%)] and the tensile strength [TS (MPa)] are in a trade-off relation, and it is extremely difficult to enhance both simultaneously. Therefore, the Cu—Be alloy was the only copper alloy that had sufficiently high thermal conductivity TC while retaining a tool steel-level high tensile strength in the past.
  • the “wide production variations” mean that the balance between electric conductivity and tensile strength can be adjusted from a high level equal to or higher than that of the Cu—Be alloy to a low level equal to that of a conventionally known copper alloy, by minutely adjusting addition quantities and/or a production condition.
  • the “balance between electric conductivity and tensile strength can be adjusted from a high level equal to or higher than that of the Cu—Be alloy” specifically means a state satisfying the following formula (a). This state is hereinafter referred to as a “state with an extremely satisfactory balance of tensile strength and electric conductivity”.
  • TS 648.06+985.48 ⁇ exp( ⁇ 0.0513 ⁇ IACS) (a) wherein TS represents tensile strength (MPa) and IACS represents electric conductivity (%).
  • the bending workability it is also desirable to ensure a level equal to that of a conventional alloy such as Cu—Be alloy.
  • a satisfactory range of bending workability satisfies B ⁇ 2.0 in a plate material with a tensile strength TS of 800 MPa or less, which satisfies the following formula (b) in a plate material having a tensile strength TS exceeding 800 MPa.
  • wear resistance is also required in addition to other characteristics such as tensile strength TS and electric conductivity IACS as described above. Therefore, it is necessary to ensure that wear resistance is equal to that of tool steel. Specifically, a hardness at room temperature of 250 or more in the Vickers hardness is regarded as excellent wear resistance.
  • the present invention involves copper alloys shown in the following (A) to (C), and a method for producing a copper alloy shown in the following (D).
  • a copper alloy characterized in that the alloy consists of, by mass %, one or more elements selected from Zn, Sn, Ag, Mn, Fe, Co, Al, Ni, Si, Mo, V, Nb, Ta, W, Ge, Te and Se of 0.1 to 20% respectively or in total, and the balance Cu and impurities; and the alloy satisfies the following formula (1): log N ⁇ 0.4742+17.629 ⁇ exp( ⁇ 0.1133 ⁇ X ) ) (1)
  • N means the total number of precipitates and inclusions, having a diameter of not smaller than 1 ⁇ m, which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m.
  • (B) A copper alloy characterized in that the alloy consists of, by mass %, an element selected from Ti of 0.01 to 5%, Zr of 0.01 to 5% and Hf of 0.01 to 5%, and one or more elements selected from Zn, Sn, Ag, Mn, Fe, Co, Al, Ni, Si, Mo, V, Nb, Ta, W. Ge, Te and Se of 0.01 to 20% respectively or in total, and the balance Cu and impurities; and the alloy satisfies the following formula (1): log N ⁇ 0.4742+17.629 ⁇ exp( ⁇ 0.1133 ⁇ X ) (1)
  • N means the total number of precipitates and inclusions, having a diameter of not smaller than 1 ⁇ m, which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m.
  • (C) A copper alloy characterized in that the alloy consists of, by mass %, Cr of 0.01 to 5%, and one or more elements selected from Zn, Sn, Ag, Mn, Fe, Co, Al, Ni, Si, Mo, V, Nb, Ta, W. Ge, Te and Se of 0.01 to 20% respectively or in total, and the balance Cu and impurities; and the alloy satisfies the following formula (1): log N ⁇ 0.4742+17.629 ⁇ exp( ⁇ 0.1133 ⁇ X ) (1)
  • N means the total number of precipitates and inclusions, having a diameter of not smaller than 1 ⁇ m, which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m.
  • the copper alloy shown in above (A), (B) or (C) may, instead of a part of Cu, contain one or more elements selected from Mg, Li, Ca and rare earth elements of 0.001 to 2 mass % respectively or in total , and/or one or more elements selected from P, B, Bi, Tl, Rb, Cs, Sr, Ba, Tc, Re, Os, Rh, In, Pd, Po, Sb, Au, Ga, S, Cd, As and Pb of 0.001 to 3 mass % respectively or in total. Further the alloy may contain 0.1 to 5 mass % of Be.
  • the ratio of the “maximum value of the average content” and the “minimum value of the average content” of at least one alloy element in a micro area is not less than 1.5.
  • the grain size of the alloy is desirably 0.01 to 35 ⁇ m.
  • (D) A method for producing a copper alloy, which satisfies the following formula (1), comprising cooling a bloom, a slab, a billet or an ingot obtained by melting a copper alloy, having a chemical composition described in the above (A), (B) or (C) followed by cooling in at least a temperature range from the temperature of the bloom, the slab, the billet or the ingot just after casting to 450° C., at a cooling rate of 0.5° C./s or more, log N ⁇ 0.4742+17.629 ⁇ exp( ⁇ 0.1133 ⁇ X ) (1)
  • N means the total number of precipitates and inclusions, having a diameter of not smaller than 1 ⁇ m which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having a diameter of not smaller than 1 ⁇ m.
  • working in a temperature range of 600° C. or lower, and a further heat treatment holding for 30 seconds or more in a temperature range of 150 to 750° C. are desirably performed.
  • the working in a temperature range of 600° C. or lower and the heat treatment of holding in a temperature range of 150 to 750° C. for 30 seconds or more may be performed for a plurality of times.
  • the working in a temperature range of 600° C. or lower may be performed.
  • the precipitates in the present invention mean metals or compounds of copper and additive elements and between additive elements, for example, Cu 4 Ti in the, alloy containing Ti, Cu 9 Zr 2 in the alloy containing Zr, metal Cr in the alloy containing Cr.
  • the inclusions mean, for example, metal oxides, metal carbides, metal nitrides and the like.
  • One of the copper alloy according to the present invention has a chemical composition consisting of 0.1 to 20% respectively or in total of at least one element selected from Zn, Sn, Ag, Mn, Fe, Co, Al, Ni, Si, Mo, V, Nb, Ta, W. Ge, Te and Se (referred to as “the first group elements” hereinafter) and the balance Cu and impurities.
  • each of these elements has an effect of improving corrosion resistance and heat resistance while keeping a balance between strength and electric conductivity. This effect is exhibited when 0.1% or more respectively or in total of these elements is contained. However, when their contents are excessive, the electric conductivity is reduced. Accordingly, these elements should be contained at 0.1 to 20% respectively or in total. Particularly, since Ag and Sn contribute to the increase in strength of the alloy by forming fine precipitates, active use of them is preferred. In the alloy that contains the following second group elements, the lower limit of the first group elements may be 0.01% because the strength can be maintained the second group elements.
  • the copper alloy of the present invention may contain an element selected from 0.01 to 5% of Ti, 0.01 to 5% of Zr and 0.01 to 5% of Hf, and also may contain 0.01 to 5.0% Cr, instead of a part of Cu.
  • these elements are referred to as the second group elements.
  • the Cr is an element that increases strength without making electric conductivity higher.
  • the Cr content is preferably 0.01% or more.
  • a content of 0.1% or more is desirable.
  • the preferable Cr content is 0.01 to 5% when it is added.
  • the copper alloy of the present invention desirably contains, instead of a part of Cu, one or more elements selected from Mg, Li, Ca and rare earth elements of 0.001 to 2% respectively or in total.
  • these elements are referred to as the third group elements.
  • Mg, Li, Ca and rare earth elements are easily bonded with an oxygen atom in the Cu matrix, leading to fine dispersion of the oxides, which enhance the high-temperature strength. This effect is noticeable when the total content of these elements is 0.001% or more. However, a content exceeding 2% could result in saturation, and causes problems such as reduction in electric conductivity and deterioration of bending workability. Therefore, when one or more element selected from Mg, Li, Ca and rare earth elements are included, the respective or total content thereof is desirably set to 0.001 to 2%.
  • the rare earth elements mean Sc, Y and lanthanide, may be added separately or in a form of misch metal.
  • the copper alloy of the present invention desirably includes 0.001 to 0.3% respectively or in total of one or more elements selected from P. B, Bi, Tl, Rb, Cs, Sr, Ba, Tc, Re, Os, Rh, In, Pd, Po, Sb, Au, Ga, S, Cd, As and Pb instead of a part of Cu.
  • As, Pd and Cd because they are detrimental elements.
  • these elements from P to Pb are referred to as the fourth group elements.
  • ⁇ T is preferably set within the range of 50 to 200° C.
  • C, N and O are generally included as impurities. These elements form carbides, nitrides and oxides with metal elements in the alloy. These elements may be actively added since the precipitates or inclusions thereof are effective, if fine, for strengthening the alloy, particularly, for enhancing high-temperature strength similarly to the precipitates of metal, compounds of copper and additive elements or between additive elements and the like, which are described later.
  • O has an effect of forming oxides in order to enhance the high-temperature strength. This effect is easily obtained in an alloy containing elements which easily form oxides, such as Mg, Li, Ca and rare earth elements, Al, Si and the like. However, in this case, a condition in which the solid solution O never remains must be selected.
  • each content is preferably limited to 1% or less, and further preferably to 0.1% or less.
  • content of H is desirably as small as possible, since H included as an impurity in the alloy, remains in the state of H 2 gas, which causes rolling flaw or the like.
  • Be is an element that contributes to precipitation-strengthening without deteriorating electric conductivity remarkably.
  • the content of Be is 0.1 mass % or more.
  • a content exceeding 5% causes not only reduction in electric conductivity but also reduction of ductility, which deteriorates workability for rolling or bending and the like. Therefore, the preferable content of Be is 0.1 to 5% when it is added.
  • the relationship between the total number N and the diameter X of precipitates and inclusions that have a diameter of not smaller than 1 ⁇ m satisfies the following formula (1):
  • N means the total number of precipitates and inclusions, having a diameter of not smaller than 1 ⁇ m, which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m.
  • fine precipitates of metal, compounds of copper and additive elements and between additive elements can improve the strength without reducing the electric conductivity. They enhance the strength by precipitation hardening. The dissolved Cr, Ti, and Zr are reduced by precipitation, and the electric conductivity of the copper matrix comes close to that of pure copper.
  • an essential requirement is regulated so that the relationship between the total number of N and the diameter X satisfies the above formula (1).
  • the total number of the precipitates and the inclusions desirably satisfies the following formula (2), and further preferably satisfies the following formula (3).
  • the diameter and the total number of the precipitates and the inclusions can be determined by using a method shown in Examples. log N ⁇ 0.4742+7.9749 ⁇ exp( ⁇ 0.1133 ⁇ X ) (2) log N ⁇ 0.4742+6.3579 ⁇ exp( ⁇ 0.1133 ⁇ X ) (3)
  • N means the total number of precipitates and inclusions, having a diameter not smaller than 1 ⁇ m which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter not smaller than 1 ⁇ m.
  • the presence of a structure, in which areas with different concentrations of alloy elements are finely mingled, in the copper alloy, or the occurrence of a periodic concentration change has an effect of facilitating acquisition of the micro-crystal grain structure, since it inhibits minute diffusion of each element and the grain boundary migration. Consequently, the strength and ductility of the copper alloy are improved according to the so-called Hall-Petch law.
  • the micro-area means an area of 0.1 to 1 ⁇ m diameter, which substantially corresponds to an irradiation area in X-ray analysis.
  • the areas with different alloy element concentrations in the present invention are the following two types.
  • the lattice constant is generally differed in spite of the same fcc structure due to the different alloy element concentrations, and also the degree of work hardening is of course differed.
  • the average content in the micro-area means the value in an analysis area when narrowing to a fixed beam diameter of 1 ⁇ m or less in the X-ray analysis.
  • the value is the average content in this area.
  • an analyzer having a field emission type electron gun is desirably used.
  • a desirable analyzing means are such that have a resolution of 1 ⁇ 5 or less of the concentration period, and 1/10 is further desirable. If the analysis area is too large during the concentration period, the whole is averaged to make the concentration difference difficult to emerge.
  • the measurement can be performed by an X-ray analysis method with a probe diameter of about 1 ⁇ m.
  • a line analysis is performed using of an X-ray analyzer with a probe diameter of about 1 ⁇ m in order to grasp the periodic structure of concentration, although it is varied depending on the materials.
  • An analysis method is determined so that the probe diameter is about 1 ⁇ 5 of the concentration period or less as described above. Then a sufficient line analysis length, where the period emerges about three times or more is determined.
  • the line analysis is performed m-times (desirably 10 times or more) under this condition, and the maximum value and the minimum value of concentration are determined for each of the line analysis results.
  • the concentration ratio is determined by the ratio of the maximum value compared to the minimum value from which the disturbance factors have been removed.
  • the concentration ratio can be determined for an alloy element, having a periodic concentration change of about 1 ⁇ m or more, without taking a concentration change of an atomic level of about 10 nm or less, such as spinodal decomposition or micro-precipitates, into consideration.
  • the electric resistance (the inverse of electric conductivity) mainly responds to a phenomenon in which the electron transition is reduced due to the scattering of dissolved elements, and is hardly affected by a macro defect such as grain boundary, the electric conductivity is never reduced by the above-mentioned fine grain structure.
  • concentration ratio the ratio of the “average content maximum value” to the “average content minimum value” in the micro-area of at least one alloy element in the matrix.
  • concentration ratio is 1.5 or more.
  • the upper limit of the concentration ratio is not particularly determined.
  • an excessively high concentration ratio might cause adverse effects, such that an excessively increased difference of the electrochemical characteristics which facilitates local corrosion, and in addition to that the fcc structure possessed by the Cu alloy cannot be kept. Therefore, the concentration ratio is set preferably to 20 or less, and more preferably to 10 or less.
  • a finer grain size of the copper alloy is advantageous for enhancing the strength, and also leads to an improvement in ductility which improves bending workability and the like.
  • the grain size is desirably set at 0.01 to 35 ⁇ m, and further desirably to 0.05 to 30 ⁇ m, and most desirably to 0.1 to 25 ⁇ m.
  • inclusions such as metal oxides, metal carbides and metal nitrides, which inhibit the fine precipitation of metals, compounds of copper and additive elements and between additive elements, tend to formed just after the solidification from the melt. It is difficult to dissolve such inclusions even if the solution treatment at a higher temperature is performed after casting. The solution treatment at a high temperature only causes coagulation and the coarsening of the precipitates and inclusions.
  • a bloom, a slab, a billet or an ingot, obtained by melting the copper alloy having the above chemical composition by casting is cooled to at least a temperature range from the bloom, the slab, the billet or the ingot temperature just after casting to 450° C., at a cooling rate of 0.5° C./s or more, whereby the relationship between the total number N and the diameter X of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m satisfies the following formula (1): log N ⁇ 0.4742+17.629 ⁇ exp( ⁇ 0.1133 ⁇ X ) (1)
  • N means the total number of precipitates and inclusions, which are found in 1 mm 2 of the alloy; and X means the diameter in ⁇ m of the precipitates and the inclusions having diameter of not smaller than 1 ⁇ m.
  • working in a temperature range of 600° C. or lower, and a holding heat treatment for 30 seconds or more in a temperature range of 150 to 750° C. after this working are desirably performed.
  • the working in a temperature range of 600° C. or lower and the holding heat treatment for 30 seconds or more in a temperature range of 150 to 750° C. are further desirably performed for a plurality of times. After the final heat treatment, the working may be further performed.
  • the precipitates such as metals, compounds of copper and added elements and between added compounds are formed in a temperature range of 280° C. or higher. Particularly, when the cooling rate in a temperature range, from the bloom, the slab, the billet or the ingot temperature just after casting to 450° C. is low, inclusions such as metal oxides, metal carbides and metal nitrides are coarsely formed, and the diameter thereof may reach 20 ⁇ m or more, and further hundreds ⁇ m. Further, the said precipitates are also coarsened to 20 ⁇ m or more.
  • the bloom, the slab, the billet or the ingot obtained by casting is made into a final product, after cooling under a predetermined condition, only by a combination of working and aging heat treatment without passing through a hot process, such as hot rolling or solution treatment.
  • a working such as rolling or drawing may be performed at 600° C. or lower.
  • a working can be performed in the cooling process after solidification.
  • precipitates such as metals, compounds of copper and additive elements and between additive elements are coarsely formed at the time of working, deteriorating the ductility, impact resistance, and fatigue property of the final product.
  • fine precipitates cannot be formed in the aging treatment, resulting in an insufficient strengthening of the copper alloy.
  • the working temperature is preferably 450° C. or lower, more preferably 250° C. or lower, and most preferably 200° C. or lower.
  • the temperature may also be 25° C. or lower.
  • the working in the above temperature range is desirably performed at a working rate (section reduction rate) of 20% or more, and more desirably 50% or more. If the working is performed at such a working rate, the dislocation introduced thereby can act as precipitation nuclei at the time of aging treatment, which leads to fine dispersion of the precipitates and also shortens of the time required for the precipitation, and therefore the reduction of dissolved elements harmful to electric conductivity can be early realized.
  • the aging treatment is effective for precipitating metals, compounds of copper and additive elements and between additive elements in order to strengthen the copper alloy, and also reduce dissolved elements (Cr, Ti, etc.) harmful to electric conductivity in order to improve the electric conductivity.
  • dissolved elements Cr, Ti, etc.
  • the aging treatment is desirably performed in a temperature range of 150 to 750° C.
  • the aging treatment temperature is desirably 200 to 750° C., further desirably 250 to 650° C., and most desirably 280 to 550° C..
  • the aging treatment time is less than 30 seconds, a desired precipitation quantity cannot be ensured even if the aging treatment temperature is high.
  • the time is longer than 72 hours, production cost becomes higher. Therefore, the aging treatment in a temperature range of 150 to 750° C. is desirably performed for 30 seconds or more.
  • the treatment time is desirably 5 minutes or more, further desirably 10 minutes or more, and most desirably 15 minutes or more.
  • the upper limit of the treatment time is not particularly limited. However, 72 hours or less is desirable from the point of the treatment cost.
  • the aging processing time can be shortened.
  • the aging treatment is preferably performed in a reducing atmosphere, in an inert gas atmosphere, or in a vacuum of 20 Pa or less in order to prevent the generation of scales due to oxidation on the surface. Excellent plating property can also be ensured by the treatment in such an atmosphere.
  • the above-mentioned working and aging treatment may be performed repeatedly as the occasion demands.
  • a desired precipitation quantity can be obtained in a shorter time than in the case of one set treatment (working and aging treatment), and precipitates such as metals, compounds of copper and additive elements and between additive elements can be more finely precipitated.
  • the second aging treatment temperature is preferably set slightly lower than the first aging treatment temperature (by 20 to 70° C.). If the second aging treatment temperature is higher, the precipitates formed in the first aging treatment are coarsened.
  • the temperature is desirably set lower than the previous aging treatment temperature.
  • the working in a temperature range of 600° C. or lower may be performed after the final heat treatment.
  • conditions other than the above production conditions for example, conditions for melting, casting and the like are not particularly limited. These treatments may be performed as follows.
  • Melting is preferably performed in a non-oxidative or reducing atmosphere. If the dissolved oxygen in a molten copper is increased, the so-called hydrogen-induced blistering due to generation of steam is caused in the subsequent process. Further, coarse oxides of easily-oxidizable dissolved elements such as Ti and Cr are formed, and if they are left in the final product, the ductility and fatigue characteristic are seriously reduced.
  • the slab, the billet or the ingot, continuous casting is preferably adapted from the point of productivity and solidification rate.
  • any other methods which satisfy the above-mentioned conditions, for example, an ingot method, can be used.
  • the casting temperature is preferably 1250° C. or higher, and further preferably 1350° C. or higher. At this temperature, Cr, Ti and Zr can be sufficiently dissolved, and formation of inclusions such as metal oxides, metal carbide and metal nitrides, precipitates such as metals, compounds of copper and additive elements and between additive elements can be prevented.
  • a method using graphite mold which is generally adapted for a copper alloy is recommended from the viewpoint of lubricating property.
  • a mold material a refractory material, which is hardly reactive with Ti, Cr or Zr that is an essential alloy element, for example, zirconia may be used.
  • Each of the resulting slabs was cooled from a temperature between 950° C. and 450° C., which is the temperature just after casting (the temperature just after taken out of the mold), by water spray.
  • the temperature change of the mold in a predetermined place was measured by a thermocouple buried in the mold, and the surface temperature of the slab, after leaving the mold, was measured in several areas by a contact type thermometer.
  • the average cooling rate, in the temperature range to 450° C., of the slab surface was calculated by using the above measuring results and a thermal conduction analysis.
  • the solidification starting point was determined by using 0.2 g of a melt of each alloy, and thermally analyzing it during continuous cooling at a predetermined rate.
  • a plate for subsequent rolling with 10 mm thickness ⁇ 8 Omm width ⁇ 150 mm length was prepared from each resulting slab by cutting and machining. For comparison, a part of the plate was subjected to a solution heat treatment at 950° C.. The plates were rolled to 2 mm thick sheets by a reduction of 80% at a room temperature (first rolling), and further subjected to aging treatment under a predetermined condition (first aging). A part of the specimens were further subjected to rolling by a reduction of 95% into 0.1 mm thickness at room temperature (second rolling), and then subjected to aging treatment under a predetermined condition (second aging). The production conditions thereof are shown in Tables 4 to 7.
  • a section of the alloy was polished and analyzed at random 10 times for a length of 50 ⁇ m by an X-ray analysis at 2000-fold magnification in order to determine the maximum values and minimum values of each alloy content in the respective line analyses. Averages of the maximum value and the minimum value were determined for eight values each after removing the two larger ones respectively from the determined maximum values and minimum values, and the ratio thereof was calculated as the content ratio.
  • a specimen 13B regulated in JIS Z 2201 was prepared from the above-mentioned specimen so that the tensile direction is parallel to the rolling direction, and according to the method regulated in JIS Z 2241, tensile strength [TS (MPa)] at room temperature (25° C.) thereof was determined.
  • a specimen of 10 mm width ⁇ 60 mm length was prepared from the above-mentioned specimen so that the longitudinal direction is parallel to the rolling direction, and the potential difference between both ends of the specimen was measured by applying current in the longitudinal direction of the specimen, and the electric resistance was determined therefrom by a 4-terminal method. Successively, the electric resistance (resistivity) per unit volume was calculated from the volume of the specimen measured by a micrometer, and the electric conductivity [IACS (%)] was determined from the ratio to resistivity 1.72 ⁇ •cm of a standard sample obtained by annealing a polycrystalline pure copper.
  • X in ⁇ circle around (1) ⁇ means that formulas (1), (2) and (3) are not satisfied.
  • ⁇ circle around (2) ⁇ means “content maximum value/content minimum value”.
  • Object element is shown in parentheses.
  • “X” in “Bending Workability” means that formula (b) is not satisfied.
  • FIG. 2 is a graph showing the relationship between tensile strength and electric conductivity in each example.
  • Tables 4 to 7 and FIG. 2 regarding the chemical composition, the content ratio and the total number of the precipitates and the inclusions are within the ranges regulated by the present invention in Inventive Examples 1 to 67 and the tensile strength and the electric conductivity satisfied the above-mentioned formula (a). Accordingly, it can be said that the balance between electric conductivity and tensile strength of these alloys are of a level equal to or higher than that of the Be-added copper alloy.
  • the copper alloy of the present invention is found to be rich in variations of tensile strength and electric conductivity.
  • Comparative Examples 1 to 4, 6, 10, 12 to 14, 16 and 17 were inferior in bending workability and electric conductivity because the content of any one of alloying elements is out of the range regulated by the present invention.
  • Comparative Examples 1 to 3 and 17 the characteristics could not be evaluated since edge cracking in the second rolling was too serious to collect the samples.
  • samples were prepared by the following method, and evaluated for wear resistance (Vickers hardness) and spark resistance.
  • Alloys having chemical compositions shown in Table 8 were melted in a high frequency furnace in the atmosphere, and were cast by the Durville process. Each bloom was produced by holding a metallic mold 1 in a state as shown in FIG. 3C ( a ), pouring a melt of about 1300° C. into the metallic mold 1 while ensuring a reducing a ⁇ mosphere by charcoal powder, then tilting the mold as shown in FIG. 3C ( b ), and solidifying the melt in a state shown in FIG. 3 ( c ).
  • the metallic mold 1 is made of cast iron with a thickness of 50 mm, and has a pipe arrangement with a cooling hole bored in the inner part so that air cooling can be performed.
  • the bloom was made to a wedge shape having a bottom section of 30 ⁇ 300 mm, an upper section of 50 ⁇ 400 mm, and a height of 700 mm so as to facilitate the pouring of the melt.
  • a part up to 300 mm from the lower end of the resulting bloom was prepared followed by surface-polishing, and then subjected to cold rolling (30 ⁇ 10 mm) and heat treatment (375° C. ⁇ 16h), whereby a plate 10 mm thick was obtained.
  • Such a plate was examined for the total number of the precipitates and the inclusions, tensile strength, electric conductivity, and bending workability by the above-mentioned method and, further, examined for wear resistance, thermal conductivity and spark generation resistance by the method described below. The results are shown in Table 8.
  • a specimen of 10 mm width ⁇ 10 mm length was prepared from each specimen, a section vertical to the rolled surface and parallel to the rolling direction was polish-finished, and the Vickers hardness at 25° C. and load 9.8N thereof was measured by the method regulated in JIS Z 2244.
  • a spark test according to the method regulated in JIS G 0566 was performed by use of a table grinder having a rotating speed of 12,000 rpm, and the spark generation was visually confirmed.
  • a copper alloy that has wide product variations, and is excellent in high-temperature strength and workability, and also excellent in the performances required for safety tool materials, or thermal conductivity, wear resistance and spark generation resistance, and a method for producing the same can be provided.
  • FIG. 1 A graph showing the relationship between the electric conductivity and thermal conductivity
  • FIG. 2 A graph showing the relationship between the tensile strength and the electric conductivity of each of examples.
  • FIG. 3 A schematic view showing a casting method by the Durville process.
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CN115305383A (zh) * 2022-07-30 2022-11-08 江西省科学院应用物理研究所 一种含混合稀土的高强度、高导电Cu-Co系合金材料及其制备方法
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CN117512385A (zh) * 2023-10-31 2024-02-06 江苏康耐特精密机械有限公司 一种多能场复合表面后处理的高精密结构件材料及其制备方法

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CA2559103A1 (en) 2005-09-22
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