CN102869805A - Cu-Ag alloy wire and method for producing Cu-Ag alloy wire - Google Patents
Cu-Ag alloy wire and method for producing Cu-Ag alloy wire Download PDFInfo
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Abstract
Provided is a high-strength Cu-Ag alloy wire having high conductivity, and a method for producing the Cu-Ag alloy wire. The Cu-Ag alloy wire is made from a copper alloy containing Ag, with the Ag content falling within the range of 0.1 mass% to 15 mass%, and the remainder made up of Cu and impurities. When an arbitrarily-defined observation field of up to 1000 nm *1000 nm is taken in the cross section of this Cu-Ag alloy wire, the area ratio of Ag crystalline precipitate present in this observation field made up by crystalline precipitate having a maximum length of a straight line that cuts the crystalline precipitate that does not exceed 100 nm is at least 40%. By uniformly dispersing extremely fine particulate Ag in the alloy, it is possible to improve dispersion strengthening, thereby improving strength, while also giving the alloy wire high conductivity.
Description
Technical field
The present invention relates to the Cu-Ag alloy wire, have the concentric cable of the centre conductor that is consisted of by this Cu-Ag alloy wire, the coaxial cable bunch that obtains by many concentric cable are bundled together and the method for making the Cu-Ag alloy wire.Particularly, the present invention relates to when having high conductivity, also to have more high-intensity Cu-Ag alloy wire.
Background technology
Be accompanied by miniaturization and the lightweight of the various Electrical and Electronic equipment such as electron device and medicine equipment, the thin footpath of the electric wire that is used for these Electrical and Electronic equipment has been produced further demand.
In order also to satisfy the needed intensity of electric wire and fatigue characteristic (for resistance crooked, that reverse etc.) and improve workability (for the workability of wire drawing, twisted wire, coil etc.) when diameter to reduce, the conductor material of electric wire need to have high breaking tenacity.Copper cash has been used as the conductor of electric wire, but the breaking tenacity of copper cash is low.For example, when applying by alternating bending and reversing and during the stress that produces diameter 0.1mm(100 μ m) following superfine copper wires ruptures easily.
One of method of the breaking tenacity of raising conductor material is to form alloy by adding a kind of element.For example, patent documentation 1 discloses the Cu-Ag alloy wire of a kind of Ag of containing.
Reference listing
Patent documentation
Patent documentation 1: the open No.2001-040439 of Japanese unexamined patent
Summary of the invention
Technical problem
Usually in copper alloy, can improve intensity such as breaking tenacity by increasing the content that adds element, but electric conductivity is reduced.The electric wire expectation that is used for electron device and medicine equipment etc. has lower resistance.Therefore, be used as conductor if having the wire rod of low electrical conductivity, then need to reduce resistance by the cross section that increases conductor.In the case, be difficult to reduce diameter.Therefore need a kind of wire rod of exploitation, even this wire rod hour also has high conductivity and high strength at diameter.
An object of the present invention is to provide a kind of Cu-Ag alloy wire, this Cu-Ag alloy wire also has higher intensity when having high conductivity.Another object of the present invention provides a kind of method of making this Cu-Ag alloy wire.Another purpose of the present invention provides a kind of concentric cable that comprises by the centre conductor that consists of of this Cu-Ag alloy wire, and the coaxial cable bunch by many concentric cable are bundled together and obtain.
The means of dealing with problems
[Cu-Ag alloy wire]
For a kind of more high-intensity Cu-Ag alloy wire that also has when having high conductivity (being equal to or higher than existing Cu-Ag alloy wire) is provided, the present inventor is by selecting Ag as adding element the Cu-Ag alloy wire to be studied, and wherein Ag is not easy to reduce electric conductivity and can improves intensity.As a result, the present inventor finds when Ag exists with the form of ultrafine particulate, can make to have high conductivity and high-intensity Cu-Ag alloy wire.The present invention is with the above-mentioned basis that is found to be.
Cu-Ag alloy wire of the present invention relates to the wire rod that is made of the copper alloy that comprises Ag.This Cu-Ag alloy wire comprises the Ag that 0.1 quality % is above and 15 quality % are following, and surplus is Cu and impurity.In this Cu-Ag alloy wire, be of a size of below the 1000nm when in the cross section of described Cu-Ag alloy wire, choosing * during any field of view below the 1000nm, in this field of view in the existing Ag precipitate, be that the area percentage of the Ag precipitate below the 100nm is more than 40% to cutting rear maximum linear length.
In Cu-Ag alloy wire of the present invention, by making the granular Ag precipitate Uniform Dispersion of ultra micro, can realize dispersion-strengthened.Therefore, can further promote intensity, and obtain high conductivity.
In an embodiment of Cu-Ag alloy wire of the present invention, the Ag precipitate also comprises fibrous precipitate.
The Ag precipitate that exists with the form of fibrous precipitate can provide fiber strengthening.In the embodiment of this Cu-Ag alloy wire, can cause the precipitation strength of Ag by the mixing microstructure of fiber strengthening and dispersion-strengthened generation, thereby intensity is further strengthened.
Cu-Ag alloy wire of the present invention can be as the centre conductor of concentric cable.Concentric cable of the present invention relates to such concentric cable, and this concentric cable comprises: have at least one wire rod centre conductor, coat the isolator of this centre conductor and be arranged at external conductor around this isolator.In described concentric cable, described wire rod is Cu-Ag alloy wire of the present invention.
Coaxial cable bunch of the present invention can form by many concentric cable of the present invention are bundled together.
Intrafascicular at concentric cable of the present invention and concentric cable of the present invention, by Cu-Ag alloy wire of the present invention is used as centre conductor, can obtain owing to precipitation strength the improvement of intensity (fatigue characteristic).
[manufacture method of Cu-Ag alloy wire]
When keeping electric conductivity (making electric conductivity be equal to or higher than the electric conductivity of existing Cu-Ag alloy wire), further put forward high-intensity method in order to provide a kind of, the present inventor is by selecting Ag as adding element the Cu-Ag alloy wire to be studied, and Ag is not easy to reduce electric conductivity and can improves intensity.As a result, the present inventor finds to have high conductivity and high-intensity Cu-Ag alloy wire by Ag content being set in the specified range and design and production method, can producing.More specifically, the present inventor finds, with compared by the prepared wire rod of the method that does not comprise following silver-colored dissolving step, prepared wire rod has identical electric conductivity by the following method, also has simultaneously higher intensity, wherein the method comprises: formation Ag fully is dissolved in the state among the Cu before wire drawing, thereby and by the wire rod through wire drawing is carried out the step that specific thermal treatment is separated out Ag.Cu-Ag alloy wire of the present invention can be made by the method for manufacturing Cu-Ag alloy wire according to the present invention, and the back will be described.
In containing the Cu-Ag alloy of a certain amount of Ag, when Ag was dissolved among the Cu, electric conductivity reduced, and when Ag separated out, electric conductivity raise.Therefore, statement " formation Ag fully is dissolved in the state among the Cu " is illustrated in the Cu-Ag alloy that contains a certain amount of Ag, has formed the low state of electric conductivity, rather than the high state of the electric conductivity that causes owing to separating out of Ag.
Before the wire drawing, in castingprocesses (in the situation that especially speed of cooling is lower) forms the state that a large amount of Ag separate out easily usually.
Thus, suggestion makes Ag fully dissolve before wire drawing, and electric conductivity is dissolved in state index among the Cu as indication Ag.
Method according to manufacturing Cu-Ag alloy wire of the present invention relates to such method: the method is made wire rod by the cast material that is made of the copper alloy that contains Ag is carried out wire drawing.In this manufacture method, form electric conductivity C (%IACS) satisfy C≤(0.1786) * x+97(wherein x (quality %) be the content of Ag (0.1 quality %≤x≤15 quality %)) solid-solution material with as will be by the material of wire drawing.In described manufacture method, under the Heating temperature more than 300 ℃, the wire rod through wire drawing is carried out at least one times thermal treatment, this heat treated hold-time is more than 0.5 hour.Definite method about the conditional expression C of electric conductivity C≤(0.1786) * x+97 will be described hereinafter.
In described manufacture method, form the material with state that Ag fully dissolves, described material is carried out wire drawing, and the wire rod through wire drawing is further carried out above-mentioned specific thermal treatment, to separate out the granular Ag precipitate of ultra micro.Therefore, can form the wherein microtexture of Ag uniform particles dispersion.Particulate Ag precipitate has produced dispersion-strengthened, thereby can improve the intensity of Cu-Ag alloy wire.In addition, by wire drawing, make the Ag that separates out before the wire drawing be stretched as fibrous Ag, so the improvement that intensity is able to by fiber strengthening.It is believed that owing to have the granular Ag precipitate of homodisperse ultra micro, have fibrous Ag precipitate or have simultaneously the granular Ag precipitate of ultra micro and fibrous Ag precipitate to have high conductivity and high-intensity Cu-Ag alloy wire thereby can make.Contain the Ag that (for example) 0.1 quality % is above and 15 quality % are following by the resulting Cu-Ag alloy wire of manufacture method of the present invention, surplus is Cu and impurity, and gauge or diameter of wire is below the 1000 μ m.
Beneficial effect of the present invention
Cu-Ag alloy wire of the present invention has high conductivity, and has high strength.Can have high conductivity and high-intensity Cu-Ag alloy wire by the method manufacturing of manufacturing Cu-Ag alloy wire according to the present invention.
Brief Description Of Drawings
Fig. 1 shows Ag content in difference is created conditions the various Cu-Ag alloy materials of manufacturing and the chart of the relation between the electric conductivity.
Fig. 2 shows heat-treat the Photomicrograph (500 times) of the wire rod (φ 2.6mm) after (separating out thermal treatment) through the material of wire drawing, and Fig. 2 comprises the Fig. 2 (I) that shows the 2-3-2 sample and the Fig. 2 (II) that shows the 2-4-2 sample.
Fig. 3 shows heat-treat the transmission electron micrograph (150000 times) of the wire rod (φ 0.9mm) after (separating out thermal treatment) through the material of wire drawing, and Fig. 3 comprises the Fig. 3 (I) that shows the 2-3 sample, the Fig. 3 (II) that shows the 2-4 sample and the Fig. 3 (III) that shows the 2-110 sample.
Fig. 4 comprises the synoptic diagram for the existing Ag precipitate of the Photomicrograph of explanatory view 3.
Fig. 5 is the synoptic diagram of the microtexture of explanation Cu-Ag alloy wire of the present invention.
Fig. 6 is the skeleton view of concentric cable of the present invention.
Embodiment
The below will describe the present invention.
[Cu-Ag alloy wire]
The Cu-Ag alloy that consists of Cu-Ag alloy wire of the present invention is that to comprise 0.1 quality % Ag(surplus above and that 15 quality % are following be Cu and impurity) binary alloy.When the content of Ag is 0.1 quality % when above, produce easily the intensity enhancing effect that forms owing to precipitation strength.When Ag content is 15 quality % when following, suppress easily because Ag excessive separated out the electric conductivity reduction that causes.Particularly, it is above and below the 10 quality % that the content of Ag is preferably 1 quality %, because can realize well balanced between high strength and high conductivity this moment.Prepare raw material, to form predetermined composition.Cu by using high purity (namely more than four or nine purity (purity 99.99%)) and Ag raw material are with the amount of minimizing impurity.Particularly when making thin footpath wire rod, can reduce to cause the amount of the foreign matter of electric wire fracture.
If the content of Ag is low, then the microgranular Ag precipitate in the Ag precipitate is separated out easily.Herein, the size of microgranular Ag precipitate is " be 100nm below to cutting rear maximum linear length ".May there be the situation that contains seedy shape Ag precipitate in the Ag precipitate.The size of coarse grain shape Ag precipitate is " to cutting rear maximum linear length greater than 100nm ".When the content of Ag increases, as the precipitate of Ag, can separate out fibrous Ag precipitate.Fibrous Ag precipitate is the precipitate that the relatively large Ag precipitate in the Ag precipitate is stretched and obtains.Particularly, when Ag content is 2 quality % when above, use microscope to observe easily fibrous Ag precipitate.The Ag precipitate mostly is greatly separates out product, and this is separated out product and basically is made of microgranular Ag precipitate and fibrous Ag precipitate.It is believed that the coarse grain shape Ag precipitate that contains some is as crystallized product.
In Cu-Ag alloy wire of the present invention, be of a size of below the 1000nm when in the cross section of described Cu-Ag alloy wire, choosing * during any field of view below the 1000nm, in the existing Ag precipitate, the area percentage of microgranular Ag precipitate is more than 40% in this field of view.As the Ag precipitate that exists in the field of view, except microgranular Ag precipitate, situation about may be also can seedy shape Ag precipitate existing.Because fibrous Ag precipitate is far longer than the size of field of view, therefore fibrous Ag precipitate is not included in " existing Ag precipitate in the field of view ".The method of choosing field of view will be described hereinafter.By forming the homodisperse microtexture of microgranular Ag precipitate, can realize by dispersion-strengthened and strength increase that produce.It is believed that, even coarse grain Ag precipitate can not have a negative impact to the characteristic of Cu-Ag alloy wire, but also be unfavorable for its characteristic is improved.
If Ag content is high, then except microgranular Ag precipitate, also there is fibrous Ag precipitate.Thus, can realize the improved strength that produced by fiber strengthening.It is believed that owing to have homodisperse microgranular Ag precipitate, have fibrous Ag precipitate or have simultaneously microgranular Ag precipitate and fibrous Ag precipitate, so the Cu-Ag alloy wire has high conductivity and high strength.
Can adopt following methods as making coarse grain shape Ag precipitate help to improve the method for Cu-Ag alloy wire characteristic.In drawing process, the king-sized coarse grain shape of size Ag precipitate is stretched as fibrous, can realize that thus the intensity that produced by fiber strengthening improves.Be not drawn as fibrous coarse grain shape Ag precipitate and be dissolved among the Cu by thermal treatment, and the Ag that dissolves separates out as much as possible and become microgranular Ag precipitate, can realize that therefore the intensity that is produced by dispersion-strengthened improves.As mentioned above, coarse grain shape Ag precipitate can be converted into microgranular Ag precipitate or fibrous Ag precipitate, thereby improves intensity.
The Cu-Ag alloy wire is generally the round line with rounded section, and has multiple gauge or diameter of wire.Preferred gauge or diameter of wire is below the φ 3mm, and especially is preferably φ 1mm(1000 μ m) below, this is because can obtain like this electric wire in thin footpath.Cu-Ag alloy wire of the present invention has high conductivity and high strength, therefore expects that this Cu-Ag alloy wire is enough to be used as the conductor of electric wire, and this electric wire not only can be by the form with the stranded twisted wire that forms of superfine wire rod, also can be the form of single line.Degree of finish during by the appropriate change wire drawing, can produce gauge or diameter of wire is that 0.01mm (10 μ m) is to 0.08mm(80 μ m) superfine Cu-Ag alloy wire.
Cu-Ag alloy wire of the present invention has high conductivity and high strength.This Cu-Ag alloy wire can be φ 0.05mm(50 μ m for (for example) gauge or diameter of wire) following, electric conductivity is that the above and tensile strength of 70%IACS is the above superfine Cu-Ag alloy wire of 1200MPa, perhaps for gauge or diameter of wire is that φ 1mm to 3mm, electric conductivity are more than the 95%IACS and to draw high intensity be Cu-Ag alloy wire more than the 300MPa, but this depends on gauge or diameter of wire and Ag content.
In addition, Cu-Ag alloy wire of the present invention may have the coating that is made of Ag, Ag alloy, Sn or Sn alloy etc. on its surface.This coating can improve wettability and the solidity to corrosion with scolder.When producing the coated Cu-Ag alloy wire of tool, can in drawing process or after final wire drawing, form coating.
[concentric cable and coaxial cable bunch]
As shown in Figure 6, concentric cable 1 of the present invention comprises centre conductor 11, coats the isolator 12 of this centre conductor 11 and is arranged at this isolator 12 external conductor 13 on every side.Concentric cable 1 also comprises the oversheath 14 that coats external conductor 13.Centre conductor 11 comprises a wire rod at least, and this wire rod is Cu-Ag alloy wire of the present invention.Coaxial cable bunch of the present invention can form by many concentric cable of the present invention are bundled together.By with the centre conductor 11 of Cu-Ag alloy wire of the present invention as concentric cable 1, can be improved by precipitation strength intensity (fatigue characteristic).
[manufacture method of Cu-Ag alloy wire]
The method of manufacturing Cu-Ag alloy wire of the present invention generally includes following casting step, drawing step and heat treatment step.
Casting step: make the step of cast material with the mixed melting metal, contain raw material A g and the Cu of fusing in the described mixed dissolution metal.
Drawing step: by the material through the casting step is carried out the step that wire rod is made in wire drawing, described wire rod has final gauge or diameter of wire.
Heat treatment step: the wire drawing material (comprising the wire drawing material with final gauge or diameter of wire) through wire drawing is carried out at least one times following specific heat treated step.
Particularly, prepared such solid-solution material as will carrying out the material of wire drawing, this solid-solution material is in Ag and fully is dissolved in state among the Cu.
[casting step]
Continuous casting is applicable to the manufacturing of cast material.In continuous casting, (for example) can clamp and pull out solidified shell by pinch roll (compressing (packing)), thus the long cast material of continuous casting.Atmosphere during casting can be air atmosphere, but also can adopt the atmosphere of the rare gas elementes such as Ar, to prevent the oxidation of molten metal.In the embodiment of a formation solid-solution material, the speed of cooling of the molten metal in the casting step is more than 8.5 ℃/second.Speed of cooling when casting is set to more than 8.5 ℃/second, namely by quenching, can suppress separating out of Ag, therefore can form the state that Ag fully dissolves.When speed of cooling increased, separating out of Ag was further suppressed.Speed of cooling is preferably more than 10 ℃/second.When pulling out solidified shell as described above, if make the speed of pulling out of solidified shell increase speed of cooling, then solidified shell can't be caught up with the speed of stretching sometimes fully.Therefore, as long as can make continuously cast material, speed of cooling is preferably high as much as possible.
Speed of cooling during casting (℃/second) is defined as following numerical value: (Tm-Tc)/and t
Mc, this numerical value by with temperature head (Tm-Tc) divided by time t
McObtain wherein Tm(℃) for namely just the mixed melting metal inject temperature (being the temperature of the molten metal of tundish) before the mold, Tc(℃) be the temperature of the position of solidifying beginning, t
Mc(second) moves to the used time of measurement point Tc for the mixed melting metal from measurement point Tm.
Adopt following methods that the speed of cooling when making is reached more than 8.5 ℃/second.For example, can adopt the water-cooled copper casting mold.Perhaps, fully to cool off in order making from the solidified shell of mold stretching, can to arrange and force cooling apparatus so that it surrounds solidified shell.Force the example of cooling apparatus to comprise the blast apparatuses such as water-cooled copper block and fan.Can utilize these equipment with the cooling of solidified shell ambient air, and utilize and through overcooled atmosphere solidified shell is cooled off.Can force the temperature of cooling apparatus and the drawing speed (casting speed) of solidified shell to control speed of cooling by suitable adjusting.
[solution treatment]
Form in the embodiment of solid-solution material at another, can carry out solution treatment to resulting cast material in the casting step (through above-mentioned quenching or the cast material through quenching not).Described solution treatment is keeping the time more than 0.5 hour to carry out preferably with the speed of cooling more than 1.5 ℃/second under the Heating temperature more than 600 ℃.
Be more than 600 ℃ and the hold-time is more than 0.5 hour the time in Heating temperature, even Ag separates out in cast material, Ag also can fully be dissolved among the Cu.Along with Heating temperature raises, Ag is tending towards being dissolved among the Cu more fully.Yet if Heating temperature is too high, the Cu-Ag alloy begins fusing.Therefore, Heating temperature is preferably below 850 ℃.Along with the hold-time increases, Ag is tending towards being dissolved among the Cu more fully.There is no particular limitation for the upper limit of hold-time, preferably selects the suitable hold-time in the scope that does not make productivity losing.
By the speed of cooling in the solution treatment is arranged on more than 1.5 ℃/second, namely by quenching, the Ag that can suppress to have dissolved separates out, and therefore can form the state that Ag fully dissolves.Along with the increase of speed of cooling in the solution treatment, can further suppress separating out of Ag.Speed of cooling is preferably more than 3 ℃/second, and for the not specific restriction of reaching the standard grade of speed of cooling.
Speed of cooling during with solution treatment (℃/second) be defined as by with temperature head (Tr-T1) divided by resulting value of 60 seconds time, wherein T1(℃) be the temperature of cooling beginning sample in the time of rear a minute, and Tr(℃) be solid solution temperature.
Speed of cooling when forcing cooling apparatus to make solution treatment by suitable employing reaches more than 1.5 ℃/second.For example, can adopt the direct cooling that utilizes water, oil or the mobile refrigerant such as husky, utilize the air blast cooling of fan etc., perhaps water-cooled copper block.When using water-cooled copper block to cool off, (for example) is arranged at water-cooled copper block around the wire rod that obtains from heat treatment furnace, thereby the wire rod ambient air is cooled.Can control speed of cooling by the temperature of suitably regulating refrigerant, the setting of forcing cooling apparatus and the amount of refrigerant or air etc.
[drawing step]
Repeatedly carry out wire drawing (being generally cold drawn silk) until obtain final gauge or diameter of wire.Consider composition (content of Ag) and final gauge or diameter of wire etc., can carry out suitable adjusting to each degree of finish.
[thermal treatment]
Under given conditions, the wire rod (particularly, for carrying out the wire drawing material of wire drawing, perhaps having passed through wire drawing until obtain the wire drawing material of final gauge or diameter of wire) that carries out wire drawing is heat-treated, to separate out Ag the state that fully dissolves from Ag.It is believed that by this thermal treatment, separated out the granular Ag precipitate of nano level ultra micro.It is believed that, when the granular Ag precipitate of ultra micro exists with homodisperse form, with have following Ultrastructural wire rod and compare, even electric conductivity is almost identical, also can produce the higher Cu-Ag alloy wire of intensity, wherein the amount of separating out of Ag is identical in the above-mentioned ultrastructure, and main existence is fibrous Ag precipitate.
Can carry out at least one times above-mentioned thermal treatment (hereinafter referred to as separating out thermal treatment) to the wire rod through wire drawing.When once separating out thermal treatment, manufacturing step is few, therefore obtains high productivity.When repeatedly separating out thermal treatment, the Ag(that separates out is microgranular Ag precipitate particularly) amount increase, improved thus intensity and electric conductivity, and eliminated the processing strain that causes owing to wire drawing, thereby increased electric conductivity, and follow-up wire drawing is carried out easily.
Separating out thermal treatment is to keep the time more than 0.5 hour to carry out under the Heating temperature more than 300 ℃.If Heating temperature was lower than 300 ℃ or hold-time less than 0.5 hour, then Ag can't fully separate out, and perhaps processes strain and can't eliminate fully.Along with the increase of Heating temperature or the prolongation of hold-time, Ag is easy to separate out more.Yet if Heating temperature is higher than 600 ℃, Ag can be dissolved among the Cu again, and reduces electric conductivity thus.Therefore, Heating temperature is preferably below 600 ℃, is particularly preferably more than 350 ℃ and below 550 ℃, more preferably more than 400 ℃ and below 450 ℃.Hold-time is preferably more than 0.5 hour and below 10 hours.Cooling when separating out thermal treatment is undertaken by (for example) stove is cold, its objective is that the naturally cooling by being statically placed in the heat treatment furnace cools off.
[test case 1]
Adopt various conditions to prepare the Cu-Ag alloy material, and the content of research Ag and the relation between the electric conductivity.The result is shown in Fig. 1 and Biao I.
Prepare the Cu-Ag alloy material by following manner.Preparation purity is that electrolytic copper more than 99.99% is as raw material Cu.Preparation purity is that silver-colored particle (Ag) more than 99.99% is as raw material A g.They are put in the crucible of high purity carbon system, in continuous casting apparatus, carry out vacuum melting.Make thus the Cu that wherein contains melting and the mixed melting metal of Ag.Shown in Fig. 1 and Biao I, the amount of the silver-colored particle that adds to be regulated, the content (concentration) that makes the Ag in the mixed melting metal is 0.1 quality % to 15 quality %.
Use prepared mixed melting metal and high purity carbon mold processed, by cast continuously to make have rounded section, gauge or diameter of wire is the cast material of φ 8.0mm.In Fig. 1, carry out sample that naturally cooling obtain with the speed of cooling of 1.5 ℃/second (less than 8.5 ℃/second) by the represented sample of solid black triangle (casting (slow cooling)) when casting; By the represented sample of white filled squares (casting (quenchings)) for by the pressure cooling apparatus such as water-cooled copper is set, surrounding the solidified shell from mold, pull out, and cool off and the sample that obtains with the speed of cooling of 10 ℃/second (more than 8.5 ℃/second); For by to being carried out the sample (solution treatment material) that solution treatment obtains by the represented cast material of solid black trilateral (speed of cooling in the castingprocesses: 2.5 ℃/second), this solution treatment is that speed of cooling with 9 ℃/second (more than 1.5 ℃/second) was 760 ℃ of lower processing 2 hours by the sample (solution treatment) shown in the solid black rhombus.
[table I]
Learn that from table I and Fig. 1 even sample has same Ag content, but its electric conductivity is also distinguished to some extent according to the difference of creating conditions.Particularly, when Ag content was identical, (1) was compared with the lower situation of when casting speed of cooling, and the electric conductivity when speed of cooling is higher during casting is lower; (2) even the speed of cooling when casting is low, but by carrying out solution treatment electric conductivity is reduced after the casting.It is believed that, thereby the reduction of this electric conductivity is because speed of cooling when improving casting or formed Ag and be dissolved in state among the Cu by carry out solution treatment after casting, and this state has caused the electric conductivity reduction.Therefore, in order to indicate " Ag is dissolved in the state among the Cu ", the electric conductivity in the time of can be with casting under the low speed of cooling is as threshold value.
To considering about the approximate expression of the relation between the electric conductivity under Ag content and the low speed of cooling.By data shown in Figure 1, the electric conductivity in the time of will hanging down speed of cooling in casting is considered as with the linear function of Ag content as variable.The proximal line of the electric conductivity when the commercially available spreadsheet " Excel " that adopts Microsoft to make is determined to hang down speed of cooling in casting is tried to achieve C=(-0.1786) * x+97, wherein x (quality %) is Ag content, C is electric conductivity.By using approximate expression, " Ag is dissolved in the state among the Cu " can be the state that electric conductivity is less than or equal to the electric conductivity when hanging down speed of cooling in casting, and namely electric conductivity C (%IACS) satisfies the state of C≤(0.1786) * x+97.
[test case 2]
Adopt various conditions to prepare the Cu-Ag alloy material, and make the Cu-Ag alloy wire by material being carried out wire drawing and (if necessary) thermal treatment.Measure electric conductivity (%IACS) and the tensile strength (MPa) of Cu-Ag alloy wire.
Prepare each sample by following mode.Prepared the raw material identical with test case 1, and prepared the mixed melting metal that contains Cu and Ag, made it satisfy the Ag content (concentration) shown in table II.According to the mode identical with test case 1, by cast continuously to make have rounded section, gauge or diameter of wire is the cast material of φ 8.0mm.With different cooling conditionss cast material is cooled off in the casting, to reach the speed of cooling shown in the table II.Speed of cooling is lower than 8.5 ℃/second the sample of sample for cooling off by the mode of naturally cooling.Speed of cooling is that the sample more than 8.5 ℃/second is the sample through quenching, and described is by the configuration water-cooled copper block through the sample that quenches, to provide cooling air to cool off around the solidified shell of being pulled out by mold; Perhaps adopt the fan air blast to cool off; Perhaps adopt these to force the combination of cooling way to be cooled off.Temperature by suitable adjusting water-cooled copper block and air quantity etc., thereby different speed of cooling in realizing making.
In the hurdle of creating conditions of table II, only put down in writing the cast material of sample (2-1,2-3,2-3-2,2-5,2-7,2-10,2-12 and 2-14 sample), these samples are that final gauge or diameter of wire is the wire rod of φ 0.04mm, and this wire rod is obtained by following methods.That is, resulting each cast material is carried out wire drawing.When gauge or diameter of wire reaches gauge or diameter of wire shown in the table II, carrying out intermediate heat treatment (separating out thermal treatment) under the condition shown in the table II, and then carrying out wire drawing.
The sample (2-2,2-4,2-4-2,2-6,2-8,2-9,2-11,2-13 and 2-15 sample) of having put down in writing cast material and heat-treat condition in the hurdle of creating conditions of table II is the wire rod (Cu-Ag alloy wire) of φ 0.04mm for final gauge or diameter of wire, and this wire rod is obtained by following methods.That is, under the heat-treat condition resulting each cast material being heat-treated (solution treatment) shown in the table II, then carry out wire drawing.When gauge or diameter of wire reaches gauge or diameter of wire shown in the table II, carrying out intermediate heat treatment (separating out thermal treatment) under the condition shown in the table II, and then carrying out wire drawing.In thermal treatment (solution treatment) condition shown in the table II, " quenching " is illustrated in the cooling step and carries out water-cooled by Heating temperature.
The 2-100 sample is that final gauge or diameter of wire is the wire rod (Cu-Ag alloy wire) of φ 0.04mm, and this wire rod is obtained by following methods.That is, showing under the heat-treat condition shown in the II resulting cast material (gauge or diameter of wire: φ 8.0mm) heat-treat (solution treatment), then carry out wire drawing.When gauge or diameter of wire reaches gauge or diameter of wire shown in the table II, carrying out intermediate heat treatment under the condition shown in the table II, and then carrying out wire drawing.The 2-110 sample is that final gauge or diameter of wire is the wire rod (Cu-Ag alloy wire) of φ 0.04mm, and this wire rod is obtained by following methods.That is, to the resulting cast material (diameter of wire: φ 8.0mm) carry out wire drawing.When gauge or diameter of wire reaches gauge or diameter of wire shown in the table II, carrying out intermediate heat treatment under the condition shown in the table II, and then carrying out wire drawing.The 2-120 sample is that final gauge or diameter of wire is the wire rod (Cu-Ag alloy wire) of φ 0.04mm, and this wire rod is obtained by following methods.That is, in the situation of not carrying out solution treatment to the resulting cast material (diameter of wire: φ 8.0mm) carry out wire drawing, until reach the gauge or diameter of wire of φ 6.6mm.Under the condition shown in the Table II to the wire drawing material (gauge or diameter of wire: φ 6.6mm) heat-treat (solution treatment), then carry out wire drawing of gained.When gauge or diameter of wire reaches the gauge or diameter of wire of showing shown in the II, carrying out intermediate heat treatment under the condition shown in the table II, and then carrying out wire drawing.
Measure resulting each cast material (gauge or diameter of wire: φ 8.0mm) and the solution treatment material (gauge or diameter of wire: electric conductivity φ 8.0mm) (%IACS), described solution treatment material is by to cast material (gauge or diameter of wire: φ 8.0mm) carry out solution treatment and obtain.The result is shown in the table II.For each the Cu-Ag alloy wire through intermediate heat treatment (separating out thermal treatment), when the gauge or diameter of wire of Cu-Ag alloy wire during in intermediate heat treatment is φ 2.6mm or φ 0.9mm, measure its tensile strength (MPa) and electric conductivity (%IACS).The result is shown in the table II.In addition, when the final gauge or diameter of wire of each wire rod is φ 0.04mm, measure its tensile strength (MPa) and electric conductivity (%IACS).The result is shown in the table II.According to JIS Z 2241 (1998) tensile strength is measured (gauge length GL:10mm).By bridge method electric conductivity is measured.
[table II]
Learn that from the table II along with the increase of Ag content, intensity trends towards increasing.Particularly, find that 2-1 to 2-15 sample namely has high strength after thermal treatment, its electric conductivity of while is equal to or higher than cast material, and (this cast material makes under lower speed of cooling, casting in the reference table I (slow cooling)) electric conductivity, wherein 2-1 to 2-15 sample is that speed of cooling by will cast the time is made as 8.5 ℃/second, or by under given conditions cast material being carried out solution treatment, thereby form the solid-solution material that electric conductivity C (%IACS) satisfies C≤(0.1786) * x+97, this solid-solution material is carried out wire drawing, and the step of going forward side by side carries out specific thermal treatment (separating out thermal treatment) and makes.After reaching final gauge or diameter of wire, still has high strength even also found 2-1 to 2-15 sample.
By relatively obtaining following discovery between the identical sample of Ag content.With compared by the 2-3 that makes under the above-mentioned specified conditions, 2-4,2-3-2 and 2-4-2 sample, 2-100 sample and 2-110 sample have high conductivity after solution treatment, but when wire drawing just through the intensity after the Overheating Treatment and the intensity after reaching final gauge or diameter of wire lower, wherein said 2-100 sample is lower in the speed of cooling in when casting, Heating temperature and speed of cooling during in solution treatment are lower, and the speed of cooling of described 2-110 sample when casting is low and do not pass through solution treatment.Compare with the 2-4-2 sample with 2-4,2-3-2, the intensity of 2-120 sample that does not form specific solid-solution material before the wire drawing is lower.
Use microscope (500 times) that the cross section of 2-3-2 and 2-4-2 sample is observed.Fig. 2 shows by carrying out the image that the image processing obtains to observing image.Elongated ropy among Fig. 2 is to obtain by the Ag that separates out is stretched.Can be clear that fibrous Ag precipitate has micron-sized size, and length is about tens microns.
Next, will observe the Ag precipitate.In the time can in the fiber photo, confirming fibrous Ag precipitate, choose the observation sample of Ag precipitate in the part that does not have fibrous Ag precipitate.Preferably upward observe observing sample at profile (cross section on the Cu-Ag alloy wire wire-drawing direction), to get rid of fibrous Ag precipitate.Choose and be of a size of below the 1000nm * any field of view 1000nm below from observing sample, and the employing transmission type microscope observes, can confirm the Ag precipitate thus.
Fig. 3 shows the transmission type microscope photo (150000 times) in the cross section of 2-3,2-4 and 2-110 sample.Field of view is of a size of 440nm * 326nm.In the Ag precipitate that in field of view, exists, to through being that each precipitate particle (particulate) below the 100nm counts to maximum linear length after cutting, and measure the total area of this particulate.For the Ag precipitate, when complete particle occurring in the field of view, such particle is measured.When particle is positioned at the border of field of view and part when cracked, such particle is not measured.Fig. 4 is included in the Photomicrograph of Fig. 3 in the existing Ag precipitate, the explanatory view that the Ag as particulate is counted.The Ag that dotted line among Fig. 4 surrounds is considered particulate.For above-mentioned each sample, the area percentage of the precipitate in the total area of precipitate, the total area of particulate, the field of view and the area percentage of the particulate in the precipitate are shown in the table III.The table III shows the total area and the area percentage of 2-1 and 2-2 sample simultaneously.
[table III]
Through in the 2-3 sample of specific heat treatment, have 9 particulates in the field of view, and the area percentage of the particulate in the precipitate is 68.9%.By cast material being carried out in the 2-4 sample that solution treatment obtains, existing whole precipitates are particulate in the field of view, and the number of particulate is 23, greater than the number in the 2-3 sample.On the other hand, identical at Ag content but speed of cooling when casting is lower and do not implement in the 2-110 sample of solution treatment, existing granule amount is 4 in the field of view, and less than the number in 2-3 number and the 2-4 sample, and the area percentage of the particulate in the precipitate is 26.1%.Ag content be higher than 2-3 number and 2-4 sample 2-1 number and the 2-2 sample in, obtain the result similar with the 2-4 sample to 2-3 number.
Fig. 5 is the synoptic diagram of having described the microtexture of Cu-Ag alloy wire of the present invention.In the drawings, the Ag that the circular expression of the oblong object in the rectangular area and the black of solid line is separated out, the Ag of the circular expression dissolving of the white of solid line.Obtain as one of the electric conductivity of table shown in the II and reason of intensity may be because: have stretched fibrous A precipitate shown in Figure 2, produced thus fiber strengthening; Or owing to have the ultra tiny Ag particle of homodisperse nano level shown in Figure 3, thereby produced dispersion-strengthened; Or owing to formed the mixing microtexture of fibrous Ag precipitate and ultra tiny Ag particle.The mixing microtexture is considered to form by following operation.For example, as shown in Figure 5, make the Ag dissolving of separating out by cast material being carried out solution treatment, thereby increase the meltage of Ag.By the material through solution treatment is carried out wire drawing, make the Ag that does not dissolve by solution treatment be drawn as fibrous Ag precipitate.Separate out thermal treatment by further enforcement, a large amount of form with particulate of Ag of solid solution is separated out, form thus and mix microtexture.On the other hand, for example, if the speed of cooling when casting is lower, then relatively large Ag precipitate can be separated out in a large number.By wire drawing the Ag precipitate is stretched as mentioned above, even but implement the above-mentioned thermal treatment of separating out, there is not the Ag precipitate of obvious precipitate particle shape yet.Therefore, mainly only there is fibrous Ag precipitate.The difference of these Ag existences can cause the difference of above-mentioned intensity.
Learn also from test-results, compare with the sample that the speed of cooling in when casting is set to more than 8.5 ℃/minute that the sample of under given conditions cast material having been implemented solution treatment is tending towards having higher intensity.Gauge or diameter of wire during the specific heat treatment implemented when wire drawing is larger, and then the intensity of final gauge or diameter of wire is tending towards higher.In addition, in the identical situation of the electric conductivity that obtains after the specific heat treatment (separating out thermal treatment), along with the raising of the speed of cooling in solid-solution material forms, after the thermal treatment and the intensity that reaches behind the final gauge or diameter of wire be tending towards further increase.
Also obtain following discovery by test-results.When manufacturing contains the Cu-Ag alloy wire of Ag of specified quantitative, by the solid-solution material that fully dissolves of preparation Ag as carrying out the material of wire drawing, and to separating out thermal treatment through the wire rod of wire drawing, can obtain such wire rod, the electric conductivity of this wire rod is equal to or higher than the electric conductivity of the existing Cu-Ag alloy wire that contains equivalent Ag, and has simultaneously higher intensity.
The present invention is not limited to above-described embodiment, and can carry out suitable change within not exceeding scope of the present invention.For example, can suitably change Ag content, when casting speed of cooling, solution treatment condition (temperature, hold-time and speed of cooling), the gauge or diameter of wire when implementing solution treatment and separating out thermal treatment and separate out heat treated condition (Heating temperature and hold-time).
Industrial applicibility
Cu-Ag alloy wire of the present invention can be suitably as the electric wire of various Electrical and Electronic equipment, such as portable electric appts such as mobile telephones, be loaded into electronic unit, medicine equipment and industrial robot etc. on the automobile etc.As a rule, the Cu-Ag alloy wire can suitably be used as the conductor (centre conductor and shielded conductor) of concentric cable.Method according to manufacturing Cu-Ag alloy wire of the present invention can be suitably for the manufacture of having high conductivity and high-intensity Cu-Ag alloy wire of the present invention.Concentric cable of the present invention and coaxial cable bunch of the present invention can suitably be used for the supply lead of above-mentioned various Electrical and Electronic equipment.
Reference symbol
1 concentric cable
11 centre conductors
12 isolators
13 external conductors
14 oversheaths
Claims (8)
1. Cu-Ag alloy wire, it is made of the copper alloy that contains Ag, and this Cu-Ag alloy wire comprises:
The Ag that 0.1 quality % is above and 15 quality % are following, surplus is Cu and impurity,
Wherein, be of a size of below the 1000nm when in the cross section of described Cu-Ag alloy wire, choosing * during any field of view below the 1000nm, in this field of view in the existing Ag precipitate, be that the area percentage of the Ag precipitate below the 100nm is more than 40% to cutting rear maximum linear length.
2. Cu-Ag alloy wire according to claim 1, wherein said Ag precipitate also comprises fibrous precipitate.
3. concentric cable comprises: have at least 1 wire rod centre conductor, coat the isolator of this centre conductor and be arranged at external conductor around this isolator,
Wherein said wire rod is Cu-Ag alloy wire according to claim 1 and 2.
4. coaxial cable bunch comprises many concentric cable according to claim 3 of bunchy.
5. a method of making the Cu-Ag alloy wire is wherein made wire rod by the cast material that is made of the copper alloy that contains Ag is carried out wire drawing, and the method comprises:
Form solid-solution material with as will be by the material of wire drawing, the electric conductivity C of this solid-solution material (%IACS) satisfies C≤(0.1786) * x+97, and wherein x (quality %) is the content (0.1 quality %≤x≤15 quality %) of Ag, and
Under the Heating temperature more than 300 ℃, the described wire rod through wire drawing is carried out at least one times thermal treatment, this heat treated hold-time is more than 0.5 hour.
6. the method for manufacturing according to claim 5 Cu-Ag alloy wire,
Wherein said solid-solution material forms by described cast material is carried out solution treatment, and
Described solution treatment is with the speed of cooling more than 1.5 ℃/second, what the time of maintenance more than 0.5 hour carried out under the Heating temperature more than 600 ℃.
7. according to claim 5 or the methods of 6 described manufacturing Cu-Ag alloy wires, wherein said cast material is to be controlled at more than 8.5 ℃/second by the speed of cooling that will cast the molten metal in the step to form.
8. Cu-Ag alloy wire, its by according to claim 5 in 7 the method for the described manufacturing of any one Cu-Ag alloy wire make, this Cu-Ag alloy wire comprises:
The Ag that 0.1 quality % is above and 15 quality % are following, surplus is Cu and impurity,
Wherein gauge or diameter of wire is below the 1000 μ m.
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| JP2010103686 | 2010-04-28 | ||
| JP2010-103686 | 2010-04-28 | ||
| JP2010230069A JP5713230B2 (en) | 2010-04-28 | 2010-10-12 | Cu-Ag alloy wire and method for producing Cu-Ag alloy wire |
| JP2010-230069 | 2010-10-12 | ||
| PCT/JP2011/060291 WO2011136284A1 (en) | 2010-04-28 | 2011-04-27 | Cu-Ag ALLOY WIRE AND METHOD FOR PRODUCING Cu-Ag ALLOY WIRE |
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| CN105261422A (en) * | 2015-10-30 | 2016-01-20 | 西北有色金属研究院 | Preparation method of high-strength high-conductivity copper-silver alloy wire |
| CN108288523A (en) * | 2017-01-10 | 2018-07-17 | 日立金属株式会社 | The manufacturing method of conductor wire, the manufacturing method and cable of conductor wire and casting conductor wire and cable |
| CN108368565A (en) * | 2016-05-16 | 2018-08-03 | 古河电气工业株式会社 | Copper series alloy wire rod |
| CN117545865A (en) * | 2022-06-07 | 2024-02-09 | 昭和电线电缆株式会社 | Cu-Ag alloy wire and method for manufacturing same |
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| KR20230138448A (en) | 2021-11-12 | 2023-10-05 | 후루카와 덴키 고교 가부시키가이샤 | Cu-Ag alloy wire |
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| KR20130093469A (en) | 2013-08-22 |
| CN102869805B (en) | 2014-12-03 |
| KR20170121307A (en) | 2017-11-01 |
| KR20180011344A (en) | 2018-01-31 |
| KR101870603B1 (en) | 2018-06-22 |
| WO2011136284A1 (en) | 2011-11-03 |
| KR101843707B1 (en) | 2018-03-29 |
| KR101790812B1 (en) | 2017-10-26 |
| JP5713230B2 (en) | 2015-05-07 |
| TW201142048A (en) | 2011-12-01 |
| JP2011246802A (en) | 2011-12-08 |
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