CN102639731A - Titanium-copper for electronic component - Google Patents
Titanium-copper for electronic component Download PDFInfo
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- CN102639731A CN102639731A CN2010800532889A CN201080053288A CN102639731A CN 102639731 A CN102639731 A CN 102639731A CN 2010800532889 A CN2010800532889 A CN 2010800532889A CN 201080053288 A CN201080053288 A CN 201080053288A CN 102639731 A CN102639731 A CN 102639731A
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- copper alloy
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
Provided is titanium-copper which has excellent strength and bendability. The titanium-copper is a copper alloy for electronic components which contains 2.0-4.0 mass% Ti, the remainder comprising copper and incidental impurities. The intensity peak of X-ray diffraction from the {220} crystal plane in a rolled surface of the copper alloy has a half-value width [beta]{220} which satisfies the relationship 3.0=<[beta]{220}/[beta]0{220}<=6.0, wherein [beta]0{220} is the half-value width of the intensity peak of X-ray diffraction from the {220} crystal plane of a standard powder of pure copper. The copper alloy, in a structure examination of a section parallel to the rolling direction, has an average crystal-grain diameter of 30 [mu]m or smaller in terms of equivalent-circle diameter.
Description
Technical field
The present invention relates to be suitable as the titanium copper and the method for manufacture thereof of electronic component-use members such as junctor.
Background technology
In recent years, be that the miniaturized of the electronic machine of representative makes progress day by day with mobile termination etc., therefore, wherein employed junctor requires the tendency of thin spaceization and slimming remarkable.Miniature connector require more its pin widths narrow, form folding very little machining shape, therefore, employed member requires to have HS obtaining necessary elasticity, and has the bendability of the excellence of bending machining that can anti-harshness.In this respect, the strength ratio of copper alloy (below be called " titanium copper ") that contains titanium is higher, is the most excellent in the copper alloy aspect stress relaxation characteristics, therefore, is that terminal uses with member as intensity is had the signal of special demands all the time.
Titanium copper is the copper alloy of age hardening type.Form the supersaturated solid solution of solute atoms Ti through solution treatment, implement the thermal treatment of long period by this state with low temperature, then because unstability is decomposed, make that the cyclical movement of Ti concentration---modulated structure develops in parent phase, intensity improves.The problem that occur this moment is: intensity and bendability are opposing characteristic this point.That is, then bendability is impaired to improve intensity, on the contrary, if pay attention to bendability then can't obtain desirable strength.Usually, improve cold rolling rate of compression, the dislocation amount that then imports increases, and dislocation desity improves, and therefore increases to help the nucleation site separated out, can improve the intensity after the ageing treatment, if but excessively improve rate of compression then the bendability variation.Therefore, make intensity and bendability and deposit the problem that becomes research.
For this reason, people are from following viewpoint, have proposed to make intensity and the bendability of titanium copper and the technology of depositing: add Fe, Co, Ni, Si grade in an imperial examination element (patent documentation 1); Be limited in the concentration of the impurity element group of solid solution in the parent phase, as the second phase particle (Cu-Ti-X is a particle), its distributional pattern with regulation separated out, them to improve the systematicness (patent documentation 2) of modulated structure; To the trace additives that can make grain refining effectively with second mutually Particle Density stipulate (patent documentation 3); Make grain refining (patent documentation 4) etc.
Under the situation of titanium copper,, there is the β phase (TiCu of consistence difference with respect to parent phase α phase
3) with the β ' of high conformity (TiCu mutually
4), β has detrimentally affect with respect to bendability, and β ' is disperseed evenly and imperceptibly mutually, help intensity and bendability and deposit, therefore, people have also proposed in inhibition β phase, to make the mutually microdispersed titanium copper of β ' (patent documentation 5).
Following technology has also been proposed: be conceived to crystalline orientation, proposed to make it satisfy I{420}/I through the control crystalline orientation
0{ 420}>1.0 and I{220}/I
0{ 220}≤3.0 are improved intensity, bendability and proof stress slackness (patent documentation 6) thus.
The prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2004-231985 communique
Patent documentation 2: TOHKEMY 2004-176163 communique
Patent documentation 3: TOHKEMY 2005-97638 communique
Patent documentation 4: TOHKEMY 2006-265611 communique
Patent documentation 5: TOHKEMY 2006-283142 communique
Patent documentation 6: TOHKEMY 2008-308734 communique.
Summary of the invention
As stated, for intensity and the bendability that improves titanium copper, former studies the whole bag of tricks, but still have room for improvement.Therefore, one of problem of the present invention is to carry out the characteristic improvement of titanium copper with viewpoint different trial in the past, to provide to have the excellent intensity and the titanium copper of bendability.Another problem of the present invention provides the method for manufacture of this titanium copper.
Titanium copper method of manufacture in the past is the order formation by the founding → homogenizing annealing → hot rolling of ingot → (annealing with cold rolling carry out repeatedly) → final solution treatment → cold rolling → ageing treatment basically.The described titanium copper of background technology also is by same order manufacturing.
The inventor is finding for solving in the process that above-mentioned problem studies: with the order of the cold rolling and ageing treatment of carrying out after the final solution treatment with carried out on the contrary in the past; Promptly replace with ageing treatment → cold rolling order; And implement stress relieving with suitable condition at last, then bendability significantly improves.That is, will compare with titanium copper of the present invention by the titanium copper of in the past order manufacturing, then the bendability of titanium copper of the present invention is more excellent under same intensity.The inventor studies titanium copper tissue of the present invention in order to investigate its reason, and the result finds on the form of dislocation desity and crystal grain, to have unique point.Specifically, carry out when cold rolling with identical rate of compression, compare during with the order that adopts cold rolling → ageing treatment, when adopting the order of ageing treatment → cold rolling, the dislocation desity of gained titanium copper raises.In other words, can be reduced to and obtain identical dislocation desity essential rate of compression when cold rolling.Rate of compression is little, and crystal grain is in the extension of rolling direction in the time of then can suppressing cold rolling, so bendability can improve.
Dislocation desity is difficult to direct mensuration.Its reason is the skewness that causes dislocation owing to the distribution of modulated structure or precipitation particles.Attempting indirect when estimating, find with calendering face on { half breadth at the X-ray diffraction intensity peak of 220} crystal face is relevant.Half breadth is the width (β) of 1/2 intensity place diffraction intensity curve of peak intensity in the diffraction intensity curve, with 2
θExpression.Along with the rising of cold rolling shrinkage, half breadth increases with dislocation desity.Therefore, among the present invention, be index with this half breadth, the state of indirect predetermined bits dislocation density.
One aspect of the present invention of accomplishing according to above-mentioned cognition is the electronic component-use copper alloy; This electronic component-use copper alloy contains 2.0-4.0 quality %Ti; Rest part contains copper and unavoidable impurities; Wherein, from the calendering face the half breadth β at the X-ray diffraction intensity peak of 220} crystal face 220} with from { the half breadth β at the X-ray diffraction intensity peak of 220} crystal face of fine copper standard powder
0220} satisfies following formula:
3.0≤β{220}/β
0{220}≤6.0，
And in the structure observation in the cross section parallel with rolling direction, the average crystalline particle diameter is represented with equivalent circle diameter, is below the 30 μ m.
In the embodiment of copper alloy of the present invention; In the structure observation in the cross section parallel with rolling direction, the average crystalline particle diameter (L) of the direction parallel with rolling direction is 1-4 with respect to the ratio (L/T) with the average crystalline particle diameter (T) of the rectangular direction of rolling direction.
In another embodiment of copper alloy of the present invention, the spring limit is 600-1000 MP a.
In the another embodiment of copper alloy of the present invention, the spring limit is 300-600 MPa.
In the another embodiment of copper alloy of the present invention, with add up to 0-0.5 quality % to contain to be selected from as among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P of triad more than a kind or 2 kinds.
Another aspect of the present invention is forging copper product (stretching the copper article), and this forging copper product contains above-mentioned copper alloy.
Another aspect of the present invention is an electronic unit, and this electronic unit possesses above-mentioned copper alloy.
Another aspect of the present invention is a junctor, and this junctor possesses above-mentioned copper alloy.
Another aspect of the present invention is the method for manufacture of electronic component-use copper alloy; Wherein, Carry out solution treatment Cu alloy material is heated to the solid solution limit of the Ti temperature when identical with addition under 730-880 ℃ more than; Said Cu alloy material contain 2.0-4.0 quality %Ti, with add up to 0-0.5 quality % to contain to be selected from arbitrarily as among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P of triad more than a kind or 2 kinds, and rest part contains copper and unavoidable impurities;
After solution treatment, under material temperature 400-500 ℃, heat 0.1-20 hour ageing treatment;
After ageing treatment, carrying out rate of compression is the finally cold rolling of 0-40%.
Comprise in the embodiment of the method for manufacture of copper alloy of the present invention: carry out stress relieving final after cold rolling, this stress relieving is with material temperature more than 100 ℃ but be lower than 350 ℃ of heating more than 0.001 hour below 40 hours; With material temperature more than 350 ℃ but be lower than 550 ℃ of heating more than 0.0001 hour below 20 hours; Or with material temperature heating below 700 ℃ more than 0.0001 hour below 0.003 hour more than 550 ℃.
Comprise in the another embodiment of the method for manufacture of copper alloy of the present invention: carry out stress relieving final after cold rolling, this stress relieving is with material temperature more than 200 ℃ but be lower than 400 ℃ of heating 0.001-20 hour.
According to the present invention, can obtain the titanium copper of intensity and excellent in bending workability.
The invention embodiment
< titanium content >
Titanium is lower than the strengthening mechanism that formation that 2.0 quality % then can't fully obtain titanium copper modulated structure originally brings, and therefore can't obtain enough intensity, on the contrary, surpasses 4.0 quality %, then separates out thick TiCu easily
3, intensity and bendability have the variation tendency.Therefore, the Ti content in the copper alloy of the present invention is 2.0-4.0 quality %, preferred 2.7-3.5 quality %.As stated, suitable through the content that makes Ti, can realize being fit to the intensity and the bendability of electronic component-use simultaneously.
< element >
In titanium copper, add the element of regulation, though then with Ti fully the high-temperature of solid solution carry out solution treatment, crystal grain is refinement easily also, has the effect of the intensity of making raising.In addition, the element of regulation promotes the formation of modulated structure.And then also to have further inhibition Ti-Cu be the effect of rapid thickization of stable phase.Therefore can obtain titanium copper age hardening performance originally.
In the titanium copper, that above-mentioned effect is the highest is Fe.Mn, Mg, Co, Ni, Si, Cr, V, Nb, Mo, Zr, B and P also can expect the effect consistent with Fe, add also visual effects separately, also can compound interpolation more than 2 kinds.
Also can show above-mentioned effect though total contains above these elements of 0.05 quality %, add up to surpass 0.5 quality %, then the balance of intensity and bendability has the variation tendency.Therefore, can with add up to 0-0.5 quality % to contain to be selected from as among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P of triad more than a kind or 2 kinds, contain 0.05-0.5 quality % preferred the total.
< crystal particle diameter >
For the intensity and the bendability that improve titanium copper, little crystal grain is suitable.Therefore, preferred average crystalline particle diameter is below the 30 μ m, more preferably below the 20 μ m, below the further preferred 10 μ m.Do not limit for lower limit is special, but since crystal particle diameter distinguish the difficulty that becomes, therefore with such situation as less than 1 μ m (< 1 μ m), so little particle diameter is also contained in the scope of the present invention.But, if become extremely little, then stress relaxation characteristics reduces, therefore when the needs stress relaxation characteristics, more than the preferred 1 μ m.Among the present invention, the average crystalline particle diameter is through with the expression of getting off: under through opticmicroscope or electron microscope observation, and the equivalent circle diameter in the structure observation in the cross section parallel with rolling direction.
Usually, crystal grain presents the elliptical shape that extends along rolling direction according to final cold rolling rate of compression, and is preferred as far as possible near just round in order to improve bendability, makes the shape of crystal grain not have anisotropy.Among the present invention,, therefore can obtain on rolling direction, to extend few crystal grain owing to can reduce cold rolling rate of compression.But, too reduce final cold rolling rate of compression, then can make undercapacity for the approaching just circle of the shape that makes crystal grain.Therefore; In the embodiment of titanium copper of the present invention; In the structure observation in the cross section parallel through electron microscope with rolling direction, with the average crystalline particle diameter (L) of rolling direction parallel direction with respect to the ratio (L/T) of the average crystalline particle diameter (T) of the rectangular direction of rolling direction (below be called " crystal grain long-width ratio ".) be 1-4, preferred 1.5-3.5, more preferably 2-3.
< half breadth >
Among the present invention, adopt calendering face { half breadth at the X-ray diffraction intensity peak of 220} crystal face is as the index of dislocation desity.This for the foregoing reasons.In the titanium copper of the present invention, from the calendering face the half breadth β at the X-ray diffraction intensity peak of 220} crystal face 220} with from { the half breadth β at the X-ray diffraction intensity peak of 220} crystal face of fine copper standard powder
0220} satisfies following formula:
3.0≤β{220}/β
0{220}≤6.0
β { 220} and β
0{ 220} measures under the same measured condition.Fine copper standard powder is defined as the copper powder of the purity 99.5% of 325 orders (JIS Z8801).
β { 220}/β
0{ 220} reduces along with the reduction of dislocation desity, on the contrary, also raises along with the rising of dislocation desity.β { 220}/β
0{ 220} reduces, and then bendability improves but the intensity reduction.On the contrary, β { 220}/β
0{ 220} increases, and then intensity improves but the bendability reduction.For realize intensity and bendability and deposit, must be 3.0≤β { 220}/β
0{ 220}≤6.0, preferred 3.5≤β { 220}/β
0{ 220}≤5.0.As in the past after final solution treatment in the method for manufacture in sequence according to cold rolling → ageing treatment, in order to make β { 220}/β
0220} is about 3.0, and must carry out rate of compression near 50% cold rolling, but in the method for manufacture of the present invention, can realize with rate of compression about 10%.Therefore, can improve dislocation desity (intensity), reduce the crystal grain long-width ratio simultaneously, that is, not damage bendability.
< spring limit >
In the copper alloy of the present invention, can be of the back, in final operation, implement stress relieving according to whether and come the regulating spring elastic limit.Therefore, can in the condition that keeps above-mentioned half breadth or crystal grain, reach desired spring limit.For example in an embodiment of copper alloy of the present invention; The spring limit that can have 300-1000 MPa in the embodiment with high spring elastic limit, can be 600-1000 MPa; Preferred 800-1000 MPa; In embodiment with low spring limit, can be 300-600 MPa, be preferably 400-600 MPa.
< purposes >
Copper alloy of the present invention can be used as various forging brass works for example plate, bar, pipe, rod and line and provide.Titanium copper of the present invention is unrestricted, can be suitable as electronic unit materials such as switch, junctor, socket, terminal, rly. and use.
< method of manufacture >
Titanium copper of the present invention can be especially through implementing suitable thermal treatment and cold rolling the manufacturing in final solution treatment and operation afterwards.Below according to the per pass operation suitable manufacturing example is described successively.
1) manufacturing of ingot
Manufacturing through fusion and the ingot that carries out of casting is to carry out in a vacuum or in the inert gas atmosphere basically.The fusion residue that adds element is arranged in fusion, and then the raising to intensity can't act on effectively.Therefore, in order to eliminate the fusion residue, dystectic element such as Fe or Cr must fully stir after adding, and keep certain hour.And the Ti ratio is easier to be dissolved among the Cu, therefore can add in element dissolving back.Therefore; It is desirable to make as follows ingot: in Cu, add be selected among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P more than a kind or 2 kinds; It is contained to add up to 0-0.5 quality %, then add Ti, it is contained with 2.0-4.0 quality %.
2) homogenizing annealing and hot rolling
Because the solidifying segregation or the crystallisate that produce when ingot is made are thick, thereby therefore it is desirable to make its solid solution that it is reduced as far as possible, and eliminate as far as possible through homogenizing annealing.This is effective for preventing bending crack.
Specifically, preferably at ingot manufacturing process post-heating to 900-970 ℃ of homogenizing annealing that carries out 3-24 hour, implement hot rolling then.For preventing liquid metal fragility, before the preferred hot rolling be below 960 ℃ in the hot rolling, and be that 90% passage (pass) is more than 900 ℃ by original thickness to reduced overall rate.Reduce the segregation of Ti in order to cause suitable recrystallize effectively, can implement the draught of each passage with 10-20 mm in each passage.
3) the 1st solution treatment
Afterwards, preferably suitably carry out repeatedly with annealing cold rolling, carry out solution treatment then, here, the reason of carrying out solid solution in advance is in order to alleviate the burden of final solution treatment.That is, final solution treatment is not the thermal treatment that is used to make the second phase particle solid solution, but because solid solution needs only this state of maintenance and only causes recrystallize simultaneously, therefore, can accomplish with slight thermal treatment.Specifically, it is 850-900 ℃ that first solution treatment can make Heating temperature, carries out 2-10 minute.The heat-up rate of preferred this moment and speed of cooling do not make the second phase particle separate out at this as quickly as possible yet.Also can not carry out first solution treatment.
4) calendering in the middle of
In the calendering, improve rate of compression more and then can the recrystallize particle in the final solution treatment be controlled to be even and fine more in the middle of before final solution treatment.Therefore, the rate of compression of middle calendering is preferably 70-99%.Rate of compression is with { (thickness before (thickness after the thickness-calendering before the calendering)/calendering) * 100%} definition.
5) final solution treatment
In the final solution treatment; It is desirable to make the complete solid solution of precipitate, if but be heated to high temperature in order to eliminate fully, then crystal grain is thick easily; Therefore Heating temperature is that (addition of Ti is when the scope of 2.0-4.0 quality % near the solid solution limit formed of the second phase particle temperature; The solid solution limit of Ti is about 730-840 ℃ with the mutually isochronous temperature of addition, when for example the addition of Ti is 3.0 quality %, is about 800 ℃).If quickly heat up to this temperature and make speed of cooling also fast, then can suppress the generation of the thick second phase particle.Therefore; Typical mode is to heat most more than 730-880 ℃ of such solid solution limit that makes Ti temperature identical with addition; More typical is to be heated to than the 730-880 ℃ of high 0-20 of temperature ℃ the temperature that such solid solution limit that makes Ti is identical with addition, preferred high 0-10 ℃ temperature.
In addition, the heat-up time of final solution treatment is short more, then can suppress the alligatoring of crystal grain more.For example can be 30-90 second heat-up time, is typically 30-60 second.At this constantly, even produce the second phase particle, as long as fine and dispersion equably is then almost harmless to intensity and bendability.But thick particle has the tendency of further growth in final ageing treatment, therefore, at this constantly, even it is also necessary as far as possible less, as far as possible little to have generated the second phase particle.
6) ageing treatment
After final solution treatment, carry out ageing treatment.Normally after final solution treatment, carried out cold rollingly in the past, but in order to obtain titanium copper of the present invention, importantly after final solution treatment, do not carry out cold rollingly, but carried out ageing treatment immediately.Its reason is, and before ageing treatment, carries out cold rolling contrast, even also can improve dislocation desity under the same rate of compression.The present invention is not intended to receive theoretical qualification, but can think that this is relevant with the generation of shear zone with intragranular crystallinity.Usually roll, then import dislocation, so the crystal strain, half breadth increases.The little then crystallinity of half breadth is high, and half breadth greatly then crystallinity is low.Under the high state of crystallinity, carry out go forward side by side line bend processing of ageing treatment, then shear zone develops easily, forms the reason of bending crack easily.When after solid solution, carrying out timeliness, intragranular evenly carries out evolution reaction, modulated structure or fine second phase particle easy and uniform development.After being controlled to be such tissue, carry out cold rollingly, compare when not carrying out timeliness through timeliness, crystal strain more easily, shear zone more is difficult to development.But degree of finish improves then that dislocation desity excessively increases, and diminishes bendability.Therefore, even low degree of finish also can suppress the development of shear zone, obtain HS simultaneously.Ageing treatment is after solution treatment, to carry out ageing treatment, therefore, reduces as the strain of separating out motivating force, so can carry out under the high temperature slightly than common aging condition.Specifically, preferably heated 0.1-20 hour down, more preferably heated 1-16 hour down at material temperature 400-480 ℃ at material temperature 400-500 ℃.
7) final cold rolling
Carry out final cold rolling after the above-mentioned ageing treatment.Can improve the intensity of titanium copper through final cold rolling processing.Can not implement also that this is cold rolling, but when obtaining HS and be purpose, rate of compression is more than 5%, and is preferred more than 10%, more preferably more than 15%.But, the long-width ratio of the too high then crystal grain of rate of compression increases excessive, and the raising effect of bendability reduces, and therefore, rate of compression is below 40%, and is preferred below 30%, more preferably below 25%.
8) stress relieving
According to the structure of electronic unit, require different shape processing.Usually, implement the position of viscous deformation such as bending machining or grooving processing and carry out work hardening, the strength of materials more improves.Guarantee that by such bending machining portion the structure of crimping is difficult to viscous deformation, therefore do not need high spring limit.Therefore in such use, can not carry out stress relieving.
On the other hand; Add the position that does not receive viscous deformation man-hour by the shape after punching press and guarantee that the structure of crimping is (for example by the structure of straight line portion (arm) distance of contact portion to the bending machining portion of terminal;, be the structure that stress in bending puts on arm perhaps like the structure of not implementing grooving processing or bending machining of forked terminal), the resistance to sag must be arranged; Therefore, high spring limit is important.
Therefore, particularly therein in the important purposes of spring limit, carry out stress relieving after cold rolling final.Be 3% when above particularly, preferably carry out stress relieving in the important purposes of spring limit therein in final cold rolling rate of compression.In addition, be 10% when above in final cold rolling rate of compression, especially preferably carry out stress relieving in the important purposes of spring limit therein.The condition of stress relieving can be habitual condition, but the dislocation uneven distribution through cold rolling importing.Through carrying out stress relieving, make dislocation rearrangement, can realize the further raising of intensity thus.But, if excessively carry out stress relieving, then dislocation disappears, and intensity reduces, and is therefore not preferred.Therefore, for example can be with material temperature more than 100 ℃ but be lower than 350 ℃ and carry out the heating below 40 hours more than 0.001 hour; With material temperature more than 350 ℃ but be lower than 550 ℃ and carry out the heating below 20 hours more than 0.0001 hour; Perhaps carry out the heating below 0.003 hour more than 0.0001 hour more than 550 ℃ below 700 ℃ with material temperature; Preferably in material temperature more than 200 ℃ but be lower than under 0.001-20 hour the condition of 400 ℃ of heating and carry out; More preferably in material temperature more than 350 ℃ but be lower than under 0.001-0.5 hour the condition of 550 ℃ of heating and carry out, more preferably if low temperature then with long-time (for example with material temperature 200-300 ℃ of heating 10-20 hour) if high temperature then carries out with the condition of short period of time (for example with heating below material temperature 550-700 ℃ 0.001-0.003 hour).
Those skilled in the art should understand, and can in the intermittence of above-mentioned each operation, suitably be used to remove operations such as grinding of surperficial oxide debris cut, grinding, sandblast pickling.
Embodiment
Below with comparative example embodiments of the invention are shown, these embodiment provide in order to understand the present invention and advantage thereof better, are not intended to limit invention.
When making the copper alloy of the present invention's example, add reactive metal Ti, therefore, adopt the vacuum melting stove in founding as the 2nd composition.In addition, sneaking into of the impurity element beyond the element given to this invention possibly cause envisioning outer spinoff generation, and for preventing trouble before it happens, raw material needs the strict higher material of purity of choosing to use.
At first, press shown in the table 1 and form, in Cu, add Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P respectively, add the Ti that forms shown in this table then respectively.Take into full account the hold-time after the interpolation, make and add element and do not have the fusion residue, then they are injected mold under Ar atmosphere, make the ingot of about 2 kg respectively.
[table 1]
Table 1. adds element (quality %)
Under 950 ℃,, carry out homogenizing annealing, under 900-950 ℃, carry out hot rolling then, obtain the hot-rolled sheet of thickness of slab 10 mm above-mentioned ingot heating 3 hours.Through surfacing deoxygenated skin, carry out cold rollingly then, process thickness of slab (2.0 mm) base bar, carry out the 1st solution treatment with the base bar.The condition of the 1st solution treatment is to heat 10 minutes down at 850 ℃.In a part of embodiment, do not carry out the 1st solution treatment.Then, in intermediary is cold rolling, cold rolling adjusting intermediary thickness of slab, making final thickness of slab is 0.10 mm, but is inserted into then in the lehre of rapid heating, carries out final solution treatment, then water-cooled.The heating condition of this moment is: the temperature when the solid solution limit of material temperature and Ti is identical with addition (during Ti concentration 3.0 quality %, is about 800 ℃; During Ti concentration 2.0 quality %, be about 730 ℃; During Ti concentration 4.0 quality %, be about 840 ℃) unanimity, and kept respectively 1 minute according to the heating condition shown in the table 2.Then, in Ar atmosphere, carry out ageing treatment according to the said condition of table 2.Cold rolling through carrying out according to the said condition of table 2 behind the pickling deoxygenated skin, anneal according to said each heating condition of table 2 at last, process the test film of invention example and comparative example.According to the difference of test film, can omit the ageing treatment that is right after after the solution treatment.
[table 2]
For each test film of gained, carry out evaluating characteristics according to following condition.The result is as shown in table 3.
< intensity >
Use press, make the JIS13B test film, make draw direction parallel with rolling direction.Carry out the tension test of this test film according to JIS-Z2241, measure 0.2% ys (YS) of calendering parallel direction.
<bendability >
A:W is crooked
According to JIS H3130, using bending radius is the W pliability test of the mould enforcement Badway (bending axis and rolling direction are same direction) of 2 times of thicknesss of slab, is made as zero when crackle does not take place, be made as when crackle takes place *.
B:180 ° of bending
Test film is pressed on the angle of piece of fillet radius (R), carries out 90 ° of bendings, at the plate (fillet radius R) of 2 times of thickness (2R) of inboard this fillet radius of clamping of 90 ° of bending machining portions, along 180 ° of the end face bendings of plate with regulation.Minimum bending radius (R) when outside curved surface does not produce the crack after 180 ° of bending machining is divided by thickness of slab (t), with the index of income value (R/t) as bendability.
Each 0.01 mm that changes of fillet radius.
< specific conductivity >
According to JIS H0505, measure specific conductivity (EC:%IACS) through four-terminal method.
< average crystalline particle diameter >
The mensuration of average crystalline particle diameter is to cut off with the cross section that FIB will be parallel with rolling direction, and the cross section is exposed, and SIM observes the cross section then, and the number of dies of tally's area is obtained the leveled circular equivalent diameter of crystal grain.Specifically, make the frame of 100 μ m * 100 μ m, counting is present in the number of the crystal grain in this frame.For all counting across the crystal grain of in-out-snap is 1/2.Area 10000 μ m with frame
2Add up to divided by this, obtain the MV of the area of per 1 crystal grain.Positive circular diameter with this area is an equivalent circle diameter, therefore with it as the average crystalline particle diameter.
< crystal particle diameter long-width ratio >
Through electrolytic polishing the tissue in the cross section parallel with rolling direction is exposed, take the field of view of 100 μ m * 100 μ m afterwards through electron microscope (Philips manufactured, XL30 SFEG).According to JIS H0501, through the process of chopping obtain with the average crystalline particle diameter of the rectangular direction of rolling direction and with the average crystalline particle diameter of rolling direction parallel direction, calculate long-width ratio.
< half breadth >
To each test film, use the X-ray diffraction device of the model rint Ultima2000 that motor of science society makes, obtain the diffraction intensity curve of calendering face by following condition determination, measure { half breadth β { the 220} at the X-ray diffraction intensity peak of 220} crystal face.With same condition determination fine copper powder standard test specimen is obtained half breadth β
0{ 220}.In the copper powder standard test specimen, { 2 of the peak of 220} face
θNear 74 °, occur.
Target: Cu manages ball
Tube voltage: 40 kV
Tube current: 40 mA
Sweep velocity: 5 °/minute
Sampling width: 0.02 °
Measurement range (2
θ): 60 °-80 °.
< spring limit (Kb) >
Spring limit (Kb) is to implement the repeatedly flexure test according to JIS H3130 (alloy numbering C1990), measures surperficial maximum stress by the moment of flexure of residual permanent strain.
[table 3]
< investigation >
Intensity and the bending machining sexual balance that can know the routine No.1-25 of invention improve well.Inventing routine 13-26 is the variation that manufacturing process is applied variation.In the invention example 13, set the 2nd time solid solution temperature higher, obtain the average crystalline particle diameter of the upper limit.Final cold rolling rate of compression is low in the invention example 14, and therefore, β is the lower limit of institute's claimed range, and long-width ratio also reduces, but also in the scope of regulation of the present invention, therefore, intensity and bending machining sexual balance improve well.Invention example 15 is compared with the routine No.4 of invention, is the result who aging temperature is set at lower limit.Invention example 16 is compared with the routine No.4 of invention, is the result who aging temperature is set at the upper limit.Invention example 17 and 18 is to have omitted the example of inventing routine No.2 and the operation stress relieving of inventing routine No.4 respectively, even can know and omitted stress relieving, still in specialized range of the present invention, intensity and bending machining sexual balance improve the β value well.With respect to invention example 17 and 18, invention example 19,20 and 21 has been carried out stress relieving, and intensity and Kb value improve thus.Inventing routine 22-25 is the example that omits the 1st solution treatment; And then No.24 and 25 is the examples that do not carry out stress relieving; Omit the 1st time solution treatment and do not carry out stress relieving even can know; Still in specialized range of the present invention, intensity and bending machining sexual balance improve the β value well.Invention example 26 is the examples that carry out stress relieving with the low temperature short period of time.
On the other hand, in comparative example No.1-3, after solution treatment, do not carry out ageing treatment but carry out cold rollingly, so half breadth is little, and the equilibrium ratio invention example of intensity and bendability is poor.In addition, among the comparative example No.4-5, after solution treatment, carried out ageing treatment, but in comparative example No.4, cold rolling rate of compression improves, half breadth excessively increases, so the equilibrium ratio of intensity and bendability invention example is poor.Among the comparative example No.5, the Heating temperature of solution treatment is too high, so crystal particle diameter increases.Final cold rolling rate of compression is high, although therefore obtained higher intensity, bendability is poor.Among the comparative example No.6,7,9 and 10, solid solubility temperature is too high, so crystal particle diameter surpasses the upper limit, bendability variation.In addition, in comparative example 7 and 8, do not carry out ageing treatment after the solution treatment but carry out cold rollingly, so half breadth is little, the balanced differences of intensity and bendability.Comparative example No.11 at high temperature carries out stress relieving, so initial recrystallization, causes dislocation desity to reduce and the β reduction, and begins solid solution again, therefore causes intensity and specific conductivity to reduce.
Claims (11)
1. electronic component-use copper alloy; This copper alloy contains 2.0-4.0 quality %Ti; Rest part contains copper and unavoidable impurities; Wherein, from the calendering face the half breadth β at the X-ray diffraction intensity peak of 220} crystal face 220} with from { the half breadth β at the X-ray diffraction intensity peak of 220} crystal face of fine copper standard powder
0220} satisfies following formula:
3.0≤β{220}/β
0{220}≤6.0，
And in the structure observation in the cross section parallel with rolling direction, the average crystalline particle diameter is represented with equivalent circle diameter, is below the 30 μ m.
2. the copper alloy of claim 1, wherein, in the structure observation in the cross section parallel with rolling direction, the average crystalline particle diameter (L) of the direction parallel with rolling direction is 1-4 with respect to the ratio (L/T) with the average crystalline particle diameter (T) of the rectangular direction of rolling direction.
3. claim 1 or 2 copper alloy, wherein, the spring limit is 600-1000 MP a.
4. claim 1 or 2 copper alloy, wherein, the spring limit is 300-600 MPa.
5. each copper alloy among the claim 1-4, wherein, with add up to 0-0.5 quality % to contain to be selected from as among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P of triad more than a kind or 2 kinds.
6. forging brass work, it contains among the claim 1-5 each copper alloy.
7. electronic unit, it possesses among the claim 1-5 each copper alloy.
8. junctor, it possesses among the claim 1-5 each copper alloy.
9. the method for manufacture of electronic component-use copper alloy; Wherein, To the solution treatment more than the temperature of Cu alloy material when 730-880 ℃ of solid solution limit that is heated to Ti is identical with addition; Said Cu alloy material contain 2.0-4.0 quality %Ti, with add up to 0-0.5 quality % to contain to be selected from arbitrarily as among Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and the P of triad more than a kind or 2 kinds, and rest part contains copper and unavoidable impurities; After solution treatment, under material temperature 400-500 ℃, heat 0.1-20 hour ageing treatment; After ageing treatment, carrying out rate of compression is the finally cold rolling of 0-40%.
10. the method for manufacture of the electronic component-use copper alloy of claim 9, it is included in and finally carries out stress relieving after cold rolling, and this stress relieving is with material temperature more than 100 ℃ but be lower than 350 ℃ of heating more than 0.001 hour below 40 hours; With material temperature more than 350 ℃ but be lower than 550 ℃ of heating more than 0.0001 hour below 20 hours; Or with material temperature heating below 700 ℃ more than 0.0001 hour below 0.003 hour more than 550 ℃.
11. the method for manufacture of the electronic component-use copper alloy of claim 9, it is included in and final carries out stress relieving after cold rolling, and this stress relieving is with material temperature more than 200 ℃ but be lower than 400 ℃ of heating 0.001-20 hour.
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| JP2010145045A JP4889801B2 (en) | 2009-11-25 | 2010-06-25 | Manufacturing method of titanium copper for electronic parts |
| PCT/JP2010/069369 WO2011065188A1 (en) | 2009-11-25 | 2010-10-29 | Titanium-copper for electronic component |
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| TWI460294B (en) | 2014-11-11 |
| KR101419152B1 (en) | 2014-07-11 |
| WO2011065188A1 (en) | 2011-06-03 |
| CN102639731B (en) | 2015-01-14 |
| KR20120076387A (en) | 2012-07-09 |
| TW201122121A (en) | 2011-07-01 |
| JP4889801B2 (en) | 2012-03-07 |
| JP2011132594A (en) | 2011-07-07 |
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