CN101981212A - Cu-Ni-Si alloy to be used in electrically conductive spring material - Google Patents
Cu-Ni-Si alloy to be used in electrically conductive spring material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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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
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Abstract
A Cu-Ni-Si base alloy containing Ni in an amount of 1.0 to 4.0 mass% and Si in a concentration of 1/6 to 1/4 of that of Ni, wherein the density of twin boundaries (Sigma3 boundaries) is 15 to 60% of all the grain boundaries. The alloy may further contain Mg: 0.2% or less, Sn: 0.2 to 1%, Zn: 0.2 to 1%, Co: 1 to 1.5%, and/or Cr: 0.05 to 0.2%.
Description
Technical field
The present invention relates to a kind of Cu-Ni-Si that is used for electronic component-use conductive elastic material is alloy, particularly relate to the electronic unit that is used for junctor, terminal, rly., switch etc., the Cu-Ni-Si of the balance excellence of intensity, bendability and electric conductivity is an alloy.
Background technology
In recent years, compactization along with electronic machine, terminal, junctor etc. also carry out miniaturization, thin-walled property, desired strength and bendability, replace solution strengthening type copper alloys such as existing phosphor bronze, brass, the needs of the such precipitation strength type copper alloy of Corson (Cu-Ni-Si system) alloy, beryllium copper and titanium copper are increased.Wherein, the balance excellence of the intensity of Corson alloy and electric conductivity is used for the increase frequency of the electronic unit of junctor etc.
Common intensity and bendability are opposite character, for the Corson alloy, keeping the high-intensity bendability that improves simultaneously also is just to have studied since in the past, extensively carry out following measure: adjust manufacturing process, the number of independent or mutual crystallization control particle diameter, precipitate and shape, texture are improved bendability thus.
In patent documentation 1, for the further Corson alloy that has added Co, Zn, Mn, Cr, Al, the grain growing when suppressing solid solution has improved bendability.In patent documentation 2, make the Corson alloy contain an amount of Ti, Zr, Hf or Th, preferably with the size of microcrystal granular, improve Punching Technology and bendability thus.In patent documentation 3, the S in the Corson alloy, O content are restricted to less than 0.005%, make Sn and Mg, the content optimization of Zn randomly, further the crystallization control particle diameter improves bendability thus.
In patent documentation 4 and 5, limit the S content in the Corson alloy, make the content optimization of Mg, Sn, Zn, the long-width ratio of crystallization control particle diameter and crystal grain is improved bendability and stress retentivity thus.In patent documentation 6, the texture of control Corson alloy, control 123}＜412〉utmost point density in orientation is in specialized range, improves bendability thus.
In patent documentation 7, the texture of control Corson alloy, control texture is to satisfy (I
(111)+ I
(311))/I
(220)＞2.0, improve bendability.In patent documentation 8, adjust hot rolling and solution treatment condition in the Corson alloy, so that in tensile strength test, do not show the yield-point effect, improve bendability.
Patent documentation 1: Japanese kokai publication hei 5-179377 communique
Patent documentation 2: Japanese kokai publication hei 6-184681 communique
Patent documentation 3: Japanese kokai publication hei 11-222641 communique
Patent documentation 4: TOHKEMY 2002-38228 communique
Patent documentation 5: TOHKEMY 2002-180161 communique
Patent documentation 6: TOHKEMY 2007-92135 communique
Patent documentation 7: TOHKEMY 2006-16629 communique
Patent documentation 8: TOHKEMY 2007-169781 communique
Summary of the invention
In recent years, along with the granular of electronic unit, except having or not be full of cracks, the size of the fold that produces at bend also becomes problem in the bendability evaluation.This be because, with bend during as electric contact, if fold is big, then contact resistance becomes unstable, the reliability that infringement is electrically connected.
But the bendability of Ping Jiaing is anti-crooked be full of cracks (slight crack) property in the prior art, does not nearly all consider flexural fold, and the Cu-Ni-Si that does not obtain anti-flexural fold excellence is an alloy.In patent documentation 3, though in the bendability evaluation, put down in writing fold, do not carry out quantitative evaluation for the size of flexural fold, do not obtain the example of corrugationless.In patent documentation 6, carried out the evaluation of flexural fold, but for the Cu-Ni-Si that obtains intensity and excellent in bending workability is an alloy, be conceived on the anodal figure of 111} 123}＜412〉orientation (patent documentation 6[0016] section), the condition of the cold rolling and solution treatment before the adjustment solution treatment (patent documentation 6[0019]).In patent documentation 8, also carried out the evaluation of flexural fold, but for the Cu-Ni-Si that obtains intensity and excellent in bending workability is an alloy, be conceived to residual Ni-Si grain (patent documentation 8[0009]), adjust Ni, Si amount, hot rolling, solution treatment condition (patent documentation 8[0019]).
The inventor is for achieving the above object, unlike the prior art, from the angle that the crystal boundary of polycrystalline metal is controlled bendability has been carried out research repeatedly, found that, by being controlled at the generation frequency of the annealing twin that produces when Cu-Ni-Si is the processing thermal treatment of alloy, the Cu-Ni-Si that obtains the intensity height and also have an excellent in vending workability in the flexural fold evaluation is an alloy.
Cu-Ni-Si of the present invention is that the copper alloy that high-intensity while bendability is good, flexural fold reduces is being kept in the alloy conduct, is applicable to the purposes of terminal, junctor etc.
Embodiment
Below, key element of the present invention and effect thereof are described.
[Ni、Si]
Ni and Si form with Ni by carrying out suitable thermal treatment
2Si is the minuteness particle of master's intermetallic compound.As a result, the intensity of alloy increases significantly, and electroconductibility also rises simultaneously.
Scope with 1.0～4.0 quality %, preferred 1.5～3 quality % is added Ni.If Ni less than 1.0 quality % then can't obtain full intensity.If Ni surpasses 4.0 quality %, then in hot rolling, produce be full of cracks.
The interpolation concentration (quality %) of Si be Ni interpolation concentration (quality %) 1/6～1/4.Lack if Si adds 1/6 of concentration ratio Ni interpolation concentration, then intensity reduces, if add more than 1/4 of concentration than Ni, then not only intensity is not had help, and excessive Si causes electroconductibility to reduce.
[Mg、Sn、Zn、Co、Cr]
Mg has the effect of improving stress relaxation properties and hot workability, if but surpass 0.2 quality %, then the heat-resisting separability of castibility (surface quality of continuous castings reduction), hot workability and plating reduces.Therefore, the concentration of Mg is defined as below 0.2%.
Sn and Zn have the intensity of improvement and stable on heating effect, and Sn has the improvement effect of anti-stress relaxation properties, and Zn has and improves the stable on heating effect that solder engages.Sn adds with 0.2～1 quality % scope, and Zn adds with 0.2～1 quality % scope.If be lower than above-mentioned scope, then can not obtain desired effects, if be higher than above-mentioned scope, then electroconductibility reduces.
Co and Cr have with Si generation compound, by separating out the effect that improves intensity.And Co has the effect that prevents thickization of crystal grain when thermal treatment, and Cr has stable on heating improvement effect.
Co adds with 1～1.5 quality % scope, and Cr adds with 0.05～0.2 quality % scope.If be lower than above-mentioned scope, then can not obtain desired effects, if be higher than above-mentioned scope, then electroconductibility reduces.
[twin boundary]
Metallic substance is generally the aggregate of the crystal grain with various crystalline orientations, i.e. polycrystal, and to cause existing the border be crystal boundary to the arrangement mode difference of atom in metallic substance.Crystal boundary is divided into big angle crystal boundary, low angle boundary, subgrain boundary according to adjacent intercrystalline misorientation, and general crystal boundary is meant that adjacent intercrystalline misorientation is the big angle crystal boundary more than 15 °.On the other hand, crystal boundary is divided into random grain boundary and heavy position crystal boundary according to adjacent intercrystalline conformability.Cu-Ni-Si is that the annealing twin that alloy produces by processing thermal treatment is the heavy position crystal boundary of ∑ 3, intercrystalline conformability height.
The ∑ value is the index of conformability of expression crystal boundary, when clip crystal boundary about lattice when overlapping, the heavy site battle array of coincidence and the density of dot matrix have the corresponding relation of ∑=n when being 1/n.Therefore twin boundary is difficult for nonaffine deformation takes place at boundary vicinity because the conformability of atom is good, and when flexural deformation, being difficult for producing with the boundary vicinity is be full of cracks, the fold of basic point.Thus, comprise the ratio of the twin boundary in whole borders (wherein, removing low angle boundary and subgrain boundary) of crystal boundary and twin boundary by control, can improve bendability.
At Cu-Ni-Si of the present invention is in the alloy, is 15%～60% by the frequency (ratio) of controlling the twin boundary (∑ 3 borders) in whole borders, is preferably 30%～60%, improves bendability.Under the situation of less than 15%, the bendability that can not obtain expecting, if surpass 60%, then crystal grain is thick during solid solution, intensity reduces.
As the method for the ratio of obtaining twin boundary, EBSP (the Electron Back Scattering Pattern) method of utilizing FESEM (Field Emission Scanning Electron Microscope) is for example arranged.The backscattering electron diffraction pattern that this method produces when making electron beam shine sample surfaces obliquely for basis (chrysanthemum ground pattern), the method for analyzing crystal orientation.After present method analyzing crystal orientation, can obtain the misorientation between adjacent crystalline orientation, determine the ratio (crystal boundary characteristic distribution) of random grain boundary and each heavy position crystal boundary.Because twin boundary is equivalent to ∑ 3 a heavy crystal boundary, so the ratio of twin boundary is with (summation of the length of heavy position crystal boundary ∑ 3)/calculate (the length summation of crystal boundary) * 100.Should illustrate that crystal boundary is meant that adjacent intercrystalline misorientation is the border more than 15 °, does not comprise low angle boundary and subgrain boundary.
Twin of the present invention is an annealing twin, is the twin of following the recrystallize that takes place by the annealing after rolling to generate.The generation frequency of twin is relevant with the stacking fault energy of material, if stacking fault energy is low, then the twin frequency that produces when annealing rises, if high, then frequency reduces.On the other hand, stacking fault energy reduces by increasing solid solution Ni and Si amount (being actually increases solid solution Si amount).Therefore, increase,, solid solution Ni and Si amount is increased get final product by preceding for stacking fault energy is reduced in final recrystallization annealing (in the present invention corresponding to solution treatment) in order to make the twin boundary frequency.
But, in the manufacture method of existing C orson alloy, Ni and Si be solid-solubilized in solution treatment the time be ordinary method owing to carry out hot rolling increased cost under unnecessary high temperature, that chaps during this external hot rolling may increase, and does not therefore carry out.In addition, the manufacture method of also useful hot rolling double as solution treatment, but after the annealing that is equivalent to solution treatment, even carry out hot rolling, the Ni-Si partial crystallization thing that produces when casting can not reach complete solid solution, and stacking fault energy is fully reduced.As a result, the frequency of the twin boundary that obtains with existing method is about 12%.On the other hand, in the present invention, speed of cooling when casting by improving, the number and the particle diameter of Ni-Si partial crystallization thing are reduced, and, in hot-rolled process, do not produce in the limit of be full of cracks, adopt the long annealing conditions of high temperature, with material cooled, make solid solution Ni and Si amount than existing method height thus, the twin boundary frequency that obtains expecting.
[manufacture method]
Corson alloy of the present invention has after " dissolve, cast → hot rolling → surfacing ", with solution treatment and general manufacture method cold rolling and the ageing treatment combination are made, the situation of carrying out stress relieving after cold rolling final is also arranged, perhaps use the situation of hot rolling double as solution treatment.Recrystallize when following solution treatment owing to annealing twin produces, therefore reach 15%～60% for the frequency that makes twin boundary, carry out in following ranges by the condition that above-mentioned casting begins till the hot rolling, in final recrystallization annealing, promptly in advance Ni and the abundant solid solution of Si are got final product before the solution treatment.
Ingot casting speed of cooling when making casting is 300～500 ℃/minute, suppresses the partial crystallization of thick Ni-Si particle when the casting cooling.The speed of ingot casting speed of cooling above 500 ℃/minute is considered impracticable from the expense angle.Then, be 940～1000 ℃ in Heating temperature, be preferably 950～980 ℃ down with annealing 3～6 hours heat-up time, make the Ni-Si particle solid solution that residues in ingot casting after, carry out hot rolling.If 940 ℃ of Heating temperature less thaies or less than 3 hours, the solid solution of then residual Ni-Si particle is insufficient.On the other hand, the annealed hot rolling be full of cracks that surpasses when hot rolling under 1000 ℃ the high temperature may increase.The annealing that surpasses 6 hours with respect to desired effects, forms over-drastic annealing in the said temperature zone, consider not preferred by the expense angle.Material temperature when hot rolling is finished is more than 650 ℃.If 650 ℃ of less than, the Ni that then in hot rolling, separates out
2Si measures increase, can not guarantee sufficient solid solution Ni and Si amount, so the twin boundary frequency reduces.
After the surfacing, implement degree of finish and be cold rolling 85% or more, after carrying out 5 seconds～30 minutes solution treatment (be final recrystallization annealing this moment) under 700～820 ℃, under 350～550 ℃, carry out 2～30 hours ageing treatment.Further, carry out cold rolling with degree of finish 5%～50%.
Embodiment 1
(manufacturing of sample)
With the electrolytic copper fusing, in the air melting stove, drop into the interpolation element of specified amount, stir molten soup.Afterwards, inject casting mold down for 1250 ℃, obtain ingot casting at pouring temperature.By changing the water-cooled condition of casting mold, the ingot casting speed of cooling during with casting is adjusted into the condition in the table.Ingot casting speed of cooling during casting is meant, after molten soup solidified, the ingot casting temperature was by 1100 ℃ to 500 ℃ average cooling rate (℃/minute).Then, this ingot casting is processed and thermal treatment, obtained the sample that thickness of slab is 0.25mm according to following steps.
(1) under the condition in table to ingot casting anneal, hot rolling, after handling thickness of slab and being specific thickness, carry out water-cooled.
(2) remove the oxide skin on top layer with surfacing.
(3) implementing cold-rolling treatment to thickness of slab is 0.3mm.
(4) 1 minute solution treatment of enforcement under the solid solubility temperature in table.
(5) under 450 ℃ * 10 hours condition, implement ageing treatment.
(6) the timeliness material is cold-rolled to 0.25mm.
For above-mentioned materials,, implement EBSP mensuration, tension test and the W pliability test relevant with twin boundary according to following benchmark.
[twin boundary]
As the method for the ratio of obtaining twin boundary, use EBSP (the Electron Back Scattering Pattern) method of utilizing FESEM (Field Emission Scanning Electron Microscope).After present method analyzing crystal orientation, obtain the misorientation between adjacent crystalline orientation, determine the crystal boundary characteristic distribution.Observing multiplying power is 1000 times, and field of view adds up to 2mm
2Heavy position crystal boundary uses the ∑ value representation, and twin boundary is equivalent to ∑ 3 a heavy crystal boundary.The ratio of twin boundary (%) is with (summations of heavy position crystal boundary ∑ 3 length)/calculate (the length summation of crystal boundary) * 100.Should illustrate that the crystal boundary in the formula is meant that adjacent intercrystalline misorientation is the border more than 15 °, does not comprise little crystal boundary and subgrain boundary.
[tensile strength]
For each copper alloy plate, on the direction parallel, carry out tension test with rolling direction, obtain according to JIS Z2241.High strength is meant among the following embodiment, and for alloy A, tensile strength is more than the 700MPa, for alloy B, more than 650MPa, for alloy C, more than 600MPa.
[crooked be full of cracks]
Make bending axis parallel, take the elongated square test film of wide 10mm * long 30mm with rolling direction.This test film is carried out W pliability test (JIS H3130), is MBR (Minimum Bend Radius) with the minimum bending radius that does not produce be full of cracks, estimates by the ratio MBR/t with thickness of slab t (mm).For alloy A, the MBR/t of Bad way (B.W.) direction is 1 when following, and the be full of cracks of bendability is evaluated as (zero), in addition is judged as bad (*).
For alloy B and C, MBR/t is 0.5 when following, judges that bendability is good.
[flexural fold]
In above-mentioned W pliability test, the fold that arrives at the curved protrusion surface observation with the test film of MBR bending machining is taken the SEM photo.On photo, carry out the width measurements of flexural fold, obtain the width of the maximum deflection fold in test film.Each is measured 3 test films for the examination material, with the width of mean value as flexural fold.At the width of the flexural fold of B.W. direction is 30 μ m when following, and the fold of bendability is evaluated as (zero), if surpass 30 μ m, then is judged as bad (*).Should illustrate that "-" expression can not be estimated in the table.
The embodiment of Ni-Si class copper alloy A of the present invention (Cu-2%Ni-0.5%Si-0.1%Mg) is as shown in table 1.
The embodiment of Ni-Si class copper alloy B of the present invention (Cu-1.6%Ni-0.4%Si-0.4%Sn-0.5%Zn) is as shown in table 2.
The embodiment of Ni-Si class copper alloy C of the present invention (Cu-1.6%Ni-0.4%Si) is as shown in table 3.
In comparative example 1,8 and 15, because therefore 300 ℃/minute of the speed of cooling less thaies during casting produce thick Ni-Si crystal grain precipitate in ingot casting, Ni and Si reduce the solid solution capacity of parent phase, stacking fault energy does not fully reduce, so twin boundary frequency less than 15%.
In comparative example 2～4,9～11 and 16～18, because not satisfy hot-rolled condition be more than 940 ℃ and be more than 3 hours and to finish temperature be in more than 650 ℃ any, therefore Ni-Si crystal grain inclusion does not have abundant solid solution, stacking fault energy does not reduce, so twin boundary frequency less than 15%.
In comparative example 5,12 and 19, because cold rolling degree of finish is below 85%, so the recrystallize during solid solution is insufficient, twin boundary frequency less than 15%.
In comparative example 6,13 and 20, because solid solubility temperature is below 700 ℃, so recrystallize is insufficient, twin boundary frequency less than 15%, and intensity also reduces.
In comparative example 7,14 and 21, because solid solubility temperature surpasses 820 ℃, so the twin boundary frequency surpasses 60%, and it is big that the crystallization particle diameter becomes, so the flexural fold width becomes big.
Embodiment 2
(manufacturing of sample)
With the electrolytic copper fusing, in the air melting stove, drop into the interpolation element of specified amount, to form the composition of the expectation shown in the table 4, stir molten soup.Afterwards, inject casting mold down for 1250 ℃ at pouring temperature, adjusting speed of cooling is 400 ℃/minute, obtains ingot casting.Then, this ingot casting is processed and thermal treatment, obtained the sample that thickness of slab is 0.25mm according to following steps.
(1) after under 950 ℃ ingot casting being carried out annealing in 4 hours, implement hot rolling, making the temperature of finishing after rolling is 700 ℃.
(2) oxide skin on top layer is carried out surfacing, handle thickness of slab to 5mm.
(3) implementing cold-rolling treatment to thickness of slab is 0.3mm.
(4) 750 ℃ of solution treatment of implementing 1 minute down.
(5) under 450 ℃ * 10 hours condition, implement ageing treatment.
(6) the timeliness material is cold-rolled to 0.25mm.
For above-mentioned materials, implement the EBSP relevant and measure, stretch and try electric conductivity and W pliability test with twin boundary.The evaluation of twin boundary frequency and W pliability test and the foregoing description 1 similarly carry out, because the influence that tensile strength is formed is big, therefore judge to be high strength more than the 600MPa.
[table 4]
The result is as shown in table 5.Twin boundary frequency as shown in table 5, that example 13～24 obtains expecting, bendability is good, and intensity might as well.The Ni amount of comparative example 22 is lower than specified amount, and bendability is good, but tensile strength reduces.The Ni amount of comparative example 23 produces the hot rolling be full of cracks than specified amount height, can not make sample.
Claims (4)
1.Cu-Ni-Si be alloy, it contains the Ni of 1.0～4.0 quality %, the quality % concentration that contains with respect to Ni is the Si of 1/6～1/4 concentration, remainder comprises Cu and unavoidable impurities, measure the texture observations of carrying out by EBSP and find that the frequency control with the twin boundary in whole crystal boundaries (∑ 3 borders) is 15%～60%.
2. Cu-Ni-Si according to claim 1 is an alloy, and it also contains the following Mg of 0.2 quality %.
3. Cu-Ni-Si according to claim 1 and 2 is an alloy, and it also contains the Sn of 0.2～1 quality %, the Zn of 0.2～1 quality %.
4. be alloy according to each described Cu-Ni-Si in the claim 1～3, it also contains the Co of 1～1.5 quality %, the Cr of 0.05～0.2 quality %.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008093847 | 2008-03-31 | ||
| JP2008-093847 | 2008-03-31 | ||
| PCT/JP2009/056540 WO2009123140A1 (en) | 2008-03-31 | 2009-03-30 | Cu-ni-si alloy to be used in electrically conductive spring material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101981212A true CN101981212A (en) | 2011-02-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009801115071A Pending CN101981212A (en) | 2008-03-31 | 2009-03-30 | Cu-Ni-Si alloy to be used in electrically conductive spring material |
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| Country | Link |
|---|---|
| JP (1) | JP4596493B2 (en) |
| KR (1) | KR101249107B1 (en) |
| CN (1) | CN101981212A (en) |
| TW (1) | TWI443204B (en) |
| WO (1) | WO2009123140A1 (en) |
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2009
- 2009-03-30 CN CN2009801115071A patent/CN101981212A/en active Pending
- 2009-03-30 JP JP2009082784A patent/JP4596493B2/en active Active
- 2009-03-30 WO PCT/JP2009/056540 patent/WO2009123140A1/en active Application Filing
- 2009-03-30 KR KR1020107016770A patent/KR101249107B1/en active IP Right Grant
- 2009-03-31 TW TW98110571A patent/TWI443204B/en active
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| CN103403202A (en) * | 2011-03-09 | 2013-11-20 | Jx日矿日石金属株式会社 | Cu-Ni-Si based alloy and process for manufacturing same |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2009123140A1 (en) | 2009-10-08 |
| JP4596493B2 (en) | 2010-12-08 |
| KR101249107B1 (en) | 2013-03-29 |
| TWI443204B (en) | 2014-07-01 |
| KR20100095476A (en) | 2010-08-30 |
| TW200948990A (en) | 2009-12-01 |
| JP2009263784A (en) | 2009-11-12 |
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