CN102453815B - Copper alloy, forged copper adopting the copper alloy, electronic component, connector and method for manufacturing copper alloy - Google Patents
Copper alloy, forged copper adopting the copper alloy, electronic component, connector and method for manufacturing copper alloy Download PDFInfo
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- CN102453815B CN102453815B CN201110342285.3A CN201110342285A CN102453815B CN 102453815 B CN102453815 B CN 102453815B CN 201110342285 A CN201110342285 A CN 201110342285A CN 102453815 B CN102453815 B CN 102453815B
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 46
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 239000010949 copper Substances 0.000 title claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 65
- 239000010936 titanium Substances 0.000 claims abstract description 59
- 238000005096 rolling process Methods 0.000 claims abstract description 33
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 31
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 229910052796 boron Inorganic materials 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 10
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 10
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 47
- 230000032683 aging Effects 0.000 claims description 29
- 238000005097 cold rolling Methods 0.000 claims description 28
- 239000006104 solid solution Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 abstract description 24
- 239000000843 powder Substances 0.000 abstract description 3
- 238000003483 aging Methods 0.000 description 26
- 239000000463 material Substances 0.000 description 22
- 239000013078 crystal Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 13
- 239000002245 particle Substances 0.000 description 12
- 238000000137 annealing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000005098 hot rolling Methods 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 238000003754 machining Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 238000001953 recrystallisation Methods 0.000 description 5
- 238000001330 spinodal decomposition reaction Methods 0.000 description 5
- 230000012010 growth Effects 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 229910010165 TiCu Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000005480 shot peening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000008467 tissue growth Effects 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
- B21B2003/005—Copper or its alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Conductive Materials (AREA)
- Non-Insulated Conductors (AREA)
Abstract
The invention provides titanium copper, forged copper, an electronic component, a connector and manufacturing method therefore. The copper alloy contains 2.0-4.0 % of Ti by mass, 0-0.5% of one or more than two third elements selected from Mn, Fe, Mg, Co, Ni, Cr, V, Mo, Nb, Zr, Si, B and P by mass in total, and copper alloy containing copper and unavoidable impurities. The ratio (I/ I0) of the X-ray diffraction intensity I of a rolling surface and the X-ray diffraction intensity IO of the pure copper powders in a rolling surface (311) and a rolling surface (200) satisfy the relationship of 15<= {I/I0(220)}/ {I/I0(200)} <= 95.
Description
Technical field
The present invention relates to the copper alloy containing titanium that is suitable for the electronic component materials such as such as connector and use its forged copper (Shen Copper product), the manufacture method of electronic component and connector and copper alloy.
Background technology
In recent years, growing along with the miniaturization being the electronic instrument of representative with portable terminal etc., the spacing of the connector wherein used narrow and the trend of low dwarfing remarkable.Small-sized connector, then pin width is narrower, forms the less machining shape of bending, therefore requires the raw material used to have to obtain the necessary high strength needed for elasticity and can the bendability of excellence of resistance to harsh bending machining.Thus, the copper alloy (hereinafter referred to as " titanium copper ") containing titanium, because strength ratio is higher, stress relaxation properties is the most excellent in copper alloy, is used as the signal system terminal raw material of requirement raw material intensity all the time.
Titanium copper is the copper alloy of age-hardening type.Specifically, by solutionizing process, form the supersaturated solid solution of solute atoms Ti, if implement more long heat treatment at low temperatures by this state, then by Spinodal decomposition, in parent phase, the modulated structure of Ti concentration cycle variation generates, and intensity improves.Based on above-mentioned enhancing mechanism, in order to improve the characteristic of titanium copper further, various method is studied.
Now, problem is, intensity and bendability are contrary characteristic.That is, if improve intensity, damage bendability, on the contrary, if pay attention to bendability, can not get required intensity.
Therefore, in the past from the 3rd elements (patent document 1) such as interpolation Fe, Co, Ni, Si, specify the concentration of the impurity element group be solid-solubilized in parent phase, make them separate out the systematicness (patent document 2) improving modulated structure with the distributional pattern specified as second phase particles (Cu-Ti-X system particle), regulation is to the density (patent document 3) making the effective trace additives of crystal grain miniaturization and second phase particles, make crystal grain miniaturization (patent document 4) angularly, in order to the intensity and bendability realizing titanium copper is studied exploitation simultaneously.
In addition, also proposed in patent document 5, be conceived to crystal orientation, in order to prevent the crackle in bending machining, regulating hot-rolled condition to meet I{420}/I
0420} > 1.0, and then regulate cold rolling rate to meet I{220}/I
0{ crystallization control orientation is carried out in 220}≤3.0, improves the anterethic technology of intensity, bendability and proof stress thus.
[prior art document]
[patent document]
[patent document 1] Japanese Unexamined Patent Publication 2004-231985 publication
[patent document 2] Japanese Unexamined Patent Publication 2004-176163 publication
[patent document 3] Japanese Unexamined Patent Publication 2005-97638 publication
[patent document 4] Japanese Unexamined Patent Publication 2006-283142 publication
[patent document 5] Japanese Unexamined Patent Publication 2008-308734 publication
Summary of the invention
Above-mentioned titanium copper casts the → order manufacture of homogenizing annealing → hot rolling → (annealing and cold rolling repeating) → final solutionizing process → cold rolling → Ageing Treatment basically by the melting of ingot, seeks the improvement of characteristic based on this step.But also have further room for improvement obtaining having in the titanium copper of more excellent characteristic.
Therefore, the present invention attempts from from the past different angles the characteristic improving titanium copper, provides thus and has the intensity of excellence and the copper alloy of bendability and use its forged copper, electronic component and connector and the manufacture method of copper alloy.
The present inventor is finding to solve in research process that above-mentioned problem carries out, after solutionizing process, if do not generate or generate the metastable phase of a part of titanium or the appropriate heat treatment (sub-Ageing Treatment) of stable phase degree, there is Spinodal decomposition to a certain degree in advance, then carry out cold rolling and Ageing Treatment subsequently and the intensity of the titanium copper finally obtained significantly improves.That is, carry out in a stage of Ageing Treatment the heat treatment step that Spinodal decomposition occurs relative to titanium copper in the past, in titanium copper manufacture method of the present invention, occur in Spinodal decomposition significantly different across cold rolling 2 stages.
Known further, by further the addition of the 3rd element being adjusted to optimal scope, can in the past by titanium copper that the second solutionizing process for the purpose of solid solution and 2 stages of the second solutionizing process for the purpose of recrystallization process, carry out solid solution and recrystallization by a solutionizing process simultaneously, obtain production efficiency excellence and the titanium copper of the balancing good of intensity and bendability.
The scheme of the present invention completed based on above-mentioned discovery is copper alloy, it contains the Ti of 2.0 ~ 4.0 quality %, amount to containing 0 ~ 0.2 quality % as the 3rd element to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, remainder comprises copper and inevitable impurity, wherein, when measuring the X-ray diffraction intensity of rolling surface, the X-ray diffraction intensity I of rolling surface and the X-ray diffraction intensity I of the fine copper powder in (311) face and (200) face
0ratio (I/I
0) meet following relational expression (1): { I/I
0(311) }/{ I/I
0(200) }≤2.54 ... (1) the X-ray diffraction intensity I of the fine copper powder, and in the X-ray diffraction intensity I of rolling surface and (220) face and (200) face
0ratio (I/I
0) meet following relational expression (2): 15≤{ I/I
0(220) }/{ I/I
0(200) }≤95 ... (2).
Another program of the present invention is copper alloy, it contains the Ti of 2.0 ~ 4.0 quality %, amount to containing 0.01 ~ 0.15 quality % as the 3rd element to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, remainder comprises copper and inevitable impurity, wherein, when measuring the X-ray diffraction intensity of rolling surface, the X-ray diffraction intensity I of rolling surface and the X-ray diffraction intensity I of the fine copper powder in (311) face and (200) face
0ratio (I/I
0) meet following relational expression (1): { I/I
0(311) }/{ I/I
0(200) }≤2.54 ... (1) the X-ray diffraction intensity I of the fine copper powder, and in the X-ray diffraction intensity I of rolling surface and (220) face and (200) face
0ratio (I/I
0) meet following relational expression (3): 30≤{ I/I
0(220) }/{ I/I
0(200) }≤95 ... (3).
Further another program of the present invention is forged copper, and it comprises above-mentioned copper alloy.
Further another program of the present invention is electronic component, and it comprises above-mentioned copper alloy.
Further another program of the present invention is connector, and it has above-mentioned copper alloy.
Further another program of the present invention is the manufacture method of above-mentioned copper alloy, it comprises: to the Ti containing 2.0 ~ 4.0 quality %, amount to and be selected from Mn containing 0 ~ 0.2 quality % as the 3rd element, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, one kind or two or more in B and P, remainder comprises the copper alloy raw material of copper and inevitable impurity, carry out being heated to the solid solution limit temperature of temperature high 0 ~ 20 DEG C more identical with addition than the solid solution limit of Ti and the solutionizing process of quenching at 730 ~ 880 DEG C, heat-treat after solutionizing process, carry out finally cold rolling with the working modulus of 5 ~ 40% after the heat treatment, Ageing Treatment is carried out after finally cold rolling.
The manufacture method of copper alloy of the present invention, in one embodiment, above-mentioned heat treatment makes electrical conductivity raise, when titanium concentration (quality %) is [Ti], the rising value C (%IACS) of electrical conductivity is made to meet following relational expression (4): 0.5≤C≤(-0.50 [Ti]
2-0.50 [Ti]+14) ... (4).
Detailed description of the invention
<Ti content >
When Ti is less than 2 quality %, due to the enhancing mechanism realized by the formation of the original modulated structure of titanium copper fully can not be obtained, therefore can not get sufficient intensity, if on the contrary more than 4.0 quality %, easily separate out thick TiCu
3, have the trend that intensity and bendability are deteriorated.Therefore, the Ti content in copper alloy of the present invention is 2.0 ~ 4.0 quality %, is preferably 2.7 ~ 3.5 quality %, more preferably 2.9 ~ 3.3 quality %.By making the content of Ti suitable, the intensity and the bendability that are suitable for electronic component can be realized simultaneously.
< the 3rd element >
Ternary have the miniaturization helping crystal grain, therefore can add the 3rd element of regulation.Specifically, at the high temperature of the abundant solid solution of Ti, carry out solutionizing process, also easily make crystal grain miniaturization, intensity easily improves.In addition, the 3rd element promotes the formation of modulated structure.Further, also there is suppression TiCu
3the effect separated out.Therefore, the age hardening capability that titanium copper is original is obtained.
In titanium copper, that above-mentioned effect is the highest is Fe.And for Mn, Mg, Co, Ni, Si, Cr, V, Nb, Mo, Zr, B and P, also can expect the effect being equivalent to Fe, add separately also effective, but also can compound two or more add.
If these elements amount to containing more than 0.01 quality %, show its effect, if total over 0.5 quality %, the solid solution limit of Ti narrows, and easily separates out thick second phase particles, although intensity improves a little, but bendability is deteriorated.Simultaneously thick second phase particles encourages the rough surface of bend, promotes the die wear in pressurization processing.Therefore, as the 3rd element set, preferably containing one kind or two or more total 0 ~ 0.5 quality % be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P, more preferably containing 0 ~ 0.2 quality %, further preferably containing 0.01 ~ 0.15 quality %.
The interpolation of the 3rd element is effective for the miniaturization of the crystal grain of titanium copper, likely raises solid solution limit temperature on the other hand, therefore must improve solid solubility temperature compared with not adding the situation of the 3rd element.All the time, in order to make the 3rd element solid solution fully, and after carrying out first time solutionizing process in the at high temperature long time, final solutionizing process is carried out.But owing to carrying out 2 solutionizing process, apply load to manufacturing step, production efficiency likely reduces.In present embodiment, by the concentration adjustment of the 3rd element in titanium copper is 0 ~ 0.2 quality %, is preferably adjusted to 0.01 ~ 0.15 quality % further, under the state of reduction treatment temperature compared with the past, solid solution and the recrystallization of the 3rd element can be carried out by 1 solutionizing process simultaneously.Thus, in the manufacture of titanium copper, necessary heat is compared with the past a small amount of, and the processing time is also the short time, and production efficiency improves, and can realize being suitable for mass-produced step.
The integrated intensity > that < is obtained by X-ray diffraction
The set tissue of the rolling surface after solutionizing process, the component ratio in (200) face is high usually, produces rotation along with the carrying out of rolling, and the component ratio in final (220) face raises.Found that of the present inventor's research, carry out the manufacturing step of present embodiment, namely after final solutionizing process, carry out cold rolling before when heat-treating, compared with the manufacturing step of step in the past, i.e. solutionizing process → cold rolling → Ageing Treatment, due to modulated structure growth in mother metal, not easily produce the rotation from (200) towards (311) face.Thus, the copper alloy of present embodiment, preferably when measuring X-ray diffraction intensity (integrated intensity) of rolling surface, the X-ray diffraction intensity I of rolling surface and the X-ray diffraction intensity I of the fine copper powder in (311) face and (200) face
0ratio (I/I
0) meet following relational expression (1):
{I/I
0(311)}/{I/I
0(200)}≤2.54…(1)。
In the present invention, fine copper standard powder is defined as the copper powders of the purity 99.5% of 325 orders (JIS Z8801).
More preferably { I/I
0(311) }/{ I/I
0(200) be } 0.50 ~ 2.00, preferred { I/I further
0(311) }/{ I/I
0(200) be } 0.80 ~ 1.75.{ I/I
0(311) }/{ I/I
0(200), when } being greater than 2.54, intensity (0.2% endurance) dies down, and bendability is likely also deteriorated.
The working modulus impact being also subject to final milling step is organized in the set of titanium copper.That is, if the working modulus of rolling is excessive, then (220) face too grows and bendability variation, if processability is too low, then the growth in (220) face is insufficient, and intensity likely reduces.The titanium copper of present embodiment preferably carries out with the working modulus of 5 ~ 40%, is more preferably 10 ~ 30%.The X-ray diffraction intensity I of the X-ray diffraction intensity I of preferred rolling surface and the fine copper powder in (220) face and (200) face is organized in the set of rolling surface now
0ratio (I/I
0) meet following relational expression (2):
15≤{I/I
0(220)}/{I/I
0(200)}≤95…(2)。
{ I/I
0(220) }/{ I/I
0(200) when } being less than 15, working modulus is low, and the work hardening realized by milling step likely becomes insufficient.
If compare with the set tissue of the situation of only carrying out 1 solutionizing process the situation of having carried out 2 solutionizing process, known, only carry out the situation of 1 solutionizing process compared with carrying out the situation of 2 solutionizing process, recrystallization set is organized weak, and the value of (220)/(200) ratio increases.Obtaining, in intensity and the good balance of bendability, except relational expression (1), more preferably meeting following relational expression (3) substitutional relation formula (2):
30≤{I/I
0(220)}/{I/I
0(200)}≤95…(3)，
Preferred { I/I further
0(220) }/{ I/I
0(200) be } 40 ~ 70, further preferred { I/I
0(220) }/{ I/I
0(200) be } 40 ~ 55.
< purposes >
The copper alloy of present embodiment can with various forged copper, and such as plate, bar, pipe, rod, paper tinsel and line morphology provide.By processing the copper alloy of present embodiment, such as, obtain the electronic components such as switch, connector, socket, terminal, relay.
< manufacture method >
One of the copper alloy of present embodiment is characterised in that, after final solutionizing process, cold rolling before under the material temperature condition of regulation, carry out the heat treatment of short time.During heat treatment, if the temperature of material is too high, overlong time, the β ' phase not having so large effect to intensity in Ageing Treatment after this, the β phase that bendability is deteriorated easily are separated out.In addition, if the temperature of material during heat treatment is too low, the time is too short, the growth of the modulated structure produced by Spinodal decomposition in Ageing Treatment easily becomes insufficient.
If heat-treat the titanium copper after solutionizing process, then along with the growth of modulated structure, electrical conductivity raises, and therefore, the degree of annealing can be changed to index with the electrical conductivity of front and back of anneal.According to the research of the present inventor, heat treatment preferably make electrical conductivity raise 0.5 ~ 8%IACS, preferably raise 1 ~ 4%IACS condition under carry out.That is, preferably carry out being less than the heat treatment of 90% of peak hardness at this.Concrete heat-treat condition corresponding to the rising of this electrical conductivity is material temperature more than 300 DEG C and lower than 700 DEG C, the heating condition of 0.001 ~ 12 hour.
More particularly, the heat treatment of present embodiment, when titanium concentration (quality %) is [Ti], the rising value C (%IACS) of electrical conductivity can meet following relational expression (4).
0.5≤C≤(-0.50[Ti]
2-0.50[Ti]+14)…(4)
According to above-mentioned (4) formula, such as, when Ti concentration is 2.0 quality %, preferably carry out under making electrical conductivity raise the condition of 0.5 ~ 11%IACS, when Ti concentration is 3.0 quality %, preferably carry out under making electrical conductivity raise the condition of 0.5 ~ 8%IACS, when Ti concentration is 4.0 quality %, preferably carry out under making electrical conductivity raise the condition of 0.5 ~ 4%IACS.
More preferably the heat treatment of present embodiment is when titanium concentration (quality %) is [Ti], and the rising value C (%IACS) of electrical conductivity can meet following relational expression (5).
1.0≤C≤(0.25[Ti]
2-3.75[Ti]+13)…(5)
According to above-mentioned (5) formula, such as, when Ti concentration is 2.0 quality %, preferably carry out under making electrical conductivity raise the condition of 1.0 ~ 6.5%IACS, when Ti concentration is 3.0 quality %, preferably carry out under making electrical conductivity raise the condition of 1.0 ~ 4%IACS, when Ti concentration is 4.0 quality %, preferably carry out under making electrical conductivity raise the condition of 1.0 ~ 2%IACS.
And, in heat treatment after final solutionizing process, when carrying out the timeliness at hardness formation peak of copper alloy, the difference of electrical conductivity such as raises 13%IACS under Ti concentration 2.0 quality %, raise 10%IACS under Ti concentration 3.0 quality %, under Ti concentration 4.0 quality %, raise about 5%IACS.That is, the heat treatment after the final solutionizing process of present embodiment, compared with the timeliness forming peak with hardness, the heat provided copper alloy is very little.
Heat treatment is preferably carried out under any one following condition.
Material temperature be more than 300 DEG C and lower than 400 DEG C, heating 0.5 ~ 3 hour
Material temperature be more than 400 DEG C and lower than 500 DEG C, heating 0.01 ~ 0.5 hour
Material temperature be more than 500 DEG C and lower than 600 DEG C, heating 0.001 ~ 0.01 hour
Material temperature be more than 600 DEG C and lower than 700 DEG C, heating 0.001 ~ 0.005 hour
In addition, heat treatment is more preferably carried out under any one following condition.
Material temperature be more than 350 DEG C and lower than 400 DEG C, heating 1 ~ 3 hour
Material temperature be more than 400 DEG C and lower than 450 DEG C, heating 0.2 ~ 0.5 hour
Material temperature be more than 500 DEG C and lower than 550 DEG C, heating 0.005 ~ 0.01 hour
Material temperature be more than 550 DEG C and lower than 600 DEG C, heating 0.001 ~ 0.005 hour
Material temperature be more than 600 DEG C and lower than 650 DEG C, heating 0.0025 ~ 0.005 hour
Below the preferred embodiment of each step is described.
1) ingot manufacturing step
Substantially carried out in a vacuum or in inert gas atmosphere by the manufacture melted and cast the ingot carried out.If have the fusing of Addition ofelements to remain in melting, then the raising for intensity can not play a role effectively.Thus, residual in order to eliminate fusing, dystectic Addition ofelements such as Fe, Cr must stir fully after interpolation, and keeps certain hour.On the other hand, Ti, due to than being easier to be melted in Cu, can add after the melting of the 3rd element set.Therefore, in Cu, add with the total content of 0 ~ 0.2 quality % that to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, then add Ti with the content of 2.0 ~ 4.0 quality % and manufacture ingot.
2) homogenizing annealing and hot rolling
Wherein, the crystal produced in solidifying segregation, casting is preferably eliminated as far as possible.This is in order in solutionizing process afterwards, fine and precipitation that is Dispersed Second Phase particle equably, also has effect for preventing mixed grain.After ingot manufacturing step, preferably be heated to 900 ~ 970 DEG C carry out 3 ~ 24 hours homogenizing annealings after, implement hot rolling.In order to prevent liquid metals fragility, be preferably set to less than 960 DEG C before hot rolling and in hot rolling.
3) the first solutionizing process
Then, solutionizing process is carried out after suitably repeating cold rolling and annealing.Specifically, the first solutionizing process can carry out 2 ~ 10 minutes under the heating-up temperature of 850 ~ 900 DEG C.Programming rate now and cooling velocity preferably do one's utmost to accelerate, second phase particles can not be separated out.But, when the addition of the 3rd element is 0.01 ~ 0.15 quality %, just can carries out solid solution and recrystallization without the first solutionizing process by means of only final solutionizing process, therefore preferably omit the first solutionizing treatment step.
4) intermediate rolling
Degree of finish in final solutionizing intermediate rolling before treatment is higher, then the second phase particles in final solutionizing process evenly and separate out imperceptibly.If but degree of finish is too high, be recrystallized when carrying out final solutionizing process set tissue growth, and produce plastic anisotropy, likely infringement pressurization shaping.Therefore, the degree of finish of intermediate rolling is preferably 70 ~ 99%.Degree of finish is defined as the thickness before (thickness after the thickness-rolling before rolling)/rolling) × 100%}.
5) final solutionizing process
The precipitate generated in casting or intermediate rolling process is there is in final solutionizing copper alloy raw material before treatment.This precipitate increases owing to likely hindering the mechanical property after bendability and timeliness, therefore in final solutionizing process, preferably by copper alloy heating raw materials to the temperature of the complete solid solution of the precipitate made in copper alloy raw material.But if be heated to high temperature until precipitate disappears completely, then the locking effect of the crystal boundary realized by precipitate is disappeared, and crystal grain is coarsening sharply.If crystal grain is coarsening sharply, then there is the trend that intensity reduces.
Therefore, as heating-up temperature, the temperature of the solid solution limit annex that the copper alloy heating raw materials before solutionizing to second phase particles is formed.When the addition of Ti is the scope of 2.0 ~ 4.0 quality %, the temperature (being called in the present invention " solid solution limit temperature ") that the solid solution limit of Ti is equal with addition is about 730 ~ 840 DEG C, such as, is about 800 DEG C when the addition of Ti is 3.0 quality %.And if be heated to rapidly this temperature, cooling velocity also accelerates, the generation of thick second phase particles is inhibited.Therefore, typically, be heated to more than the solid solution limit of the Ti of 730 ~ 880 DEG C temperature identical with addition, more typically say, be heated to the temperature of the solid solution limit of the Ti than 730 ~ 880 DEG C temperature high 0 ~ 20 DEG C identical with addition, the preferably temperature of high 0 ~ 10 DEG C.
In order to suppress the generation of second phase particles thick in final solutionizing process, preferably as far as possible promptly carry out the heating and cooling of copper alloy raw material.Specifically, by high about 50 ~ 500 DEG C in the temperature of the solid solution limit annex formed than second phase particles, preferably configure copper alloy raw material in the atmosphere of high about 150 ~ 500 DEG C and come to heat rapidly.Be cooled through water-cooled etc. to carry out.
6) heat treatment
Heat-treat after final solutionizing process.Heat treated condition is described above.
7) final cold rolling
After above-mentioned annealing, carry out final cold rolling.By final cold working, the intensity of titanium copper can be improved.Now, when degree of finish is less than 5%, can not get sufficient effect, therefore preferably make degree of finish be more than 5%.But if degree of finish is too high, then separate out with intragranular compared with the lattice deformability caused, the flat machining deformation caused of crystal grain increases, bendability is deteriorated.And then in the Ageing Treatment implemented as required, stress relief annealing, easily produce crystal boundary separate out, therefore degree of finish is less than 40%, is preferably 5 ~ 40%, is more preferably 10 ~ 30%, more preferably 15 ~ 25%.
8) Ageing Treatment
Ageing Treatment is carried out after finally cold rolling.The condition of Ageing Treatment can be usual condition, but if compared with the pastly slightly carry out Ageing Treatment, then the balance of intensity and bendability improves further.Specifically, Ageing Treatment is carried out preferably heat the condition of 3 ~ 12 hours at material temperature 300 ~ 400 DEG C under.And, when not carrying out Ageing Treatment, aging time short (being less than 2 hours) time or aging temperature low (lower than 290 DEG C) time, intensity and electrical conductivity likely reduce.In addition, when aging time long (more than 13 hours) or aging temp height (more than 450 DEG C), electrical conductivity raises, but intensity likely reduces.
Ageing Treatment is more preferably carried out under any one following condition.
Material temperature be more than 340 DEG C and lower than 360 DEG C, heating 5 ~ 8 hours
Material temperature be more than 360 DEG C and lower than 380 DEG C, heating 4 ~ 7 hours
Material temperature be more than 380 DEG C and lower than 400 DEG C, heating 3 ~ 6 hours
Ageing Treatment is preferred further carries out under any one following condition.
Material temperature be more than 340 DEG C and lower than 360 DEG C, heating 6 ~ 7 hours
Material temperature be more than 360 DEG C and lower than 380 DEG C, heating 5 ~ 6 hours
Material temperature be more than 380 DEG C and lower than 400 DEG C, heating 4 ~ 6 hours
And, if those skilled in the art, be then appreciated that the step such as grinding, polishing, shot-peening pickling suitably can carrying out the oxide skin for removing surface in the interval of above steps.
[embodiment]
Below examples and comparative examples of the present invention are described, but these embodiments are in order to understand the present invention and advantage thereof more well and provide, and are not intended to limit invention.
When manufacturing the copper alloy of example of the present invention, add active metal Ti as the second composition, when therefore melting, use vacuum melting stove.In addition, in order to prevent being mixed into of impurity element beyond the element owing to specifying in the present invention from producing unexpected side effect, the strict higher raw material of purity of selecting uses.
After the 3rd element for interpolation table 1 as required in Cu, the Ti of the concentration of interpolation table 1, remainder have the ingot of copper and the inevitable composition of impurity, after carrying out heating the homogenizing annealing of 3 hours at 950 DEG C, at 900 ~ 950 DEG C, carry out hot rolling, obtain the hot rolled plate that thickness of slab is 10mm.After surfacing deoxygenated skin, carry out cold rolling, form the thickness of slab (1.5mm) of base bar, (addition according to the 3rd element) carries out the first time solutionizing process of base article as required.The condition of first time solutionizing process is heat 7.5 minutes at 850 DEG C.Then in the middle of the cold rolling middle adjustment of centre thickness of slab carry out cold rolling make final thickness of slab be 0.25mm after, be inserted in the annealing furnace that can carry out heating rapidly and carry out final solutionizing process, then carry out water-cooled.Heating condition is now, with material temperature be temperature that the solid solution limit of Ti is identical with addition (during Ti concentration 3.2 quality % about 800 DEG C, Ti concentration 2.0 quality % time about 730 DEG C, Ti concentration 4.0 quality % time about 840 DEG C) be benchmark, under the heating condition that table 1 is recorded, keep 1 minute respectively to form the condition of the temperature high 0 ~ 20 DEG C more identical with addition than the solid solution limit of Ti.
Then, carry out under the condition utilizing test film to record at table 1 cold rolling after, heat-treat under the condition recorded in table 1 in an ar atmosphere.After carrying out deoxygenated skin by pickling, carry out final cold rolling under the condition that table 1 is recorded, carry out Ageing Treatment under each heating condition finally recorded at table 1, form the test film of embodiment and comparative example.
[table 1]
For each test film obtained, carry out evaluating characteristics under the following conditions.Result is as shown in table 2.
< intensity >
Draw direction use pressuring machine parallel with rolling direction is made to manufacture JIS 13B test film.Carry out the tension test of this test film according to JIS-Z2241, measure 0.2% endurance (YS) of rolling direction.
< bendability >
According to JIS H3130, carry out the W bend test of Badway (bending axis and rolling direction are equidirectional), measure the ratio MBR/t value of least radius (MBR) and the thickness of slab (t) do not cracked.
< electrical conductivity >
According to JIS H 0505, measure electrical conductivity (EC:%IACS) by 4 terminal methods.
< crystal orientation >
For each test film, use the X-ray diffraction device of motor society model rint Ultima2000 of science, under following condition determination, obtain the diffracted intensity curve of rolling surface, measure X-ray diffraction intensity (integrated value) I of (111) crystal plane, (200) crystal plane, (220) crystal plane, (311) crystal plane.Under same condition determination, for pure copper powder standard sample, also X-ray diffraction intensity (integrated value) I is tried to achieve to (111) crystal plane, (200) crystal plane, (220) crystal plane, (311) crystal plane
0, calculate I/I respectively
0(111), I/I
0(200), I/I
0(220), I/I
0(311) { I/I, is tried to achieve
0(311) }/{ I/I
0} and { I/I (200)
0(220) }/{ I/I
0(200) }.
Target: Cu pipe ball
Tube voltage: 40kV
Tube current: 40mA
Sweep speed: 5 °/min
Sampling width: 0.02 °
[table 2]
< investigates >
Comparative example 1 ~ 5 represents that the Addition ofelements of the 3rd element is 0 ~ 0.17 quality %, does not carry out the first solutionizing process and only carries out 1 final solutionizing process, example when manufacturing according to the step in the past of final solutionizing process → cold rolling → Ageing Treatment.In comparative example 1 ~ 5, can not get sufficient intensity.
Comparative example 6 ~ 10 represents that the Addition ofelements of the 3rd element is 0 ~ 0.17 quality %, carry out the solutionizing process (the first solutionizing process and final solutionizing process) in 2 stages, example when manufacturing according to the step in the past of final solutionizing process → cold rolling → Ageing Treatment.In comparative example 5 ~ 10, although bendability improves, can not get sufficient intensity.
When comparative example 11 represents the order manufacture according to final solutionizing process → heat treatment → cold rolling → Ageing Treatment, the example of degree of finish when excessively reducing cold rolling.In comparative example 11, because degree of finish is too low, can not get sufficient intensity.
When comparative example 12 represents the step manufacture according to final solutionizing process → heat treatment → cold rolling → Ageing Treatment, the example of degree of finish when excessively improving cold rolling.In comparative example 12, although obtain sufficient intensity, because degree of finish is too high, bendability is deteriorated.
When comparative example 13 represents the step manufacture according to final solutionizing process → heat treatment → cold rolling → Ageing Treatment, final solutionizing process is carried out under the hardness of titanium copper is close to the condition (peak aging condition) at peak, and then the example when very short time carries out final Ageing Treatment.In comparative example 13, because the heat treatment after solutionizing is near peak, thick stablizing is separated out mutually, and bendability is deteriorated.
More known with comparative example 1 ~ 13, in embodiment 1 ~ 11, intensity and bending machining sexual balance improve well.
Claims (6)
1. copper alloy, it is the Ti containing 2.0 ~ 4.0 quality %, amount to containing 0 ~ 0.2 quality % as the 3rd element to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, remainder comprises the copper alloy of copper and inevitable impurity, wherein, when measuring the X-ray diffraction intensity of rolling surface
The X-ray diffraction intensity I of rolling surface and the X-ray diffraction intensity I of the fine copper powder in (311) face and (200) face
0ratio (I/I
0) meet following relational expression (1):
{I/I
0(311)}/{I/I
0(200)}≤2.54…(1)，
And the X-ray diffraction intensity I of fine copper powder in the X-ray diffraction intensity I of rolling surface and (220) face and (200) face
0ratio (I/I
0) meet following relational expression (2):
15≤{I/I
0(220)}/{I/I
0(200)}≤95…(2)。
2. copper alloy, it is the Ti containing 2.0 ~ 4.0 quality %, amount to containing 0.01 ~ 0.15 quality % as the 3rd element to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, remainder comprises the copper alloy of copper and inevitable impurity, wherein, when measuring the X-ray diffraction intensity of rolling surface
The X-ray diffraction intensity I of rolling surface and the X-ray diffraction intensity I of the fine copper powder in (311) face and (200) face
0ratio (I/I
0) meet following relational expression (1):
{I/I
0(311)}/{I/I
0(200)}≤2.54…(1)，
And the X-ray diffraction intensity I of fine copper powder in the X-ray diffraction intensity I of rolling surface and (220) face and (200) face
0ratio (I/I
0) meet following relational expression (3):
30≤{I/I
0(220)}/{I/I
0(200)}≤95…(3)。
3. forged copper, it comprises the copper alloy described in claim 1 or 2.
4. electronic component, it comprises the copper alloy described in claim 1 or 2.
5. connector, it has the copper alloy described in claim 1 or 2.
6. the manufacture method of the copper alloy described in claim 1 or 2, it comprises for the Ti containing 2.0 ~ 4.0 quality %, amount to containing 0 ~ 0.2 quality % as the 3rd element to be selected from Mn, Fe, Mg, Co, Ni, Cr, V, Nb, Mo, Zr, Si, B and P one kind or two or more, remainder comprises the copper alloy raw material of copper and inevitable impurity
Described copper alloy raw material is carried out at 730 ~ 880 DEG C be heated to the solid solution limit temperature of temperature high 0 ~ 20 DEG C more identical with addition than the solid solution limit of Ti and the solutionizing process of quenching,
After solutionizing process, heat-treat,
Carry out finally cold rolling with the working modulus of 5 ~ 40% after the heat treatment,
Ageing Treatment is carried out after finally cold rolling,
Wherein, described heat treatment makes electrical conductivity raise, and when titanium concentration (quality %) is [Ti], makes the rising value C (%IACS) of electrical conductivity meet following relational expression (4):
0.5≤C≤(－0.50[Ti]
2－0.50[Ti]＋14)…(4)。
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| JP5718436B1 (en) | 2013-11-18 | 2015-05-13 | Jx日鉱日石金属株式会社 | Titanium copper for electronic parts |
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| JP6080822B2 (en) * | 2014-09-19 | 2017-02-15 | Ｊｘ金属株式会社 | Titanium copper for electronic parts and manufacturing method thereof |
| KR101627696B1 (en) | 2015-12-28 | 2016-06-07 | 주식회사 풍산 | Copper alloy material for car and electrical and electronic components and process for producing same |
| JP6703878B2 (en) * | 2016-03-31 | 2020-06-03 | Ｊｘ金属株式会社 | Titanium copper foil and its manufacturing method |
| JP6907282B2 (en) * | 2019-09-25 | 2021-07-21 | Ｊｘ金属株式会社 | Titanium-copper alloy plate for vapor chamber and vapor chamber |
| CN112548495B (en) * | 2020-11-26 | 2022-03-01 | 西北有色金属研究院 | Forging method of plate blank for superconducting wire barrier layer niobium sheet |
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