CN104928521B - The Fe-P series copper alloy plates of intensity, heat resistance and excellent in bending workability - Google Patents
The Fe-P series copper alloy plates of intensity, heat resistance and excellent in bending workability Download PDFInfo
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- CN104928521B CN104928521B CN201510101381.7A CN201510101381A CN104928521B CN 104928521 B CN104928521 B CN 104928521B CN 201510101381 A CN201510101381 A CN 201510101381A CN 104928521 B CN104928521 B CN 104928521B
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 38
- 238000005452 bending Methods 0.000 title claims description 7
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 238000001556 precipitation Methods 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000005096 rolling process Methods 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 12
- 229910052718 tin Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 9
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 238000001887 electron backscatter diffraction Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 description 47
- 239000002244 precipitate Substances 0.000 description 26
- 238000005098 hot rolling Methods 0.000 description 25
- 238000001953 recrystallisation Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 17
- 238000001816 cooling Methods 0.000 description 15
- 238000005097 cold rolling Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 235000013339 cereals Nutrition 0.000 description 9
- 238000007747 plating Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 7
- 229910000679 solder Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 238000005538 encapsulation Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 208000037656 Respiratory Sounds Diseases 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910000906 Bronze Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 235000020985 whole grains Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
- C22F1/08—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)
- Materials Engineering (AREA)
- Mechanical 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 present invention provides a kind of with high intensity, heat resistance and the excellent Fe P series copper alloy plates of oxide-film adhesion.By constituting as follows：Fe：1.6~2.6 mass %；P：0.01~0.15 mass %；Zn：0.01~1.0 mass %；Sn and Mg more than one：0.1~0.5 mass %；C：Below 0.003 mass %；Co, Si and Cr are added up to below 0.05 mass %；Surplus is made up of Cu and inevitable impurity, when observing the crystalline structure in section parallel with rolling direction and vertical with plate face with EBSD, to the weighted average that the diameter of equivalent circle of each crystal grain is weighted it is less than 10 μm with area, conductance is more than 50%IACS, Vickers hardness is more than 180Hv, and diameter of equivalent circle is that the presence density of the precipitation particles of the Fe or Fe P-compounds of 10~40nm is 20/μm2More than.
Description
Technical field
The present invention relates to intensity, heat resistance and excellent in bending workability, be suitable as semiconductor lead frame, terminal,
The Fe-P series copper alloy plates of the electric electronic element material of connector, busbar etc..
Background technology
Copper and acid bronze alloy are very high due to conductance heat conductivity, it is possible to as the electricity headed by lead frame
Pneumoelectric subcomponent material.In recent years, the thin-walled of lead frame, thin pin, thin spaceization are increasingly advanced, and a part is even up to
Below 100 μm of thickness, this requirement has intensity very high.
In addition, in the making of lead frame, the web for copper and acid bronze alloy to be rolled into specific thickness can be carried out,
Implement punch process, etching process and be processed into the operation of the shape of regulation.In punch process, for eliminating punching belt
Strain strain relief operation in, with more than 400 DEG C of temperature heat etc. and implement the situation of high-temperature heating treatment also very
It is many.Additionally, can also implement the die molding and wire bonding in the treatment of various platings, encapsulation process, resin moulded.
Therefore, for blaster fuse frame material, conductance, intensity (key property) are not required nothing more than, also require stampability,
Heat resistance (degree of intensity decreases when being heated to high temperature), in addition with etching, various platings, solder adhesion, oxygen
Change (secondary characteristics) such as film adhesion, resin adhesion, wire bondings.
Although without all fully meeting the materials of these characteristics, as the blaster fuse frame material of many pin IC, from
Characteristic, cost, can be from the viewpoint of availability, by with Cu-2.2 mass %Fe-0.03 mass %P-0.12 mass %Zn
It is mark for the CDA Alloy 194 of standard chemical composition, with Cu-3.0 mass %Ni-0.65 mass %Si-0.15 mass %Mg
CDA Alloy7025 of quasi- chemical composition and with Cu-0.23 mass %Cr-0.25 mass %Sn0.20 mass %Zn as standard
The CDA Alloy 18045 of chemical composition are included.Further, so-called CDA means copper development association of the U.S..
Here, particularly in the blaster fuse frame material of many pin IC for needing intensity, use intensity highest CDA
Alloy 7025 (Vickers hardness 200Hv).But, in the material because it is a large amount of containing the Ni for reducing the adhesion of oxide-film,
Si, so there is the low such shortcoming of adhesion of oxide-film.
Semiconductor device turns into master by the encapsulation of thermosetting resin encapsulation of semiconductor chip from economy this point
Stream, it is important that the reliability for remaining potted.The reliability of encapsulation depends on the adhesion of moulding resin and lead frame.If through
The low oxide-film of adhesion is formed in lead frame surface by the thermal process in the assembling procedure of semiconductor device, then molding tree
Fat is reduced with the adhesion of lead frame, heat during due to being installed to printed circuit board (PCB), is caused encapsulation crackle, is peeled off generation, envelope
The reliability reduction of dress.
Therefore, in order to ensure the reliability of encapsulation, it is important that the adhesion of the oxide-film of blaster fuse frame material is high, but
The characteristic of CDA Alloy 7025 is low.In addition, CDA Alloy 7025 also have because etching and processing etc. occur dirt, plating it is close
The problems such as connecing property is reduced, there is in price also unworkable one side high.
On the other hand, the CDA Alloy 194 of Fe-P systems, even as the ESH of maximum intensity quality, intensity is still very
Low, tensile strength is 550N/mm2Left and right, Vickers hardness is 160Hv or so.Other heat resistance also than relatively low, if for example with 450
DEG C heating 5 minutes or so, then soften to less than the 80% of script intensity.But, CDA Alloy 194 are secondary stampability etc.
There is no great defect in characteristic, the adhesion of oxide-film is also excellent, it is cheap and can availability it is also good, therefore made extensively
With.
Described in patent document 1 by adding Mg and Sn in Fe-P series copper alloys, make Fe-P series copper alloys high-strength
Degreeization.In addition, in patent document 2, describing, by making crystalline structure whole grain, and stampability (punching processing is improved
And bendability) Fe-P series copper alloy plates.Described in patent document 3 and carried out for Fe-P series copper alloys by taking
Hot rolling and it is cold rolling after, be heated to 950~1050 DEG C, then carry out being chilled to less than 300 DEG C solution treatment etc. specifically manufacture
Method, so as to improve the intensity and heat resistance of Fe-P series copper alloy plates.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 4-41631 publications
Patent document 2：Japanese Unexamined Patent Publication 2000-104131 publications
Patent document 3：Japanese Unexamined Patent Publication 2012-57242 publications
Invent problem to be solved
But, although the Fe-P series copper alloy plate high intensity of patent document 1, heat resistance be cannot say for sure fully, in addition for
Stampability is studied.Although the Fe-P series copper alloy plate stampabilities of patent document 2 are excellent, heat resistance be cannot say for sure fully.
Although the Fe-P series copper alloy plate intensity and excellent heat resistance of patent document 3, study for stampability.
The content of the invention
The present invention be in view of present situation as Fe-P series copper alloy plates and complete, its object is to, there is provided it is a kind of high-strength
Degree, heat resistance is high, and the also excellent Fe-P series copper alloy plates of stampability (particularly bendability).
Means for solving the problems
Fe-P series copper alloys plate of the invention is characterised by, by constituting as follows：Fe：1.6~2.6 mass %；P：0.01
~0.15 mass %；Zn：0.01~1.0 mass %；Sn and Mg more than one：0.1~0.5 mass %；C：0.003 mass %
Below；Co, Si and Cr are added up to below 0.05 mass %；Surplus is made up of Cu and inevitable impurity, with EBSD observation with
During the crystalline structure in parallel and vertical with the plate face section of rolling direction, the diameter of equivalent circle of each crystal grain is weighted with area
Weighted average be less than 10 μm, conductance be more than 50%IACS, Vickers hardness be more than 180Hv, diameter of equivalent circle 10~
The presence density of the precipitation particles of the Fe or Fe-P compounds of 40nm is 20/μm2More than.Further, in the present invention, " copper is closed
Golden plate " this term is used with the meaning comprising copper alloy bar.
Invention effect
In accordance with the invention it is possible to provide with the intensity close to CDAAlloy 7025, intensity, heat resistance and oxide-film
The excellent Fe-P series copper alloy plates of adhesion.
Brief description of the drawings
Fig. 1 is the microscope macrograph of No.20,21,23 of embodiment.
Specific embodiment
Hereinafter, more specifically it is illustrated for Fe-P series copper alloys plate of the invention.
(chemical composition of Fe-P series copper alloys)
Fe contributes to the raising of the intensity and heat resistance of Fe-P series copper alloy plates, in addition, tying in having suppression hot rolling or again
The effect of the grain growth in crystalline substance heat treatment.When the content of Fe is less than 1.6 mass %, the effect above is insufficient.On the other hand, if
The content of Fe is higher than 2.6 mass %, then generate thick Fe particles because two liquid phase separations, crystallization are separated out when melting, casting
(more than diameter number μm), plating, etching reduction.Therefore, the content of Fe is 1.6~2.6 mass %, and lower limit is preferably 1.7
Quality %, more preferably 1.8 mass %, the upper limit are preferably 2.5 mass %, more preferably 2.4 mass %.
P also forms the precipitation particles of Fe-P compounds in addition to helpful as deoxidier, makes Fe-P series copper alloy plates
Intensity and heat resistance improve.In addition, effects of the P with the grain growth in suppression hot rolling or in dynamic recrystallization treatment.P's contains
When amount is less than 0.01 mass %, the effect above is insufficient.On the other hand, if the content of P is higher than 0.15 mass %, conductance drop
It is low, and oxide-film adhesion reduction.Therefore, the content of P is 0.01~0.15 mass %, and lower limit is preferably 0.015 matter
Amount %, more preferably 0.02 mass %, the upper limit is preferably 0.13 mass %, more preferably 0.10 mass %.
Zn improves the adhesion of the solder heat resistance fissility of Fe-P series copper alloy plates, oxide-film.The content of Zn is less than
During 0.01 mass %, its effect is insufficient, on the other hand, if being higher than 1.0 mass %, conductance reduction.Therefore, the content of Zn
It is 0.01~1.0 mass %, lower limit is preferably 0.02 mass %, more preferably 0.05 mass %, and the upper limit is preferably 0.8 matter
Amount %, more preferably 0.5 mass %.
Sn and the Mg solid solution in mother metal, with the effect that the intensity for making Fe-P series copper alloy plates and heat resistance are improved, can add
Plus more than one (one kind of Sn or Mg or its both) of Sn and Mg.More than one the content of Sn and Mg is less than 0.2 mass %
When, the effect above is insufficient, it is impossible to meet more than Vickers hardness 180Hv.On the other hand, if the content of more than one of Sn and Mg
Higher than 0.5 mass %, then the adhesion reduction of conductance reduction, and oxide-film.Therefore, more than one the content of Sn and Mg
It is 0.2~0.5 mass %, lower limit is preferably 0.25 mass %, more preferably 0.3 mass %, and the upper limit is preferably 0.45 mass %,
More preferably 0.40 mass %.
In Fe-P series copper alloys, if it is higher than 0.003 mass % as the content of the C of inevitable impurity, or equally
It is higher than 0.05 mass % as the total of content of Co, Si and Cr of inevitable impurity, then two liquid phase separations, crystallization is separated out
The thick Fe particles for causing easily are generated.Therefore, the intensity of Fe-P series copper alloys and heat resistance reduction, in addition, plating, erosion
Quarter property is reduced.Therefore, C content is made for below 0.003 mass %, the total content for making Co, Si and Cr is below 0.05 mass %.
Further, the wood of molten surface is dispersed in when there is situation as follows, i.e. C due to fusing, casting for the purpose such as anti-oxidant
Charcoal, granular graphite and graphite jig etc. and infinity is mixed into.In this case, in order to reduce C content, following means can be utilized：
Use the few Fe raw materials of C content；Reduce charcoal, the dispersion volume of granular graphite；Increase charcoal, the size of granular graphite and reduce and liquation
Contact area；Carry out mould change etc..
(average crystal grain diameter)
With EBSD (Electron BackScatter Diffraction) observation Fe-P series copper alloy plates and rolling side
To crystalline structure (the crystal boundary condition in parallel and vertical with plate face section：More than 5 ° of misorientation), try to achieve all brilliant of sightingpiston
The diameter of equivalent circle of grain, weighted average is tried to achieve so that area is weighted to the diameter of equivalent circle of each crystal grain, in the present invention will
It is used as average crystal grain diameter.Its weighted average why is taken as average crystal grain diameter, because as Fe-P series copper alloy plates
When so having thick grain to mix with microfine, if only taking, addition is average, the crystal grain diameter for drawing is small must to exceed actual conditions.
If the average crystal grain diameter is higher than 10 μm, bendability, punching processing reduction, and intensity, heat resistance are also reduced.Cause
This, average crystal grain diameter is less than 10 μm, more preferably preferably less than 8 μm, less than 6 μm.Average crystal grain diameter is the smaller the better,
Lower limit does not need tailor-made, but can be allowed to miniaturization to 3 μm or so according to manufacture method described later.
(the presence density of precipitation particles)
The precipitation particles of 10~40nm of diameter of equivalent circle among the precipitation particles of Fe or Fe-P compounds, by dislocation pinning
Improve the intensity of Fe-P series copper alloy plates and heat resistance.But, if the presence density of the precipitation particles is less than 20/μm2Then
The precipitation particles that anchoring can be carried out is few, and the raising of intensity and heat resistance is insufficient.Therefore, the Fe of 10~40nm of diameter of equivalent circle
Or the presence density of the precipitation particles of Fe-P compounds is 20/μm2More than, preferably 25/μm2More than, more preferably 30
Individual/μm2More than.There is density and be the bigger the better in it, higher limit does not need special provision, if in compositing range of the invention,
Then by manufacture method described later, density can be promoted to 40/μm2Left and right.
(manufacture method of Fe-P series copper alloy plates)
Manufacture method of the invention is as follows.
First, ingot bar is by using melt raw materials such as common crucible-type smelting furnaces, after carrying out composition adjustment, then to usual
Metal die, carbon mold etc. among pour into a mould liquation and manufacture.
Secondly, ingot bar is heated to 850~1050 DEG C of temperature, hot rolling, hot rolling is carried out with Reduction by rolling more than 50%
End temp be more than 750 DEG C.Cooling after hot rolling, by water-cooled etc., with more than 10 DEG C/sec cooling velocities, for from
The scope of hot rolling end temp (=cooling started temperature) at least to 300 DEG C is rapidly cooled down.
When the heating-up temperature of hot rolling is less than 850 DEG C, Fe, Fe-P compound are separated out and coarsening, therefore this part Fe, P quilt
Consumption, fine Fe, Fe-P compound separated out through separating out heat treatment is reduced, the intensity of product, heat resistance reduction.The opposing party
Face, close to fusing point if higher than 1050 DEG C, therefore hot-rolled crackle occurs.In addition, oxidation aggravation, causes oxide to be rolled up by hot rolling
Enter, in remaining in sheet as defect.Therefore, the heating-up temperature of hot rolling is 850~1050 DEG C, preferably 870~1030
DEG C, more preferably 890~1010 DEG C.
If the Reduction by rolling of hot rolling is smaller than 50%, recrystallization is not caused, there is the possibility of cast sturcture's remaining.Cause
This, the Reduction by rolling of hot rolling is more than 50%, preferably more than 60%, more preferably more than 70%.
If the end temp of hot rolling is less than 750 DEG C, the amount of precipitation of Fe, Fe-P compound increases and coarsening, therefore
Separate out fine Fe, Fe-P compound separated out in heat treatment to reduce, intensity and the heat resistance reduction of sheet.If in addition, heat
The end temp for rolling is less than 750 DEG C, then the average crystal grain diameter of sheet becomes big.This is considered as Fe, the Fe- due to coarsening
P-compound, as the starting point of recrystallization, promotes recrystallization in dynamic recrystallization treatment.Therefore, the end temp of hot rolling is 750 DEG C
More than, preferably more than 770 DEG C, more preferably more than 790 DEG C.
Cooling velocity after hot rolling, if from hot rolling end temp to being less than 10 DEG C/sec in the range of 300 DEG C, cooling down
In also have Fe, Fe-P compound separate out and coarsening, therefore separate out heat treatment in separate out fine Fe, Fe-P compound subtract
It is few, intensity and the heat resistance reduction of sheet.Therefore, the cooling velocity after hot rolling is more than 10 DEG C/sec, preferably 20 DEG C/sec
More than, more preferably more than 30 DEG C/sec.After hot rolling material cooling reaches 300 DEG C, it is not necessary to chilling.
Thereafter, the oxide skin of hot rolling material is removed, is carried out cold rolling.In order to be obtained in the dynamic recrystallization treatment for subsequently carrying out
Even recrystallized structure, cold rolling Reduction by rolling is more than 50%, preferably more than 60%, more preferably more than 70%.
Dynamic recrystallization treatment is the heat treatment for forming fine recrystal grain, with 550~900 DEG C of left sides of heating-up temperature
It is right to be kept for 1 second~10 minutes or so.When heating-up temperature is less than 550 DEG C, it is difficult to recrystallize, if being higher than 900 DEG C, recrystallize
Coarse grains.Therefore, heating-up temperature is 550~900 DEG C, more preferably preferably 570~880 DEG C, 590~860 DEG C or so.
Retention time can suitably select according to heating-up temperature, be 1 second~10 minutes short time of degree.If the retention time is less than 1 second,
Then it is difficult to recrystallize.If the retention time is higher than 10 minutes, recrystal grain coarsening, the average crystal grain diameter of sheet becomes
Greatly.In addition, Fe, Fe-P compound amount of precipitation increase and coarsening, therefore behind precipitation heat treatment in separate out it is fine
Fe, Fe-P compound reduce.Therefore, the retention time be 1 second~10 minutes, preferably 2 seconds~5 minutes, more preferably 5 seconds~
2 minutes or so.
In addition, scope of the firing rate of dynamic recrystallization treatment more than 300 DEG C is more than 1 DEG C/sec.The firing rate is low
When 1 DEG C/sec, there is the precipitation of Fe, Fe-P compound in heating, cannot get fine recrystal grain.This be considered as by
Fe the and Fe-P compounds separated out in heating coarsening with the rising of temperature, its starting point for turning into recrystallization promotes again
Crystallization.In addition, because there is precipitation and the coarsening of Fe, Fe-P compound in heating, being separated out in heat treatment is separated out
Fine Fe, Fe-P compound is reduced.Therefore, the firing rate of dynamic recrystallization treatment is more than 1 DEG C/sec, preferably 2 DEG C/sec
More than, more preferably more than 5 DEG C/sec.
Additionally, the cooling velocity after dynamic recrystallization treatment is more than 5 DEG C/sec from heating-up temperature to 300 DEG C of scope.The temperature
When the cooling velocity for spending scope is less than 5 DEG C/sec, there is precipitation and the coarsening of Fe, Fe-P compound in cooling, therefore separating out
Fine Fe, Fe-P compound separated out in heat treatment is reduced.Therefore, the cooling velocity after dynamic recrystallization treatment be 5 DEG C/sec with
On, preferably more than 10 DEG C/sec, more preferably more than 20 DEG C/sec.
After dynamic recrystallization treatment, carry out or do not carry out cold rolling, carry out precipitation heat treatment.It is for a large amount of to separate out heat treatment
The heat treatment of the precipitate of fine (diameter of equivalent circle is 10~40nm's) Fe, Fe-P compound of generation, although do not carry out cold
Rolling can also generate precipitate, but cold rolling by carrying out, and precipitate can be made expeditiously to separate out, and further improve intensity.
Separate out the degree that heat treatment is kept 0.5~30 hour with the degree of 300~600 DEG C of heating-up temperature.Heating-up temperature is low
When 300 DEG C, amount of precipitation is few, if being higher than 600 DEG C, the easy coarsening of precipitate.Therefore, heating-up temperature is 300~600 DEG C,
Preferably 320~580 DEG C, more preferably 340~560 DEG C.Retention time can suitably select according to heating-up temperature, be 0.5~
The time of 30 hours or so.When retention time is less than 0.5 hour, precipitation is easily insufficient, if being higher than 30 hours, to productivity
The influence of reduction becomes big.Therefore, the retention time is 0.5~30 hour, more preferably preferably 1~25 hour, 1.5~20 hours
Left and right.
Further, it is preferably repeated multiple times to carry out precipitation heat treatment in order to further improve intensity.Carry out at multiple precipitation heat
, it is necessary to be carried out between heat treatment is separated out cold rolling during reason.It is cold rolling by this and formed as Fe, Fe-Pization in copper alloy plate
The part of the drop out point of compound, it is new in precipitation heat treatment behind to form precipitate.If carrying out repeatedly separating out heat treatment, analyse
The density for going out thing increases, it is possible to increase intensity., it is necessary to separate out the hardness after heat treatment the when repeatedly separate out heat treatment
The 1st high, the 2nd high, more many modes higher of number of times of precipitation heat treatment of the 3rd ratio of 2 ratios are appropriate to select precipitation to be heat-treated
Cold processing ratio between condition (temperature, time) and precipitation heat treatment.That is, selected condition is, by the 2nd later precipitation
Heat treatment, in addition to the precipitate for existing before this, can also newly form the bar of the precipitate of 10~40nm of diameter of equivalent circle
Part.Specifically think, for example, more repeat to separate out the number of times of heat treatment, more make the temperature reduction that precipitation is heat-treated.Separate out at heat
Hardness after reason, even if also not uprised repeatedly or during step-down on the contrary repeating to separate out heat treatment, then precipitate coarsening, fine
The density of precipitate does not increase.
Then carry out final cold rolling, reach the intensity and thickness of slab of regulation.After final cold rolling, it is also possible to carry out low temperature
Annealing (also referred to as stress relief annealing).With semiconductor device miniaturization, it is highly integrated and come the fine of lead frame match somebody with somebody
Line, the quality requirements of glacing flatness and reduction internal stress on plate are increasingly improved, and process annealing is improved for these qualities
Effectively.
【Embodiment】
Composition adjustment is carried out after smelting copper alloy raw material in coreless induction furnace, (cooling means is as water with carbon mold ingot casting
It is cold), obtain thickness 50mm, width 180mm, the ingot bar of length 100mm.The chemical composition of the Fe-P series copper alloys for obtaining is displayed in
In table 1.Further, the Fe-P series copper alloys shown in table 1 are in addition to the element shown in table 1, also containing inevitable impurity, its
Middle Ti, Zr, Be, V, Nb, Mo, W, Mg total amount is below 0.01 mass %, B, Na, S, Ca, As, Se, Cd, In, Sb, Pb, Bi, MM
(mixed rare earth alloy) total amount is below 0.005 mass %.These elements are a small amount of, to Fe-P series copper alloys plate of the invention
Characteristic is not impacted.
【Table 1】
* it is unsatisfactory for regulation part of the invention
Then, after each ingot bar being heated into 1hr with 950 DEG C, thickness 18mm is hot-rolled down to, water-cooled is carried out after hot rolling.On heat
The end temp (cooling started temperature) for rolling, No.1~23,25~28 are more than 750 DEG C, and only No.24 is less than 750 DEG C.
No.24 because extending interpass time, the end temp step-down of hot rolling.The cooling velocity of the water-cooled for carrying out after hot rolling
All more than 10 DEG C/sec.
After carrying out facing except descale, to reach thickness 16mm for the two sides of the hot rolled plate of No.1~28, enter
The cold rolling, dynamic recrystallization treatment of row, precipitation heat treatment, final cold rolling and stress relief annealing, obtain the Fe-P systems copper of thickness 0.15mm
Alloy sheets.Further, on separating out the number of times being heat-treated, No.1~10,13~25,28 are 1 time.No.11,12,26,27 carry out 2
It is secondary to separate out heat treatment, carried out with 60% working modulus after the 1st precipitation heat treatment cold rolling.
Hot rolling end temp, dynamic recrystallization treatment, the process conditions of the rolling rate for separating out heat treatment and final cold rolling show
In table 2.
【Table 2】
The Fe-P series copper alloys plate that will be obtained as sample, by following main points determine average crystal grain diameter, precipitate density,
Hardness, conductance, W bendabilities, solder heat resistance fissility, the measure of oxide-film adhesion before and after tensile strength, heating.Its knot
Fruit is displayed in table 3.In addition, with light microscope (multiplying power：500 times) observation obtained by Fe-P series copper alloy plates surface,
Investigation is whether there is because of the thick Fe particles that two liquid phase separations, crystallization are separated out and occurred.On observe thick Fe particles No.20,
21st, 23, its microscope macrograph shows in Fig. 1.The particle of slightly deep grey is thick Fe particles.
(average crystal grain diameter)
With the crystalline structure in the section parallel with rolling direction and vertical with plate face of EBSD observation samples, will be with crystal boundary bar
Part：Whole crystal grain that misorientation is parsed for more than 5 ° are quantized with diameter of equivalent circle, and each crystal grain is worked as with area
Amount circular diameter is weighted and tries to achieve weighted average, in this, as the average crystal grain diameter of sample.Therefore, average crystal grain diameter by
Following formula is calculated.
Average crystal grain diameter=(a1 × d1+...+aN × dN)/A
Wherein, ai：The area of each crystal grain
di：The diameter of each crystal grain
A：The area sum of N number of crystal grain.
(precipitate density)
The tissue of sample is observed with 150,000 times of transmission electron microscopes, it is more than 10nm and below 40nm to determine particle diameter
Precipitation particles number, calculate per unit area in number (it is individual/μm2), as precipitate density.
(tensile strength)
Being made by sample makes the longitudinally JIS-5 test film parallel with rolling direction, according to the benchmark of JISZ2241
Tension test is carried out, is measured.
(hardness before and after heating)
With micro Vickers apply 4.9N load, determine from sample extract test film heating before hardness and
Hardness after being heated 1 minute with 550 DEG C.Then ,/preceding hardness the ratio of heating is calculated after heating.Hardness before heating is in more than 180Hv
For good, after heating/heating before hardness ratio be evaluated as more than 0.90 well.
(conductance)
Sample is passed through into Milling Process into the test film of the slat of 10mm wide × 300mm long, using double bridge formula resistance
Determine device and determine resistance, calculated by averga cross section area method.More than conductance 50%IACS is evaluated as well in the present invention.
(W bendabilities)
L.D. the and T.D. test films of the 10mm wide for being extracted from sample, W bendings (R/t=is carried out according to JCBA-T307
1), observe the outward appearance of bending section and evaluated.In L.D. and T.D. test films are any, there is being evaluated as of crackle × (no
It is good), occur it is shaggy be evaluated as Δ (bad), crackle or rough surface is nonevent is evaluated as zero (good).Further,
So-called L.D. (Londitudinal to Rolling Direction) test film, means that length direction is the parallel side of rolling
To sweep is the test film for rolling vertical direction, so-called T.D. (Transverse to Rolling Direction) experiment
Piece, means that length direction is rolling vertical direction, and sweep is the test film for rolling parallel direction.
(solder heat resistance fissility)
Weak active scaling powder is coated with the test film of the slat extracted from sample, 245 DEG C of welding bath is being held in
(Sn-3%Ag-0.5%Cu) after being impregnated 5 seconds in, with 150 DEG C of stove heat 1000hr.Afterwards, apply for the test film
180 ° of bendings and flex back to be added with work, torn flexing back to be added with after transparent repair sheets band is pasted by the Ministry of worker, according to there is open
It is attached on repair sheets band, whether the solder for observing processing department is peeled off.Stripping film is attached with repair sheets band there occurs stripping
From, × (bad) is evaluated as, without the not peeling-off of attachment stripping film, it is evaluated as zero (good).
(oxide-film adhesion)
Oxide-film adhesion is evaluated by oxide-film contiguity keeping temperature.It is clear alkaline cathode electrolysis to be carried out for sample
After washing, then wash → pickling (10% sulfuric acid) → washing → drying after, heated 5 minutes with various temperature in an atmosphere, make
With the sample after heating, disbonded test is carried out by adhesive tape.Heating-up temperature is changed with 10 DEG C of increment, and the stripping of oxide-film will not occur
From highest temperature as oxide-film touch keeping temperature.It is good that oxide-film contiguity maintains the temperature at more than 300 DEG C.Alkalescence
Catholyte is cleaned with liquid temperature：60 DEG C, cathode-current density：5A/dm2, the time：The condition of 30sec is carried out.Cleaning fluid is with hydrogen
Sodium oxide molybdena is principal component (40%), in addition containing phosphate, silicate, carbonate, surfactant, with the concentration of 50g/L
Dissolve the aqueous solution of representational commercially available alkaline cathode electrolytic cleaned medicament.The disbonded test carried out by adhesive tape, with viscous
The commercially available adhesive tape of patch (Sumitomo 3M societies repair sheets band) and the method torn is carried out.
【Table 3】
* it is unsatisfactory for present invention provide that part
Example No.1~13, in prescribed limit of the invention, the end temp of hot rolling is up to 750 to the composition of copper alloy
More than DEG C, the heating of dynamic recrystallization treatment, cooling velocity are big, and are the holding conditions between high temperature, short time.Therefore, average crystal grain
Diameter is small, and precipitate density is high, with high intensity (including Vickers hardness) and heat resistance, good bendability, solder heat resistance stripping
From property and oxide-film adhesion.
Wherein No.11,12, enter 2 times and separate out heat treatment, and the cold working rate between being heat-treated precipitation is 60%, with chemical group
Compared into the example No.1 being substantially the same, average crystal grain diameter is small, and precipitate density is high, and intensity is high.
On the other hand, No.14 is more because of the content of P, outside prescribed limit of the invention, so conductance is low, oxide-film
Adhesion is poor.
, because the content of P is few, outside prescribed limit of the invention, so crystal grain diameter is big, precipitate density is low for No.15,
Intensity (particularly Vickers hardness) and heat resistance are low, and bendability is poor.
No.16 average crystal grain diameters are small, and precipitate density is high, with high intensity, heat resistance, bendability.But, because Zn
Content it is few, outside prescribed limit of the invention, so solder heat resistance fissility is poor.
No.17 average crystal grain diameters are small, and precipitate density is high, with high intensity, heat resistance, bendability.But, Zn's contains
Amount is more, and outside prescribed limit of the invention, therefore conductance is low.
No.18 is few because of total content of Sn and Mg, outside prescribed limit of the invention, so average crystal grain diameter is small,
Precipitate density is also high, but intensity and heat resistance are low.
No.19 is more because of total content of Sn and Mg, outside prescribed limit of the invention, so conductance is low, oxide-film
Adhesion is poor.
No.20 is more because of the content of C, outside prescribed limit of the invention, so as shown in Fig. 1 (a), thick Fe particles are big
Amount generation, easily generates projection and does not plate portion etc. when carrying out the plating of Ag etc., can speculate that plating is low.In addition, No.20 is averagely brilliant
Grain diameter is big, and precipitate density is low, and compared with the similar No.2 of composition, intensity and heat resistance are low, and bendability is poor.
No.21 is more because of total content of Co, Si, Cr, outside prescribed limit of the invention, so as shown in Fig. 1 (b),
Thick Fe particles are largely generated, and can speculate that plating is low.In addition, No.21 average crystal grain diameters are big, precipitate density is low, with group
Compared into similar No.2, intensity and heat resistance are low, and bendability is poor.
, because the content of Fe is few, outside prescribed limit of the invention, so average crystal grain diameter is big, precipitate is close for No.22
Degree is low, and intensity and heat resistance are low, and bendability is poor.
No.23 average crystal grain diameters are small, and precipitate density is high, with high intensity, heat resistance, bendability.But, Fe's contains
Amount is more, and outside prescribed limit of the invention, therefore as shown in Fig. 1 (c), thick Fe particles are largely generated, and can speculate that plating is low.
No.24 because the end temp of hot rolling is low, be less than 750 DEG C, therefore, average crystal grain diameter is big, precipitate density
Low, intensity and heat resistance are low, and bendability is poor.
No.25 is because the heating of dynamic recrystallization treatment, cooling velocity are small, and are compared with prolonged maintaining item under low temperature
Part, so average crystal grain diameter is big, precipitate density is low, and intensity and heat resistance are low, and bendability is poor.
No.26 because the temperature for separating out heat treatment for the 2nd time is identical with the 1st time, with same composition under except separating out at hot
The No.12 that process conditions beyond reason are similar to is compared, and precipitate density and intensity (containing Vickers hardness) are reduced.
No.27 because the 2nd time separate out heat treatment temperature it is higher, with same composition under except separate out heat treatment in addition to
The similar No.12 of process conditions is compared, precipitate density, intensity (containing Vickers hardness) and heat resistance reduction.In addition, average crystal grain
Diameter is big, and bendability is poor.
No.28 is because the keeping temperature of dynamic recrystallization treatment is high, and average crystal grain diameter is big, intensity (particularly Vickers
Hardness) it is low, bendability is poor.
Claims (1)
1. Fe-P series copper alloy plates of a kind of intensity, heat resistance and excellent in bending workability, it is characterised in that by constituting as follows：
Fe：1.6~2.6 mass %；P：0.01~0.15 mass %；Zn：0.01~1.0 mass %；Sn and Mg more than one：0.2
~0.5 mass %；C：Below 0.003 mass %；Co, Si and Cr are added up to below 0.05 mass %；Surplus is by Cu and can not keep away
The impurity exempted from is constituted, when observing the crystalline structure in section parallel with rolling direction and vertical with plate face with EBSD, with area pair
Below 10 μm, conductance is more than 50%IACS, Vickers hardness to the weighted average that the diameter of equivalent circle of each crystal grain is weighted
It is more than 180Hv, diameter of equivalent circle is that the presence density of the precipitation particles of the Fe or Fe-P compounds of 10~40nm is 20/μ
m2More than.
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| JP7242996B2 (en) * | 2018-03-28 | 2023-03-22 | 三菱マテリアル株式会社 | Copper alloy |
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| JP3772319B2 (en) * | 1997-03-24 | 2006-05-10 | 同和鉱業株式会社 | Copper alloy for lead frame and manufacturing method thereof |
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| CN100510131C (en) * | 2004-08-17 | 2009-07-08 | 株式会社神户制钢所 | Copper alloy plate for electric and electronic parts having bending workability |
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