CN105525135A - Low-anisotropic-index high-intensity Cu-Ni-Si alloy and preparing process thereof - Google Patents
Low-anisotropic-index high-intensity Cu-Ni-Si alloy and preparing process thereof Download PDFInfo
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- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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Abstract
The invention discloses a low-anisotropic-index high-intensity Cu-Ni-Si alloy and a preparing process thereof. The low-anisotropic-index high-intensity Cu-Ni-Si alloy and the preparing process are suitable for cold rolling copper-based thin panels for lead frames. The alloy comprises, by chemical mass percent, 2%-3% of Ni, 0.5%-1.0% of Si, 0.1%-0.5% of Sn, 0.05%-0.1% of Fe, 0.1%-0.3% of Mg, 0.05%-0.08% of Zn, 0.2%-0.5% of RE and the balance Cu. Yttrium-based heavy rare earth is added for purifying a copper solution, and Ni2Si precipitation is improved; meanwhile, harmful texture is effectively restrained through the process that low temperature annealing is combined with grading solid dissolving before solid dissolving; and by controlling the cold rolling reduction rate, a transverse shearing belt is obtained for a product, and anisotropism is greatly improved. The alloy has the beneficial effects that the strength of extension ranges from 650 MPa to 750 MPa, the elongation ranges from 13% to 18%, the in-plane anisotropy (IPA) of the intensity is smaller than 6%, the in-plane anisotropy (IPA) of the elongation is smaller than 8%, and defects of warping, deformation and cracking of the Cu-Ni-Si alloy in the blanking process can be effectively reduced.
Description
Technical field
The present invention relates to the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index and preparation technology thereof, be specially adapted to cold rolled sheet material used for lead frame, belong to high property copper alloy exploitation and processing technique field.
Background technology
Cu-Ni-Si system (C7025) alloy belongs to typical ageing strengthening type high strength and medium conductivity alloy, is widely used in the electron devices such as lead frame, terminal and junctor owing to having good weldability, solidity to corrosion, oxidation-resistance and plasticity.In the last few years, in order to meet market and research and development needs, the C7025 alloy of different-alloy system is researched and developed successfully in laboratory in succession, large quantity research has been made both at home and abroad in its microalloying mechanism, preparation technology and microtexture, obtain intensity to coordinate with the excellent of conductivity, but, C7025 lumber recovery in actual production process is lower, unstable product quality, downstream client's objection product is frequent, the use properties of product is poor, is in particular in that crackle appears in hot-rolled sheet, easily occurs burr and the problem such as bending during product stamping-out.The anisotropy of C7025 alloy, after especially cold rolling thermal treatment, the anisotropy of product is the key factor affecting product deep processing quality.
As everyone knows, Cu-Ni-Si alloy processing and heat treatment process in, the otherness of weave construction, and the formation of modulated structure and thermal treatment texture all can to its anisotropy behavior generation certain influence.How reducing the anisotropic index of Cu-Ni-Si alloy further, improve the over-all properties of product, is the further industrialization key issue of restriction copper alloy for lead-wire frame strip.Large quantity research has been done in the anisotropy behavior to aluminium, copper alloy such as SNGHRK, and propose concept IPA (the %) (IPA of plane anisotropy index, in-planeanisotropy,=(2Xmax-Xmid-Xmin)/2Xmax, Xmax represents the maximum value of three direction mechanical properties, Xmid represents intermediate value, and Xmin represents minimum value), quantification can characterize the different sexual behaviour of sheet alloy by anisotropic index.
From strengthening means; patent [ZL200410036828.9] protects emphatically the impact of the ratio alloy performance of Ni and Si; patent [CN102703754B] refer to increase V and carrys out crystal grain thinning; high-strength highly-conductive Cu-Ni-Si alloy can be obtained; patent [CN102021359B] mentions classification rolling technique, can obtain the strong Cu-Ni-Si alloy of superelevation.Above patent documentation is all the precipitation thermodynamics and dynamics conditions being controlled second phase particles by Composition Design and process innovation, plays the effect of refined crystalline strengthening and precipitation strength further.But, the performance index of intensity and deep shaping property conflict often.Although Second Phase Precipitation amount is higher, intensity and conductivity better, excessive second-phase can cause the behavior of sheet material anisotropy to increase the weight of, bending machining performance decline.
Following patent documentation is protected from Grain Boundary Character, grain morphology and the optimization method of texture angle to the bending property of Cu-Ni-Si alloy respectively:
Patent documentation [1] CN101503770A
Patent documentation [2] CN103781925A
Patent documentation [3] CN102985572A
Patent documentation [4] CN103429771A
Patent documentation [1] by control alloyed copper sheet alloy 420} and 220} crystal plane and pure copper powder { 420} is with { the X-ray intensity ratio of 220} crystal plane and the grain size of sheet material, to improve bending machining performance and the proof stress relaxation property of alloy.And in the grain orientation relation of this copper alloy plate X-ray intensity than formula (1) and formula (2) below meeting, when the average crystal grain diameter of alloy is between 10-60 μm, copper alloy plate obtains has good bending machining performance and proof stress relaxation property.
I{420}/I
0{420}＞1.0(1)
I{220}/I
0{220}≤3.0(2)
Wherein I is that the X-ray diffraction of this copper alloy plate crystal plane is strong, I
0it is the X-ray diffraction intensity of standard pure copper powder crystal plane.
In patent documentation [2], by controlling the content of different texture in copper alloy plate, improve intensity and the bending machining performance of copper alloy.And find that { area occupation ratio of 001}<100> is more than 5% when Cube orientation, { area occupation ratio of 110}<112> is below 20% for Brass orientation, { area occupation ratio of 112}<111> is below 20% for Copper orientation, when work hardening exponent is below 0.2, copper alloy plate has excellent intensity, bendability.
In patent documentation [3], inventor controls between 0.4-0.6 by the mean value of the aspect ratio (major diameter of the minor axis/crystal grain of crystal grain) by crystal grain in alloy structure, mean value in all crystal grains of Goss texture controls between 1.2-1.5, special grain boundary ∑
6all grain boundaries length and L
бwith the ratio (L of all special grain boundary length and L
б/ L) control between 60-70%, obtaining elastic limit value is 450-600N/mm
2, at 150 DEG C, the solder heat resistance separability of 1000 hours is good, deep draw excellent in workability.
In patent documentation [4], by controlling top layer and central part in the { { maximum value of the X-ray intensity of 001}<100> orientation on 200} positive pole figure, improve the bendability of sheet alloy, particularly improve the bendability after notch processing.
Above patent, the emphasis of concern mainly concentrates on the intensity of copper alloy plate, bending machining performance, proof stress slackness and separability.From Composition Design angle, adopt the micro alloying elements such as Al, Fe, Sn and Mg, technique, texturing temperature and cold rolling system and draft in major control course of hot rolling, finally implement accurately to control to the texture characteristic of product, grain morphology and Grain Boundary Character.
Summary of the invention
The invention provides a kind of high-strength deep-draw Cu-Ni-Si alloy and preparation technology thereof of less anisotropy index, by adding the Y base mixing RE of trace, coordinate rational cold-rolling process and thermal treatment process, effectively can reduce the anisotropy of high-strength Cu-Ni-Si alloy, be particularly suitable for the punching process of materials of lead frame, significantly reduce warpage, cracking and the defect such as bending.
For achieving the above object, technical scheme of the present invention is:
The high-strength Cu-Ni-Si alloy of a kind of less anisotropy index of the present invention, each component chemical mass percent is as follows: Ni:2 ~ 3%, Si:0.5 ~ 1.0%, Sn:0.1 ~ 0.5%, Fe:0.05% ~ 0.1%, Mg:0.1% ~ 0.3%, Zn:0.05% ~ 0.08%, RE:0.2% ~ 0.5%, remaining as Cu and inevitable impurity, and the mass ratio of Ni and Si is 4 ~ 5.
Preferably, the composition preferred yttrium base ion type rareearth master alloy of described RE mishmetal, wherein Y content accounts for 50%, La content and accounts for 30%, Ce content and account for 20%.
The preparation technology of the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index of the present invention, comprises the steps:
(1) hot rolling technology: carry out melting according to designed each component chemical mass percent, horizontal casting, then hot rolling is carried out to foundry goods obtain hot-rolled sheet, hot rolling start rolling temperature is 850 ~ 950 DEG C, finishing temperature is 750 ~ 850 DEG C, carries out softening annealing after hot rolling;
(2) once cold rolling technique: the hot-roll annealing plate in step (1) is carried out once cold rolling;
(3) low-temperature annealing: carry out low-temperature annealing after cold rolling in step (2);
(4) grade and stage process: rapid classification solid solution is carried out to low-temperature annealing plate in step (3);
(5) secondary cold-rolling technique: secondary cold-rolling is carried out to the sheet material after step (4) solid solution;
(6) low temperature aging process: finally carry out ageing treatment to step (5) gained secondary cold-rolling plate, aging temp design is at 400 ~ 500 DEG C, and preferably 430 DEG C ~ 460 DEG C, aging time is 4 ~ 6h.
Preferably, the once cold rolling draft of hot-roll annealing plate is greater than 60% in step (2), applies secondary cold-rolling draft in step (5) between 25 ~ 35%, and preferably about 30%, twice total reduction is more than 85%.
Preferably, in step (3) low-temperature annealing condition be annealing temperature at 100 ~ 300 DEG C, soaking time is 3 ~ 6 hours; furnace cooling; described low-temperature annealing is carried out in the gas shield stove of nitrogen or argon gas, and temperature preferably 200 DEG C, soaking time preferably 4 hours.
Preferably, in step (4), solid solubility temperature design is at 850 ~ 900 DEG C, solution time 60 ~ 80s, solution heat system design first quick and back slow, fast heating rate is 30 ~ 50 DEG C/s preferably, and slow heat is 1 ~ 5 DEG C/s preferably, stagnation point preferably 750 DEG C to 800 DEG C.
Preferably, alloy structure is characterized as with α-Cu for matrix phase, and average crystal grain diameter is 40-60 μm, matrix Dispersed precipitate nano level δ-Ni
2si precipitated phase, and transversely (perpendicular to roll to) there is equally distributed shear zone, matrix texture component meet:
0.6<V
(A+G+B)/V
(C+S)<1.0
Wherein V
(A+G+B)volume fraction sum shared by this sheet alloy A ({ 012}<100>), G (Goss:{011}<100>), B (Brass:{011}<211>) texture component, V
(C+S)it is volume fraction sum shared by this sheet alloy C (Copper:{112}<111>) and S ({ 123}<634>) texture component.
Beneficial effect of the present invention is:
1. the present invention is by carrying out Composition Design and process optimization to Cu-Ni-Si alloy, make full use of yttrium base ionic RE to the purification of melt and Grain refinement, coordinate reasonably cold rolling and thermal treatment process, facilitate the Precipitation of second-phase and the Volume fraction of crucial texture, weave construction can be obtained with α-Cu for matrix, average grain size is at 40 μm ~ 60 μm, sheet material after timeliness has laterally equally distributed shear zone, its tensile strength is between 650 ~ 750MPa, elongation is between 13 ~ 18%, the anisotropic index (IPA) of intensity and elongation is less than the performance of 6% and 8% respectively.
2. the present invention adopts solution heat system first quick and back slow; by rapid heating refinement matrix grain size; reduce recrystallization temperature; be conducive to a small amount of A{012}<100> texture, the formation of Copper texture; simultaneously in slow heat process; now there is recrystallize in crystal grain substantially, and recrystallization texture basically forms, Ni
2si precipitated phase can slowly back dissolving in matrix, for follow-up timeliness lays the foundation.
3., in order to reduce the anisotropy of Cu-Ni-Si alloy strip, this patent, by controlling the draft of once cold rolling and secondary cold-rolling, makes final copper alloy plate obtain transversely equally distributed shear zone.The formation of shear zone can not only improve transverse strength by dislocations strengthening; also impel the crystal grain of Copper orientation and S orientation to turn to Goss orientation by improper slippage and non-crystallographic shear simultaneously; Brass orientation is become again by Goss orientation transition; although the existence of Brass orientation and Goss orientation can reduce anisotropy; if but lateral shear ratio increases; Brass component and the corresponding increase of Goss component; the elongation of Cu-Ni-Si alloy can be had a strong impact on; therefore, the volume ratio of final texture component be controlled within the specific limits.
4. the volume fraction ratio that the final crystal grain of Cu-Ni-Si alloy sheet material that prepared by this technique closes bond orientation meets formula (1) 0.6<V (A+G+B)/V (C+S) <1.0 (1)
Wherein V (A+G+B) is the volume fraction summation shared by this sheet alloy A{012}<100>, Goss{011}<211> and Brass{011}<211> texture, and V (C+S) is this sheet alloy Copper{112}<111> and the volume fraction summation shared by S{123}<634> texture.
5. present invention process is simple, and equipment requirements is not high, and most copper strip processing enterprise all can realize, and is applicable to copper sheet electron devices such as manufacturing materials of lead frame.
Accompanying drawing explanation
Fig. 1 is preparation technology's schematic diagram of the embodiment of the present invention 1;
Fig. 2 is that the OM that organizes of the solid solution state of Cu-Ni-Si alloy sheet material in the embodiment of the present invention 1 schemes;
Fig. 3 is that the OM that organizes in the embodiment of the present invention 1 after Cu-Ni-Si alloy sheet material timeliness schemes;
Fig. 4 is the spatial orientation distribution function figure of Cu-Ni-Si alloy sheet material in the embodiment 1 utilizing XRD to record;
Fig. 5 is the grain orientation distribution plan of Cu-Ni-Si alloy sheet material aging state in embodiment 1.
Embodiment
With concrete embodiment, the present invention is described in further details by reference to the accompanying drawings.
Embodiment 1:
The high-strength Cu-Ni-Si alloy of a kind of less anisotropy index, its each composition component is as table 1:
The chemical composition (wt%) of Cu-Ni-Si alloy in table 1 embodiment 1
| Ni | Si | Mg | Zn | Sn | Fe | RE | Cu |
| 3.12 | 0.72 | 0.226 | 0.06 | 0.51 | 0.076 | 0.3 | Surplus |
A preparation technology for the high-strength Cu-Ni-Si alloy of less anisotropy index, comprises the steps:
(1) carry out melting and casting by the composition of table 1, melting is carried out in medium-frequency induction furnace, and cast ingot dimension is 120 × 100 × 25mm.Strand is heated to 930 DEG C of insulation 2h, two roller hot rollss carry out hot rolling, the start rolling temperature of hot rolling is 920 DEG C, rolling 10 passages, final sheet metal thickness is 5mm, and finishing temperature is 780 DEG C, water-cooled immediately after hot rolling completes, hot-rolled sheet after water-cooled is heated to the softening annealing of 600 DEG C of insulation 12h, carries out the milling face operation of upper and lower 0.5mm after softening annealing;
(2) once cold rolling technique: carry out cold rolling on 4-roller cold rolling mill, the sheet metal thickness after once cold rolling is 0.6mm.
(3) low-temperature annealing: cold rolling complete after sheet material carry out low-temperature annealing, annealing temperature is 200 DEG C, and annealing time is 4h, and annealing atmosphere adopt nitrogen protection.
(4) grade and stage process: stress relief annealed sheet material carries out solution treatment, solid solution craft adopts two-part heating cycle first quick and back slow.First be heated to 780 DEG C in the mode of 45 DEG C/s rapid heating, after be heated to 860 DEG C in the slow heat mode of 5 DEG C/s, solid solution soaking time is 70s, and solution treatment adopts continuous annealing furnace, argon shield.
(5) secondary cold-rolling technique: the sheet material after solid solution carries out secondary cold-rolling, the sheet metal thickness after cold rolling is 0.4mm.
(6) low temperature aging process: the sheet material after secondary cold-rolling carries out ageing treatment, ageing treatment has N
2carry out in the annealing furnace of atmosphere.Aging temp is 450 DEG C, and aging time is 5h.
Comparative example 1:
Be with the difference of embodiment 1, its each composition component of alloy is as following table 2:
The chemical composition (wt%) of Cu-Ni-Si alloy in table 2 comparative example 1
| Ni | Si | Mg | Zn | Sn | Fe | RE | Cu |
| 3.16 | 0.75 | 0.232 | 0.06 | 0.54 | 0.08 | - | Surplus |
Comparative example 2:
Be with the difference of embodiment 1, do not carry out the low temperature annealing process as described in step (3).
Comparative example 3:
Be with the difference of comparative example 1, do not carry out the low temperature annealing process as described in step (3).
Based on above-mentioned, carry out mechanical property, anisotropic index to the result of embodiment 1 and above-mentioned comparative example, the test of the average grain size of crucial texture Volume fraction and final timeliness plate, result is as shown in table 3 below:
The test result of the mechanical property of table 3 embodiment 1 and above-mentioned comparative example, IPA value and crucial texture volume ratio and average grain size
Note: according to the mechanical experimental results in alloy 3 directions, carries out the calculating of the in-plane anisotropy index IPA value of alloy by following formula:
IPA＝(2Xmax-Xmid-Xmin)/2Xmax×100％
Wherein: Xmax, Xmin are respectively the maxima and minima of 0 °, 45 °, 90 ° direction Rm, Rp0.2, A, Xmid is intermediate value.
As shown in Figure 2, the tissue of sheet material solid solution state in embodiment 1, its average grain size is 48 μm; As shown in Figure 3, in embodiment 1, the intra-die of sheet material alloy exists in a large number along the uniform shear zone (Shearband) of horizontal distribution, and this shear zone is one of key factor controlling crucial texture Volume fraction; As shown in Figure 4, can find out, its texture of high-strength Cu-Ni-Si alloy mainly A{012}<100>, Brass{011}<211>, Goss{011}<100>, Copper{112}<111> and S{123}<634> texture of less anisotropy index; As shown in Figure 5, the Copper texture after solid solution and S texture are the texture more easily forming shear zone, and particularly Copper texture, under certain secondary cold-rolling draft, Copper texture is changed to Goss texture by shear zone, and S texture easily changes to Brass texture.Arranged in pairs or groups smoothly by grade and stage and secondary cold-rolling technique and can control the Volume fraction of final texture component very well.
In sum, comparative example 1 and comparative example 1, comparative example 2 and comparative example 3 known, after Cu-Ni-Si alloy adds mishmetal, crystal grain obtains refinement, the tensile strength of alloy, yield strength all have raising in various degree, and unit elongation change is less, and the IPA value of intensity and elongation also obviously reduces.It can also be seen that from table 3, invention example 3,4 all meets the Volume fraction (above formula 1) of crucial texture, control the content of Brass texture and Goss texture preferably, and average grain size is between 40 μm ~ 60 μm.Comparative examples 2 and embodiment 1 known, after adding low-temperature annealing before solid solution, the intensity of alloy improves further, and in embodiment 1, intensity I PA value is all less than 6, and the IPA value of unit elongation is less than 8.
As known by the technical knowledge, the present invention can be realized by other the embodiment not departing from its spirit or essential feature.Therefore, above-mentioned disclosed embodiment, with regard to each side, all just illustrates, is not only.Within the scope of the present invention all or equal the change in scope of the present invention all comprise by the present invention.
Claims (7)
1. the high-strength Cu-Ni-Si alloy of less anisotropy index, it is characterized in that, each component chemical mass percent is as follows: Ni:2 ~ 3%, Si:0.5 ~ 1.0%, Sn:0.1 ~ 0.5%, Fe:0.05% ~ 0.1%, Mg:0.1% ~ 0.3%, Zn:0.05% ~ 0.08%, RE:0.2% ~ 0.5%, remaining as Cu and inevitable impurity, and the mass ratio of Ni and Si is 4 ~ 5.
2. the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index according to claim 1, is characterized in that, the composition preferred yttrium base ion type rareearth master alloy of described RE mishmetal, and wherein Y content accounts for 50%, La content and accounts for 30%, Ce content and account for 20%.
3. a preparation technology for the high-strength Cu-Ni-Si alloy of less anisotropy index as claimed in claim 1, is characterized in that, comprise the steps:
(1) hot rolling technology: carry out melting, horizontal casting according to designed each component chemical mass percent, then hot rolling is carried out to foundry goods obtain hot-rolled sheet, hot rolling start rolling temperature is 850 ~ 950 DEG C, and finishing temperature is 750 ~ 850 DEG C, carries out softening annealing after hot rolling;
(2) once cold rolling technique: the hot-roll annealing plate in step (1) is carried out once cold rolling;
(3) low-temperature annealing: carry out low-temperature annealing after cold rolling in step (2);
(4) grade and stage process: rapid classification solid solution is carried out to low-temperature annealing plate in step (3);
(5) secondary cold-rolling technique: secondary cold-rolling is carried out to the sheet material after step (4) solid solution;
(6) low temperature aging process: finally carry out ageing treatment to step (5) gained secondary cold-rolling plate, aging temp design is at 400 ~ 500 DEG C, and preferably 430 DEG C ~ 460 DEG C, aging time is 4 ~ 6h.
4. the preparation technology of the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index according to claim 3, it is characterized in that, in step (2), the once cold rolling draft of hot-roll annealing plate is greater than 60%, secondary cold-rolling draft is applied between 25 ~ 35% in step (5), preferably about 30%, twice total reduction is more than 85%.
5. the preparation technology of the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index according to claim 3; it is characterized in that; in step (3), low-temperature annealing condition is that annealing temperature is at 100 ~ 300 DEG C; soaking time is 3 ~ 6 hours; furnace cooling; described low-temperature annealing is carried out in the gas shield stove of nitrogen or argon gas, and temperature preferably 200 DEG C, soaking time preferably 4 hours.
6. the preparation technology of the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index according to claim 3, it is characterized in that, in step (4), solid solubility temperature design is at 850 ~ 900 DEG C, solution time 60 ~ 80s, solution heat system design first quick and back slow, fast heating rate is 30 ~ 50 DEG C/s preferably, and slow heat is 1 ~ 5 DEG C/s preferably, stagnation point preferably 750 DEG C to 800 DEG C.
7. according to claim 1 and the high-strength Cu-Ni-Si alloy of a kind of less anisotropy index according to claim 3, it is characterized in that, alloy structure is characterized as with α-Cu for matrix phase, and average crystal grain diameter is 40-60 μm, matrix Dispersed precipitate nano level δ-Ni
2si precipitated phase, and transversely (perpendicular to roll to) there is equally distributed shear zone, matrix texture component meet:
0.6<V
(A+G+B)/V
(C+S)<1.0
Wherein V
(A+G+B)this sheet alloy A({012}<100>), G(Goss:{011}<100>), B(Brass:{011}<211>) volume fraction sum shared by texture component, V
(C+S)this sheet alloy C(Copper:{112}<111>) and S({123}<634>) volume fraction sum shared by texture component.
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| CN112739838B (en) * | 2018-09-27 | 2022-08-02 | 同和金属技术有限公司 | Cu-Ni-Al based copper alloy sheet material, method for producing same, and conductive spring member |
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| CN112813368B (en) * | 2020-12-25 | 2022-05-13 | 大连交通大学 | High-performance Cu-Ni-Si alloy plate strip and production process thereof |
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| CN117403096B (en) * | 2023-12-13 | 2024-03-12 | 宁波兴业盛泰集团有限公司 | High-strength high-conductivity high-temperature-resistant copper-zirconium alloy material and preparation method thereof |
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