CN102978431B - Method for manufacturing copper-iron alloy used for lead frame - Google Patents
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Abstract
The present invention discloses a method for manufacturing copper-iron alloy used for lead frame, comprising the following steps: melting, injecting in a blank mold, cooling; hot rolling and calendaring the casting blank; repeatedly cold rolling and calendaring, and two-stage continuous annealing hot rolled strips; cold rolling processing to make the variation of thickness be above 40%, and then low-temperature annealing to obtain the finished strips. In the manufacturing process, the component content is controlled including 2.0-2.6 wt% of Fe, 0.05-0.1 wt% of Ti, 0.01-0.03 wt% of B, 0-0.05 wt% of Na, 0.01-1.5 wt% of Mo, the balance being Cu and impurities. According to the present invention, the copper iron alloy structure is homogeneous, and the precipitated phase is fine and dispersed. The finished product is high in tensile strength, hardness, conductivity, and elongation, and can meet the demands of the electronics industry on the performance of the lead frame material. The copper iron alloy has excellent hot workability, and is a best material for the production of the lead frame and other electrical and electronic components.
Description
Technical field
The present invention relates to a kind of manufacture method of alloy, relate in particular to a kind of manufacture method of the alloy for the manufacture of down-lead bracket.
Background technology
At present, electronics and information industry has become a mainstay industry of China, and semiconducter device is as the foundation stone of this mainstay industry, and it comprises outer enclosure and internal integrated circuit; Unicircuit (IC) comprises chip, lead-in wire and down-lead bracket, adhesives, packaged material etc.Wherein, the major function of down-lead bracket is for chip provides mechanical support carrier, also has the external circuit of connection simultaneously, transmits the functions such as electrical signal and heat radiation.Therefore IC encapsulation need to possess the over-all propertieies such as high strength, high conduction, high thermal conductivity and good weldability, solidity to corrosion, plastic packaging, oxidation-resistance.
Research, trial-production, the production of China's down-lead bracket material are started late, down-lead bracket copper strips industrial scale is little, description is few, only have at present minority enterprise can produce the seldom alloy of model in batches, and there is quality low precision, quality is unstable, softening temperature is low, internal stress is inhomogeneous, width and the problem such as thickness deviation is overproof, appearance requirement is defective.Copper-iron alloy, as the main raw of manufacturing down-lead bracket, has accounted for 80% of market total value at present, and alloy designations has kind more than 100.
The C194 alloy that wherein China produces is wherein representative a kind of.But the quality of the C194 down-lead bracket copper-iron alloy of producing at present can't meet the demands, low precision, description is few, unstable properties, copper strips yield rate, less than 50%, has larger defect at aspects such as template situation, residualinternal stress, surface smoothness, limit portion burrs.
Summary of the invention
The invention provides the manufacture method of copper-iron alloy for a kind of down-lead bracket, it can effectively solve down-lead bracket and not meet the problems such as production requirement, alloy structure are inhomogeneous, precipitated phase small and dispersed by copper-iron alloy over-all properties, adopts the characteristics such as tensile strength, hardness, unit elongation, specific conductivity and softening temperature of copper-iron alloy prepared by manufacture method of the present invention all can meet preferably the many requirement of electronics industry to down-lead bracket material property.
Copper-iron alloy manufacture method for down-lead bracket of the present invention comprises the following steps:
(1) first major ingredient and auxiliary material are injected to mold after 1250～1350 ℃ of meltings, in the temperature range of liquidus temperature to 380 ℃, with 80 ℃/more than min speed of cooling, carry out coolingly, in manufacturing processed, control alloying constituent and content F e and be 2.0～2.6wt%, Ti and be 0.05～0.1wt%, B and be 0.01～0.03wt%, Na and be 0～0.05wt%, Mo and be 0.01～1.5wt%, all the other components and be Cu and inevitable impurity;
(2) strand obtaining is carried out to hot rolling calendering in the Heating temperature below 1000 ℃, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity;
(3) hot rolled band is carried out repeatedly to cold rolling calendering and 300 ℃～600 ℃ twin-stage continuous annealings, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity;
(4) carrying out cold rolling rolling processing reaches more than 40% its amounts of thickness variation, carry out again 420 ℃ of following low-temperature annealings, obtain band finished product, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity.
Preferably, the major ingredient in step (1) is No. 1 electrolytic copper, and auxiliary material is copper iron master alloy, copper boron master alloy, simple substance titanium, SODIUM METAL and mishmetal.
Preferably, the crystal grain diameter of controlling band in step (2) the hot rolling calendering course of processing is less than 50 μ m;
Preferably, the crystal grain diameter of controlling band in the cold rolled annealed course of processing in step (3) is less than 50 μ m.
Preferably, the copper-iron alloy making through step (4) also contains element and the total amount more than at least one in As, Sb, Bi, Bb, Co, Ni element and is less than 0.05wt%.
Preferably, the tensile strength of described copper alloy is that 600MBa is above, hardness 180Hv above, specific conductivity 66%IACS is above, unit elongation is more than 7.0%.
The preparation method's of down-lead bracket copper-iron alloy of the present invention beneficial effect is:
(1) copper-iron alloy over-all properties of the present invention is superior, alloy structure even, precipitated phase small and dispersed, and alloy price is relatively low, and production efficiency is high;
(2) tensile strength of finished product reaches that 600MBa is above, hardness 180Hv above, specific conductivity 66%IACS is above, unit elongation is more than 7.0%, can meet preferably the many requirement of electronics industry to blaster fuse frame material performance;
(3) down-lead bracket of the present invention also has good hot workability with copper-iron alloy, is conducive to manufacture, and is the best materials of producing the electrical and electronic parts such as down-lead bracket.
Embodiment
In order to make those skilled in the art more clearly understand the copper-iron alloy manufacture method for down-lead bracket of the present invention, below by embodiment, describe its technical scheme in detail.
For meeting desired kind of specific character of the material for electrical/electronic components such as down-lead bracket, the invention provides a kind of manufacture method of the copper-iron alloy for down-lead bracket, select best Ti, B, the component concentration of Na, Mo, with the advanced persons' such as the rolling processing conditions of most suitable slab cooling condition, strand and heat-treat condition process means, manufacture.
In the present invention, all content, proportioning or per-cent are mass ratio.
Down-lead bracket copper-iron alloy, Fe:2.0～2.6wt% in this copper-iron alloy, Ti:0.05～0.1wt%, B:0.01～0.03wt%, Na:0～0.05wt%, Mo:0.01～1.5wt%, in copper alloy, also contain at least one above element and total amount in As, Sb, Bi, Bb, Co, Ni element and be less than 0.05wt%, and S content is below 25BBm; The tensile strength 600MBa of this copper-iron alloy is above, hardness 180Hv is above, specific conductivity 66%IACS is above, unit elongation is more than 7.0%.
Each component content of copper-iron alloy of the present invention: Fe is the main strengthening element in alloy, and alloy is after suitable ageing treatment, and the particle formal distribution that Fe element distributes with disperse is in copper matrix and play ageing strengthening effect.Due to the saturation solubility of Fe under normal temperature in Cu minimum (being only 0.0004% below at 300 ℃), alloy can be realized higher specific conductivity; Can crystal grain thinning by adding a small amount of Fe, postpone the recrystallization process of copper, improve its intensity and hardness, but excessive plasticity, specific conductivity and the thermal conductivity that can reduce copper of Fe element, the addition of Fe element is controlled at 2.0～2.6 scope.
Adding of Ti can prevent from equating effect at metallic matrix with there is fragility second in the middle of coating, can improve the welding property of alloy, but low-alloyed conductivity can fall in excessive interpolation Ti element, the content of Ti element is limited in to 0.05～0.1 scope.
When room temperature, the solubleness of B in copper is almost nil, can reduce specific conductivity and the thermal conductivity of copper, but it has desirable influence to the mechanical property of copper and welding property, B can also improve the mobility of copper-iron alloy melt, B is that the form with reductor adds when copper smelting iron alloy, and unnecessary B is solid-solubilized in copper matrix can prevent hydrogen embrittlement; In the ag(e)ing process of alloy, B is also combined with Fe, forms the precipitate of Fe3B and plays certain ageing strengthening effect.Adding of B is for deoxidation, is solid-solubilized in copper matrix and prevents hydrogen embrittlement, rather than strengthen by separating out Fe3B.When giving full play to the advantageous effect of B element, should reduce B content as far as possible, to guarantee the high conduction performance of alloy, the content of B element is limited to 0.01～0.03 scope.
Add micro-Na that the specific conductivity of copper is declined, but can improve the oxidation-resistance property of copper, and copper is had to desoxydatoin.Identical with the principle that limits B element, the content of Na element is limited in 0～0.05 scope.
The effect of mixed rare-earth elements Mo is mainly:
(1) deoxidation dehydrogenation: the chemically reactive of rare earth is very strong, with the avidity of the oxygen avidity much larger than copper and oxygen, and generates the rare earth oxide that fusing point is higher than copper, density ratio copper is little, receives good desoxydatoin; Rare earth and hydrogen are combined into the hydride that density is little, float up to copper liquid surface, at high temperature again decompose, and discharge hydrogen, or oxidizedly enter slag and be removed;
(2) cleaning molten: rare earth to the effect that removes of other harmful element also clearly, these dystectic rare earth compounds will keep solid state from liquid copper, to discharge together with slag, thereby reach the effect that removes detrimental impurity, rare earth especially can be removed crystal boundary impurity element significantly, impurity element has increased the significant quantity of the elements such as Fe, B after removing, can increase substantially the intensity of alloy;
(3) crystal grain thinning: add Mo in alloy, obvious crystal grain thinning in fusion-casting process, improves alloy alloy plasticity after follow-up thermomechanical treatment;
(4) promote second phase particles to separate out: in alloy, add after Mo, the second phase particles of separating out in band (fe) is tiny, disperse, and size is probably at 5～20nm; In addition, can put forward heavy alloyed recrystallization temperature, thereby improve the high temperature resistance softening performance of alloy after interpolation Mo, the softening temperature of interalloy of the present invention, all more than 480 ℃, adds appropriate mishmetal Mo, and composition range is controlled at 0.01～1.5.
In technical solution of the present invention, based on the impact of sulphur on technique and product in major ingredient impurity, its major ingredient is selected electrolytic copper No. 1, sulfur-bearing as few as possible in impurity, and will prevent punch process time because oil pollution is sneaked into S, even if deformation performance when a small amount of S also can make hot rolling sharply declines, control the content of S, workpiece cracking in the time that hot rolling can being avoided.Conventionally, the content of S must be less than 0.0025wt%, and ideal value is to be less than 0.0015wt%.
Alloy manufacture method for down-lead bracket of the present invention comprises the steps:
(1) first by No. 1 electrolytic copper 1250～1350 ℃ of fusings, after adding the meltings such as copper iron master alloy, copper boron master alloy, sodium simple substance, titanium simple substance and mishmetal, carry out minitype vertical type semicontinuous casting, utilize mold carry out once cooling and utilize water to drench to carry out secondary cooling, make speed of cooling in the temperature range of liquidus line to 380 ℃ 80 ℃/more than min, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are 0.01～1.5wt%;
(2) after strand heats in the temperature range of 900～1000 ℃, through hot rolling calendering, make its thickness reach 6mm, the end temp of hot rolling calendering is 700 ℃, by chilling, make grain-size be less than 50 μ m, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are 0.01～1.5wt%;
(3) hot rolled band being carried out repeatedly to cold rolling calendering, to make its thickness be 1mm, in the temperature range of 300 ℃～600 ℃, carry out twin-stage annealing, make the crystal grain diameter of the calendering band after annealing be less than 50 μ m, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are 0.01～1.5wt%;
(4) cold rolling calendering makes thickness reach 0.5mm, then carries out low-temperature annealing, obtains band finished product; In manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are 0.01～1.5wt%.
In manufacturing process of the present invention: alloy raw material is No. 1 electrolytic copper, copper iron master alloy, copper boron master alloy, sodium simple substance, titanium simple substance and mishmetal, adopt medium-frequency induction furnace melting.
Casting technique after raw material fusing be take continuous casting as best, and semicontinuous casting also can.In castingprocesses in the temperature range of liquidus line to 380 ℃, with 80 ℃/more than min speed of cooling, carrying out coolingly, during lower than 80 ℃/min, will there is the segregation of element in speed of cooling, later hot rolling is brought to adverse influence, and cause the reduction of production efficiency; Control speed of cooling, the temperature range of preferred liquid phase line temperature to 380 ℃; Below 380 ℃, during casting, the length of cooling time changes the excessive segregation that alloying element can not occur.
After melt-casting, carry out hot-work.Hot worked Heating temperature should be the scope of 900～1000 ℃, if temperature surpasses ceiling temperature, it is overheated to occur, and causes hot rolling cracking, reduces production efficiency.While carrying out hot rolling in the temperature range of 900～1000 ℃, small segregation and cast structure will disappear, within the scope of the constituent contents such as Fe of the present invention, Ti, B, can obtain the rolled strip of homogeneous microstructure, more preferably hot rolling temperature is 950 ℃ of left and right.After hot rolling, crystal grain diameter is below 50 μ m, and crystal grain diameter is greater than 50 μ m, and cold processing ratio thereafter, the condition and range of annealing will narrow down, and make deterioration in characteristics.
After hot rolling, carry out as required surfacing cut, repeatedly carry out thereafter the annealing in the temperature range of cold rolling processing and 300～600 ℃.Adopt the twin-stage continuous annealing of low temperature after first high temperature, reach the object (crystal grain diameter is less than 50 μ m) of controlling grain-size and precipitated phase.Temperature is during lower than 300 ℃, and carrying out structure property, to control the required time longer; Surpass 600 ℃, in the short period of time, crystal grain will become thick.If the crystallization crystal grain after annealing is greater than 50 μ m, can make the mechanical characteristicies such as tensile strength and processing characteristics reduce.Therefore make crystal grain diameter be less than 50 μ m, better crystal grain diameter is less than 25 μ m.
Resulting annealed material, carrying out cold rolling rolling processing reaches more than 40% its amounts of thickness variation, also carry out 420 ℃ of following low-temperature annealings, obtain that tensile strength 600MBa is above, hardness 180Hv is above, specific conductivity 66%IACS is above, more than 7.0% copper-iron alloy of unit elongation.When cold processing ratio is discontented with 40%, the insufficient strength because work hardening produces, can not improve mechanical characteristics completely.Therefore desirable working modulus is more than 50%.In order further to carry heavy alloyed tensile strength, hardness, unit elongation, especially the characteristic such as specific conductivity, low temperature annealing process is very necessary, at the temperature of 420 ℃, because of thermal capacity excessive, material is softened at short notice, and no matter adopt intermittent type or continous way, the characteristic that all easily produces material internal is uneven.Therefore, stress relief annealed condition should be below 420 ℃.
Embodiment:
The copper-iron alloy № 1～6 of composition as shown in table 1 (wt%),
Table 1
It should be noted that, in the fusion process of alloy, each element all has scaling loss in various degree, its burn out rate Fe:1～2%, Ti:1～3%, B:2～5%, Na:20～30%, Mo:30～50%; In the process of batching, should supply.When melting starts, first add electrolytic copper and copper iron master alloy, start heating, after its fusing, first add 1/3 copper boron master alloy, insulation 1～3min; Add afterwards titanium, sodium and rare earth, after its fusing, be incubated 3～5min, then add the copper boron master alloy of residue 2/3, after fine melt, be incubated 10min casting; Use the strand of minitype vertical type semicontinuous caster casting 70 * 180 * 1000 (mm), utilize mold carry out once cooling and utilize water to drench to carry out secondary cooling, make speed of cooling in the temperature range of liquidus line to 380 ℃ 80 ℃/more than min.Thereafter, after each strand heats in the temperature range of 900～1000 ℃, through hot rolling calendering so that its thickness is 6mm, from surface and the crackle at edge evaluate hot rolling.After overpickling, the experiment material that does not observe crackle under the opticmicroscope of 50 times is evaluated as, and it is poor that the experiment material that can observe crackle is evaluated as.The end temp of hot rolling calendering is 700 ℃, by chilling, makes grain-size be controlled at 50 μ m left and right.Then carrying out cold rolling calendering, to make its thickness be 1mm, carries out twin-stage anneal in the temperature range of 300～600 ℃, impels second phase particles to separate out raising performance, and carrying out afterwards cold rolling calendering, to make its thickness be 0.5mm again, finally carries out low-temperature annealing.
Clip test film from above resulting band, carries out the mensuration of tensile strength, hardness, unit elongation and specific conductivity, and property indices is all measured according to GB.Resulting outcome record is in table 2 above.
Table 2
Obviously, this copper-iron alloy has good hot workability, is conducive to manufacture, and especially has the characteristics such as good tensile strength, hardness, unit elongation and specific conductivity, is the best materials of producing the electrical and electronic parts such as down-lead bracket; This copper-iron alloy belongs to the row that Cu-Fe is associated golden C194.
By specific embodiment, technical solution of the present invention has been done to further illustrate above, the example providing is only exemplary applications, can not be interpreted as a kind of restriction to the claims in the present invention protection domain.
Claims (5)
1. for a copper-iron alloy manufacture method for down-lead bracket, it is characterized in that, described manufacture method comprises the following steps:
(1) first major ingredient and auxiliary material are injected to mold after 1250～1350 ℃ of meltings, in the temperature range of liquidus temperature to 380 ℃, with 80 ℃/more than min speed of cooling, carry out coolingly, in manufacturing processed, control alloying constituent and content F e and be 2.0～2.6wt%, Ti and be 0.05～0.1wt%, B and be 0.01～0.03wt%, Na and be 0～0.05wt%, Mo and be 0.01～1.5wt%, all the other components and be Cu and inevitable impurity;
(2) strand obtaining is carried out to hot rolling calendering in the Heating temperature below 1000 ℃, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity;
(3) hot rolled band is carried out repeatedly to cold rolling calendering and 300 ℃～600 ℃ twin-stage continuous annealings, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity;
(4) carrying out cold rolling rolling processing reaches more than 40% its amounts of thickness variation, carry out again 420 ℃ of following low-temperature annealings, obtain band finished product, in manufacturing processed, control composition content F e is that 2.0～2.6wt%, Ti are that 0.05～0.1wt%, B are that 0.01～0.03wt%, Na are that 0～0.05wt%, Mo are that 0.01～1.5wt%, all the other components are Cu and inevitable impurity.
2. manufacture method as claimed in claim 1, is characterized in that, the crystal grain diameter of controlling band in step (2) the hot rolling calendering course of processing is less than 50 μ m.
3. manufacture method as claimed in claim 1, is characterized in that, the crystal grain diameter of controlling band in step (3) in the cold rolled annealed course of processing is less than 50 μ m.
4. manufacture method as claimed in claim 1, is characterized in that, the copper-iron alloy making through step (4) also contains element and the total amount more than at least one in As, Sb, Bi, Co, Ni element and is less than 0.05wt%.
5. manufacture method as claimed in claim 1, is characterized in that, the tensile strength of described copper-iron alloy is that 600MPa is above, hardness 180HV above, specific conductivity 66%IACS is above, unit elongation is more than 7.0%.
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