CN108359835A - A kind of high-wearing feature Cu-Ni-Si alloy electronic package materials and preparation method thereof - Google Patents

A kind of high-wearing feature Cu-Ni-Si alloy electronic package materials and preparation method thereof Download PDF

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CN108359835A
CN108359835A CN201810148288.5A CN201810148288A CN108359835A CN 108359835 A CN108359835 A CN 108359835A CN 201810148288 A CN201810148288 A CN 201810148288A CN 108359835 A CN108359835 A CN 108359835A
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copper
alloy
nickel
cobalt
melting
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张毅
高直
安俊超
李丽华
万欣娣
王智勇
劳晓东
孙慧丽
柴哲
宋克兴
田保红
刘勇
国秀花
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Henan University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/28Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon

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Abstract

A kind of high-wearing feature Cu Ni Si alloy electronic package materials, are made of following components in percentage by weight:0.2~1.5% nickel, 0.1~0.6% silicon, 0.1 ~ 0.3% magnesium, 0.1~0.3% silver, 0.2~1.5% cobalt, 0.1~0.5% Cr2O3, 0.1~0.4% PbO, surplus is copper and inevitable impurity element.The present invention has prepared a kind of high-wearing feature and the excellent Cu Ni Si alloy electronic package materials of conductivity and tensile strength by unique preparation process, to meet the performance requirement of copper alloy used for electronic packaging.

Description

A kind of high-wearing feature Cu-Ni-Si alloy electronic package materials and preparation method thereof
Technical field
The present invention relates to Cu alloy material technical field, the Cu-Ni-Si alloy electronics of specifically a kind of high-wearing feature Encapsulating material and preparation method thereof.
Background technology
The blaster fuse frame material indispensable as integrated antenna package carries fixed chip, information output and circuit The multitasks such as heat dissipation.Therefore, hyundai electronics industry be based on use demand, to electronic package material high strength & high electric-conduction with And the requirements such as good heat conductivity are increasingly harsh.In recent years, with electronic unit highly integrated and miniaturization, be thinning Fast development correspondingly also more improves the calling hierarchy of the copper alloy used in integrated circuit.Currently, The circuit lead frame copper alloy mainly developed in the prior art has Cu-Ag, Cu-Mg, Cu-Cr-Zr and Cu-Ni- Si alloys.Wherein, Cu-Ni-Si alloys are widely used with its balanced electric conductivity with hardness number.
But the intensity index of copper alloy and conductive capability have shifting correlation, i.e.,:Ensure preferably to lead Electric rate is it is necessary to making sacrifices to its strength character.Therefore, the key point of alloy preparation technology is to ensure to significantly reduce conduction Under the premise of performance, its intensity is farthest improved.Meanwhile the wear resistance of material is also improved, make in the hope of extending it Use the service life.
Chinese patent on November 29th, 2012(Notification number:CN 102925746 A)A kind of disclosed high-performance Cu-Ni-Si It is that alloy and its preparation and processing method are obtained by techniques such as D.C.casting, hot rolling, annealing, cold rolling, solid solution and ageing treatments The tensile strength of alloy can maintain 730 ~ 820MPa, but conductivity is only capable of maintaining 40 ~ 50%IACS.Chinese patent 2012 6 The moon 5(Notification number:CN 102703754 A)A kind of disclosed high-strength and high-conductivity Cu-Ni-Si based alloys, the alloy Group is divided into:Cu (95.5 ~ 97.5)-Ni (2.0 ~ 3.0)-Si (0.5 ~ 1.2)-V (0 ~ 0.3), elemental vanadium V improves conjunction The timeliness power of gold, timeliness obtains Ni of the Dispersed precipitate of high-volume fractional on matrix in the short time2Si and (NiV)2Si enhances Phase, but its conductivity is not high, only 60%IACS, and the characterization without wear-resisting property.
Invention content
It is asked to solve the technology that Cu-Ni-Si alloy conductives rate in the prior art cannot be taken into account simultaneously with tensile strength Topic.The present invention has prepared a kind of high-wearing feature and the excellent Cu- of conductivity and tensile strength by unique preparation process Ni-Si alloy electronic package materials, to meet the performance requirement of copper alloy used for electronic packaging.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:A kind of high-wearing feature Cu-Ni-Si conjunctions Golden electronic package material, is made of following components in percentage by weight:0.2~1.5% nickel, 0.1~0.6% silicon, 0.1 ~ 0.3% magnesium, 0.1~0.3% silver, 0.2~1.5% cobalt, 0.1~0.5% Cr2O3, 0.1~0.4% PbO, surplus is copper With inevitable impurity element.In the Cu-Ni-Si alloys, the weight proportion of the total weight and silicon of nickel and cobalt is(4~5): 1, and nickel is identical with the weight of cobalt.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
Step 1: preparing intermediate alloy:
(1)It is matched according to above-mentioned weight percent, copper, magnesium, nickel and cobalt is weighed respectively, later, by the copper weighed according to 4:4:2 ratio Example is divided into three parts, then, by 4:4:2 three parts of copper are mixed with the magnesium, nickel and cobalt weighed respectively, obtain copper magnesium compound, Cupro-nickel mixture and copper cobalt mixture;
(2)By step(1)Copper magnesium compound, cupro-nickel mixture or copper cobalt mixture obtained be placed in pressure be 0.04~ Melting is carried out in the argon gas atmosphere smelting furnace of 0.06Mpa, the molten metal that temperature is 1050~1110 DEG C is made, then, by institute Molten metal casting is obtained in the ingot mould for being preheated to 80~120 DEG C, later, by gained ingot casting cooled to room temperature, obtains copper Magnesium intermediate alloy, cupro-nickel intermediate alloy or copper cobalt intermediate alloy, it is spare;
Continuous up-casting:It is matched according to above-mentioned weight percent, weighs pure silicon, silver powder, Cr respectively2O3Powder, PbO powder and step 1 system Copper magnesium intermediate alloy, cupro-nickel intermediate alloy or the merging of copper cobalt intermediate alloy be covered in the vacuum melting furnace crucible of charcoal layer into Row melting obtains liquid alloy, later, under logical argon gas protective condition, carries out drawing company to liquid alloy using trailer system Bar stock is made in continuous casting, spare;
Step 3: continuously extruded:Bar stock made from step 2 is put into continuous extruder, slab is made, it is spare;
Step 4: solution treatment:Slab made from step 3 is placed in heat-treatment furnace, under 870~920 DEG C of temperature conditions, It keeps the temperature 1~2h and carries out solution treatment, then carry out water quenching;
Step 5: pre- cold rolling-timeliness-cold rolling:The pre- cold rolling that deflection is 40~80% is carried out to the slab after step 4 water quenching to become Shape under 400~550 DEG C of temperature conditions, carries out the ageing treatment of 1~4h of heat preservation, followed by second of deflection later For 20~80% cold-rolling deformation to get completed electronic encapsulating material.
Further, in step 1, the temperature when melting is 1230~1280 DEG C, and stove is evacuated to before melting Interior pressure is 5 × 10-2Pa。
Further, in step 2, the guard method of the logical argon gas is that pressure is in applying argon gas to vacuum melting furnace 45kPa, temperature when casting are 1180~1250 DEG C.
Further, in step 2, the casting speed when Continuous Up casting is 280 mm/min.
Further, in step 3, the extrusion ratio of the continuous extruder is 5~10:1, rotating speed is 2 ~ 3r/min, is squeezed Press temperature >=820 DEG C.
Beneficial effects of the present invention:
(1)A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature provided by the present invention are in Cu-Ni-Si alloys On the basis of magnesium, silver, cobalt and trace Cr is added2O3And PbO.Via the effect of the microalloying between various ingredients, tension is constituted Performance and conductivity are excellent, and the electronic package material copper alloy with high-wearing feature.In alloy compositions, nickel is given birth to silicon At Ni2Si, and be precipitated on Cu matrixes, the elongation percentage of alloy can be fully improved, prevents hot calender from cracking.Silver adds Enter to greatly improve the conductivity of alloy, while can also further increase the elongation percentage of alloy;The cobalt added can be uniform Dispersed precipitate is in significantly reducing, the wear rate of alloy on Copper substrate;Cr2O3Wear resistence can be effectively promoted as friction component Can, PbO plays anti-attrition lubricating action.The present invention makes each group by limiting the ingredient of alloy and its per distribution ratio of each component Divide comprehensive function, significantly improves the comprehensive performance of Cu-Ni-Si alloy materials, make the tensile strength of finished product Cu-Ni-Si alloys More than >=560MPa, conductivity >=67%IACS, elongation percentage >=10%, microhardness >=180HV, pull-off force >=49kN can be preferably Meet requirement of the electronic package material to Cu-Ni-Si alloy properties.
(2)The present invention has abandoned conventional all materials mixed smelting and has carried out Cu-Ni-Si alloy preparations in preparation process Method, and unique previously prepared copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy has been selected to match as melting Material, adds pure silicon, silver powder and Cr2O3Powder, PbO powder carry out the mode of operation of melting, can effectively reduce the easy oxygen such as magnesium, cobalt The scaling loss amount for changing element accurately controls conducive to alloying component realization, keeps ingredient uniform, internal no significant defect.Meanwhile Cr2O3 Powder, PbO powder be added can also significant refining alloy crystal grain, improve the abrasion resistance properties of alloy.
(3), the present invention pass through limit alloy ingredient and its each component quality proportioning, silicon:Nickel+cobalt is 1:5~1:4, Nickel:Cobalt is 1:1.Pass through continuous up-casting, continuously extruded, solution treatment, drawing deformation, the techniques such as drawing deformation and ageing treatment behaviour Make, make final alloy tensile strength be more than >=560MPa, conductivity >=67%IACS, elongation percentage >=10%, microhardness >= 180HV, pull-off force >=49kN can preferably meet requirement of the electronic package material to Cu-Ni-Si alloy properties.
Specific implementation mode
Only invention is further described in detail for following embodiments, but does not constitute any limitation of the invention.
A kind of high-wearing feature Cu-Ni-Si alloy electronic package materials, consist of the following components in percentage by weight:0.2~ 1.5% nickel, 0.1~0.6% silicon, 0.1 ~ 0.3% magnesium, 0.1~0.3% silver, 0.2~1.5% cobalt, 0.1~0.5% Cr2O3, 0.1~0.4% PbO, surplus is copper and inevitable impurity element.In alloy, the total weight and silicon of nickel and cobalt Weight proportion is(4~5):1, and nickel is identical with the weight of cobalt.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 90 DEG C of ingot mould is molded Ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 110 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:It matches, is weighed respectively in copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel according to above-mentioned weight percent Between alloy, pure silicon, silver powder and Cr2O3Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, vacuumize Pressure is 5 × 10 in stove-2Pa, it is 45kPa to be then charged with argon gas and protect to pressure in stove;Smelting technology is controlled at 1230 ~1280 DEG C, casting temperature is controlled at 1180~1250 DEG C;Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtain bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 5~10:1, rotating speed is 2 ~ 3r/min, squeezes temperature and is not less than 820 DEG C;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, control temperature 870~ 920 DEG C, 1~2h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, and deflection is 40~ 80%;The deformed alloy of pre- cold rolling is subjected to the lower ageing treatment of argon gas protection, control temperature at 400~550 DEG C, keep the temperature 1~ 4h;Secondary cold-rolling deformation is carried out later, and deflection is 20~80% to get finished product Cu-Ni-Si alloy electronic package materials.
Embodiment 1
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:0.2% Nickel, 0.1% silicon, 0.1% magnesium, 0.1% silver, 0.2% cobalt, 0.1% Cr2O3, 0.1% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 80 DEG C of ingot mould at Type ingot casting obtains copper magnesium intermediate alloy after natural cooling, spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1230 DEG C, casting temperature is controlled at 1180 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 5:1, rotating speed 3r/min, it is 820 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 870 DEG C, 1h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling::By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 40%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 1h at 400 DEG C;It carries out later Secondary cold-rolling deforms, and deflection is 20% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 2
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:0.4% Nickel, 0.2% silicon, 0.1% magnesium, 0.1% silver, 0.4% cobalt, 0.1% Cr2O3, 0.1% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 120 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1240 DEG C, casting temperature is controlled at 1190 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtained bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 6:1, rotating speed 3r/min, it is 820 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 880 DEG C, 1.5h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 50%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 1.5h at 420 DEG C;It is laggard Row secondary cold-rolling deforms, and deflection is 30% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 3
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:0.5% Nickel, 0.2% silicon, 0.1% magnesium, 0.2% silver, 0.5% cobalt, 0.3% Cr2O3, 0.2% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1250 DEG C, casting temperature is controlled at 1200 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 7:1, rotating speed 3r/min, it is 840 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 890 DEG C, 1.5h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 50%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 1.5h at 450 DEG C;It is laggard Row secondary cold-rolling deforms, and deflection is 40% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 4
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:0.6% Nickel, 0.3% silicon, 0.3% magnesium, 0.2% silver, 0.6% cobalt, 0.5% Cr2O3, 0.4% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1250 DEG C, casting temperature is controlled at 1210 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 8:1, rotating speed 3r/min, it is 830 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 900 DEG C, 2h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 60%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 2h at 480 DEG C;It carries out later Secondary cold-rolling deforms, and deflection is 50% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 5
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:0.8% Nickel, 0.4% silicon, 0.3% magnesium, 0.3% silver, 0.8% cobalt, 0.5% Cr2O3, 0.4% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1280 DEG C, casting temperature is controlled at 1250 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 10:1, rotating speed 2r/min, it is 860 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 920 DEG C, 2h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 80%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 3h at 550 DEG C;It carries out later Secondary cold-rolling deforms, and deflection is 50% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 6
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:1.5% Nickel, 0.6% silicon, 0.3% magnesium, 0.3% silver, 1.5% cobalt, 0.4% Cr2O3, 0.3% PbO, surplus is copper and can not keep away The impurity element exempted from.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1260 DEG C, casting temperature is controlled at 1230 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 9:1, rotating speed 2r/min, it is 860 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 920 DEG C, 1.5h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 60%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 4h at 520 DEG C;It carries out later Secondary cold-rolling deforms, and deflection is 80% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
Embodiment 7
A kind of Cu-Ni-Si alloy electronic package materials of high-wearing feature, consist of the following components in percentage by weight:1.0% Nickel, 0.4% silicon, the magnesium of .3%, 0.3% silver, 1.0% cobalt, 0.3% Cr2O3, 0.4% PbO, surplus is for copper and unavoidably Impurity element.
A kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials, includes the following steps:
(1)Prepare copper magnesium intermediate alloy:The copper of magnesium and component copper gross mass 40% is put into vacuum non-consumable electrode arc melting Melting is carried out in stove, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, Control in-furnace temperature is increased to 1050 ~ 1100 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to and is preheated in 100 DEG C of ingot mould It is molded ingot casting, copper magnesium intermediate alloy is obtained after natural cooling, it is spare;
(2)Prepare copper cobalt intermediate alloy:The copper of component copper gross mass 20%, cobalt are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1050 ~ 1080 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains copper cobalt intermediate alloy after natural cooling, spare;
(3)Prepare cupro-nickel intermediate alloy:The copper of component copper gross mass 40%, nickel are put into vacuum non-consumable electrode arc melting stove Interior carry out melting, it is 5 × 10 to be evacuated to pressure in stove-2Pa, it is 0.05MPa to be then charged with pressure in argon gas to stove, later, control In-furnace temperature processed is increased to 1080 ~ 1110 DEG C, carries out 0.5 ~ 1h of melting, melt is cast to be preheated in 100 DEG C of ingot mould at Type ingot casting obtains cupro-nickel intermediate alloy after natural cooling, spare;
(4)Continuous up-casting:By copper magnesium intermediate alloy, copper cobalt intermediate alloy, cupro-nickel intermediate alloy, pure silicon, silver powder and Cr2O3 Powder, PbO powder, merging are covered with melting in the vacuum melting furnace crucible of charcoal layer, and it is 5 × 10 to be evacuated to pressure in stove-2Pa, then It is 45kPa to be filled with argon gas and protect to pressure in stove;Controlled at 1260 DEG C, casting temperature is controlled at 1200 DEG C smelting technology; Using trailer system Continuous Up casting bar stock, casting speed is 280 mm/min, obtains bar stock;
(5)It is continuously extruded:By step(4)Obtained bar stock prepares slab by the molding machine of continuous extruder, continuously extruded The extrusion ratio of machine is 8:1, rotating speed 2r/min, it is 850 DEG C to squeeze temperature;
(6)Solution treatment:By step(5)Slab obtained, which is fitted into heat-treatment furnace, carries out solution treatment, and control temperature is 920 DEG C, 1h is kept the temperature, water quenching is then carried out;
(7)Pre- cold rolling-timeliness-cold rolling:By step(6)Alloy after solution treatment carries out pre- cold-rolling deformation, deflection 70%; The deformed alloy of pre- cold rolling is subjected to the ageing treatment under argon gas protection, control temperature keeps the temperature 2h at 500 DEG C;It carries out later Secondary cold-rolling deforms, and deflection is 80% to get finished product Cu-Ni-Si alloy electronic package materials.
To Cu-Ni-Si alloys electronic package material manufactured in the present embodiment carry out tensile strength, conductivity, elongation percentage and The measurement of the alloy properties such as microhardness, result are as shown in table 1 below.
1 primary alloy constituent of the present invention of table and performance(20℃)
Alloying component Tensile strength/MPa Conductivity/IACS% Elongation percentage/% Pull-off force/kN Microhardness/HV
Embodiment 1 560 67 10 49 180
Embodiment 2 571 69 11 50 184
Embodiment 3 579 69 11 51 191
Embodiment 4 588 72 12 56 195
Embodiment 5 602 73 13 58 198
Embodiment 6 608 76 13 54 206
Embodiment 7 598 71 12 52 197

Claims (7)

1. a kind of high-wearing feature Cu-Ni-Si alloy electronic package materials, it is characterised in that:By following components in percentage by weight It constitutes:0.2~1.5% nickel, 0.1~0.6% silicon, 0.1 ~ 0.3% magnesium, 0.1~0.3% silver, 0.2~1.5% cobalt, 0.1 ~0.5% Cr2O3, 0.1~0.4% PbO, surplus is copper and inevitable impurity element.
2. according to a kind of high-wearing feature Cu-Ni-Si alloy electronic package materials described in claim 1, it is characterised in that:Institute It states in Cu-Ni-Si alloys, the weight proportion of the total weight and silicon of nickel and cobalt is(4~5):1, and nickel is identical with the weight of cobalt.
3. a kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials according to claim 1 or 2, It is characterized in that, includes the following steps:
Step 1: preparing intermediate alloy:
(1)It is matched according to above-mentioned weight percent, copper, magnesium, nickel and cobalt is weighed respectively, later, by the copper weighed according to 4:4:2 ratio Example is divided into three parts, then, by 4:4:2 three parts of copper are mixed with the magnesium, nickel and cobalt weighed respectively, obtain copper magnesium compound, Cupro-nickel mixture and copper cobalt mixture;
(2)By step(1)Copper magnesium compound, cupro-nickel mixture or copper cobalt mixture obtained be placed in pressure be 0.04~ Melting is carried out in the argon gas atmosphere smelting furnace of 0.06Mpa, the molten metal that temperature is 1050~1110 DEG C is made, then, by institute Molten metal casting is obtained in the ingot mould for being preheated to 80~120 DEG C, later, by gained ingot casting cooled to room temperature, obtains copper Magnesium intermediate alloy, cupro-nickel intermediate alloy or copper cobalt intermediate alloy, it is spare;
Step 2: continuous up-casting:It is matched according to above-mentioned weight percent, weighs pure silicon, silver powder, Cr respectively2O3Powder, PbO powder and step Copper magnesium intermediate alloy made from rapid one, cupro-nickel intermediate alloy or the merging of copper cobalt intermediate alloy are covered with the vacuum melting furnace earthenware of charcoal layer Melting is carried out in crucible, obtains liquid alloy, and later, under logical argon gas protective condition, liquid alloy is carried out using trailer system Bar stock is made in Continuous Up casting, spare;
Step 3: continuously extruded:Bar stock made from step 2 is put into continuous extruder, slab is made, it is spare;
Step 4: solution treatment:Slab made from step 3 is placed in heat-treatment furnace, under 870~920 DEG C of temperature conditions, It keeps the temperature 1~2h and carries out solution treatment, then carry out water quenching;
Step 5: pre- cold rolling-timeliness-cold rolling:The pre- cold rolling that deflection is 40~80% is carried out to the slab after step 4 water quenching to become Shape under 400~550 DEG C of temperature conditions, carries out the ageing treatment of 1~4h of heat preservation, followed by second of deflection later For 20~80% cold-rolling deformation to get completed electronic encapsulating material.
4. a kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials according to claim 3, special Sign is:In step 1, the temperature when melting is 1230~1280 DEG C, and it is 5 that pressure in stove is evacuated to before melting ×10-2Pa。
5. a kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials according to claim 3, special Sign is:In step 2, the guard method of the logical argon gas is that pressure is 45kPa, casting in applying argon gas to vacuum melting furnace When temperature be 1180~1250 DEG C.
6. a kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials according to claim 3, special Sign is:In step 2, the casting speed when Continuous Up casting is 280 mm/min.
7. a kind of preparation method of high-wearing feature Cu-Ni-Si alloy electronic package materials according to claim 3, special Sign is:In step 3, the extrusion ratio of the continuous extruder is 5~10:1, rotating speed be 2 ~ 3r/min, squeeze temperature >= 820℃。
CN201810148288.5A 2018-02-13 2018-02-13 A kind of high-wearing feature Cu-Ni-Si alloy electronic package materials and preparation method thereof Pending CN108359835A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397220A (en) * 2013-08-07 2013-11-20 大唐洛阳热电有限责任公司 Highly compression-resistant double-layer copper-alloy contact wire and preparation method thereof
CN106676319A (en) * 2016-11-29 2017-05-17 河南科技大学 High-strength and high-conductivity copper magnesium alloy contact wire and preparing method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397220A (en) * 2013-08-07 2013-11-20 大唐洛阳热电有限责任公司 Highly compression-resistant double-layer copper-alloy contact wire and preparation method thereof
CN106676319A (en) * 2016-11-29 2017-05-17 河南科技大学 High-strength and high-conductivity copper magnesium alloy contact wire and preparing method thereof

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