CN109881040A - A kind of tin plating alloy wire of bonding containing gold - Google Patents
A kind of tin plating alloy wire of bonding containing gold Download PDFInfo
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- CN109881040A CN109881040A CN201910312110.4A CN201910312110A CN109881040A CN 109881040 A CN109881040 A CN 109881040A CN 201910312110 A CN201910312110 A CN 201910312110A CN 109881040 A CN109881040 A CN 109881040A
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Abstract
The present invention relates to metallic bond plying technical fields, in particular to a kind of tin plating alloy wire of bonding containing gold, the alloy wire includes alloy wire ontology and the tin coating for being wrapped in alloy wire body outer surface, when preparing alloy wire ontology, using copper as matrix, it reasonably joined gold thereto, silver, aluminium, manganese and lanthanum element, and using the alloy wire preparation method of science, make gold, silver, aluminium, manganese and lanthanum element are evenly distributed in Copper substrate, so as to improve the comprehensive performance of Copper substrate, and its nucleation rate is improved by nano silica fume and nitride powder, strengthen its mechanical property；Making alloy wire of the invention not only has higher Fracture Force and elongation, and bonding performance is more preferable, and has lower resistivity, and electric conductivity is more preferably；Meanwhile present invention also improves the tin plating techniques of copper alloy wire, optimize immersion plating tin liquor, with the chemical plating stannum technology of immersion tin technology instead of conventional, make the smooth surface of alloy wire of the invention, coating is uniform, fine and close, almost without flaw.
Description
Technical field
The present invention relates to metallic bond plying technical fields, and in particular to a kind of tin plating alloy wire of bonding containing gold.
Background technique
Bonding line is a kind of using lametta, keeps metal lead wire and substrate pads tight using heat, pressure, ultrasonic energy
Close soldering realizes the information mutual communication of the electric interconnection and chip chamber between chip and substrate, is the common package material of microelectronic field
Material.The bonding line of early stage is mostly made of proof gold, but this bonding line is expensive, at high cost, and to reduce cost, bonding line is gradually
Replaced by various bonding alloy lines, such as fine silver plates gold bonding wire, each Albatra metal bonding line.Copper wire is low, conductive due to price
The advantages such as rate is good, hardness is big make copper alloy bonding line become most widely used bonding line instantly.But existing copper alloy bonding
Line has surface oxidizable mostly, and the problems such as drawing broken string easily occurs in poor mechanical property.Therefore, research and development can satisfy bonding material
The linking copper wire that material various aspects mechanical property can simultaneously provide more preferable surface oxidation-resistant is particularly important.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention proposes a kind of tin plating alloy wire of bonding containing gold, the conjunctions
Gold thread not only has higher Fracture Force and elongation, and bonding performance is more preferable, and has lower resistivity, and electric conductivity is more
It is good.
To achieve the goals above, the technical scheme adopted by the invention is that:
The present invention provides a kind of tin plating alloy wire of bonding containing gold, which includes alloy wire ontology and is wrapped in
The tin coating of the alloy wire body outer surface, the alloy wire ontology are made of the raw material of following weight percent:
Gold 0.5%~1.5%, silver 0.003%~0.009%, aluminium 0.001%~0.005%, nano silica fume 0.1%~
0.8%, nitride powder 0.8%~1.5%, manganese 0.3%~0.5%, lanthanum 0.05%~0.1%, surplus is copper.
Preferably, the tin coating with a thickness of 50~80nm.
Preferably, the purity of the gold, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper is all larger than 99.99%.
The present invention also provides a kind of methods for preparing the above-mentioned tin plating alloy wire of bonding containing gold, and this method includes following step
It is rapid:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper are put into vacuum electric
It in arc furnace, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Pa, being then passed through argon gas thereto makes vacuum electric
Air pressure in arc furnace reaches 0.5~0.8MPa, is then warming up to 800~1000 DEG C with the heating rate of 30~40 DEG C/min, then
1300~1500 DEG C are warming up to the heating rate of 50~60 DEG C/min, 20~30min is kept the temperature, is stirred during heat preservation every 10min
It mixes once, obtains alloying metal liquid, finally but by alloying metal liquid cooling, obtain alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride crucible of vacuum continuous casting equipment, is first risen
For temperature to 300~500 DEG C of 2~3h of heat preservation, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, makes temperature
Degree rise to 800~1000 DEG C after stops vacuumizing, be then passed through in crucible argon gas make in crucible air pressure arrival 0.5~
0.8MPa, and temperature is promoted to 1300~1500 DEG C, alloying metal liquid is obtained after keeping the temperature 20~30min, finally continues to be passed through
Argon gas makes the air pressure in crucible reach 1.0~1.2MPa, and being drawn by way of interval cast to form diameter immediately is 8~12mm
The alloying metal bar of size；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Under 1300~1500 DEG C of annealing temperature anneal 6~12h, under 500~700 DEG C of annealing temperature anneal 10~for 24 hours；
S4, rough system: 6~8h is kept the temperature under the conditions of the alloying metal bar after annealing is first placed in 400~450 DEG C, so
It is drawn into the alloy wire drawing of 3~5mm by wire drawing machine again afterwards；
S5, middle drawing: 4~6h is kept the temperature under the conditions of alloy wire drawing obtained in S4 step is first placed in 500~550 DEG C, so
It is drawn into the alloy wire drawing of 0.8~1.3mm by wire drawing machine again afterwards；
S6, thin drawing: 2~4h is kept the temperature under the conditions of alloy wire drawing obtained in S5 step is first placed in 600~650 DEG C, so
It is drawn into the alloy wire drawing of 0.1~0.3mm by wire drawing machine again afterwards；
S7, fine drawing: keeping the temperature 1~2h under the conditions of alloy wire drawing obtained in S6 step is first placed in 700~750 DEG C,
Then the alloy wire drawing of 0.018~0.030mm is drawn by wire drawing machine again；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
Primary 20~the 30s of sulfuric acid cleaned for being 8%~15% with volume fraction, clean 15 with alcohol-water mixed solution second~
25s, cleans 10~20s with deionized water for the third time, and cleaning is dried in the environment of being placed on 180~200 DEG C；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, is then injected tin plating electrolyte with the speed of 13-15 μ L/min with medical needle tubing and is grown
In tubular mould, by elongate tubular mold after filling, 12~14h is dried in the environment of being placed in 180~200 DEG C, is obtained after drying demoulding
To plating tin alloy wire drawing；
The preparation method of the tin plating electrolyte are as follows: sijna rice flour and Polyethylene Octylphenol Ether are dissolved in quickening liquid in succession
In, make the mass fraction 1.0%~2.0% of sijna rice flour, and make the volume fraction of Polyethylene Octylphenol Ether
15%~20%；
The quickening liquid includes the ingredient of following volumes percentage:
Surfactant 2.0%~3.0%, rosin 2.0%~3.0%, phenol 0.1%~0.3%, surplus are that alcohol is molten
Agent；
S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, and it is tin plating to obtain the bonding containing gold
Alloy wire.
Preferably, the drawing speed of rough system described in S4 step is 350~400m/min.
Preferably, the drawing speed of middle drawing described in S5 step is 250~300m/min.
Preferably, the drawing speed carefully drawn described in S6 step is 150~200m/min.
Preferably, the drawing speed carefully drawn described in S7 step is 70~100m/min.
Preferably, the alcohol-water mixed solution is by dehydrated alcohol and deionized water according to dehydrated alcohol: deionized water=
The volume ratio of 1:2 mixes.
Preferably, the surfactant is by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: virtue
Fragrant acid: succinic acid=1:1:2 volume ratio mixes, and the alcoholic solvent is ethyl alcohol and isopropanol according to ethyl alcohol: isopropanol=
The volume ratio of 1:3 mixes.
Compared with prior art, the beneficial effects of the present invention are:
A kind of tin plating alloy wire of bonding containing gold provided by the invention, it is reasonable thereto to be added using copper as matrix
Gold, silver, aluminium, manganese, lanthanum element and nano silica fume and nitride powder utilize gold using the alloy wire preparation method of science
Belong to the characteristic being made of in fused solution the atomic group of vigorous exercise and hole, gold is made by reasonable casting technique, silver,
Aluminium, manganese, lanthanum element are evenly distributed in Copper substrate, so as to improve the comprehensive performance of Copper substrate.Wherein, golden, silver and aluminium element
(weight percent of gold element is 0.5%~1.5%, and the weight percent of silver element is 0.003%~0.009%, aluminium for addition
The weight percent of element is 0.001%~0.005%) electric property of copper alloy wire can be improved；Manganese and lanthanum element plus
Enter (weight percent of manganese element is 0.3%~0.5%, and the weight percent of lanthanum element is 0.05%~0.1%) to enhance
The inoxidizability of copper alloy wire avoids copper alloy that the difficulty of violent oxidation and enlarged surface cleaning occurs in casting process
Degree；In addition, the formation of crystal grain includes heterogeneous forming core and two processes of growing up, nano silica fume in the process of setting of copper alloy
Addition with nitride powder can serve as the core of heterogeneous forming core in the forming process of crystal grain, improve nucleation rate, refinement
Crystal grain, so that the mechanical property to copper alloy plays invigoration effect；It is found by the test of mechanical property and electric property, and it is normal
The preparation method of rule copper alloy wire is compared, and alloy wire of the invention not only has higher Fracture Force and elongation, bonding performance
More preferably, and there is lower resistivity, electric conductivity is more preferably.
In addition, immersion plating tin liquor is optimized present invention also improves the tin plating technique of copper alloy wire, with the replacement of immersion tin technology
Conventional chemical plating stannum technology, makes the smooth surface of alloy wire of the invention, coating uniformly, it is fine and close, almost without flaw,
Better than the effect of chemical plating stannum, to not only ensure that alloy wire has preferable inoxidizability, corrosion resistance and shielding (anti-
Interference), and coating uniformly, fine and close is also beneficial to reduce the resistivity of alloy wire, improves its electric conductivity.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1:
A kind of tin plating alloy wire of bonding containing gold is present embodiments provided, which includes alloy wire ontology and package
In the tin coating of alloy wire body outer surface, wherein tin coating with a thickness of 50nm, alloy wire ontology is by following weight percent
Raw material be made:
Gold 0.5%, silver 0.003%, aluminium 0.001%, nano silica fume 0.1%, nitride powder (average grain diameter 20nm)
0.8%, manganese 0.3%, lanthanum 0.05%, surplus is copper.
The purity of gold in above-mentioned formula, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper is required to be greater than
99.99%.
At the same time, the present embodiment additionally provides a kind of method for preparing the above-mentioned tin plating alloy wire of bonding containing gold, the party
Method the following steps are included:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper are put into K-DHM-
It in 600 type vacuum arc furnace ignitions, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Then Pa is passed through thereto
Argon gas makes the air pressure in vacuum arc furnace ignition reach 0.5MPa, is then warming up to 800 DEG C with the heating rate of 30 DEG C/min, then with 50
DEG C/heating rate of min is warming up to 1300 DEG C, keeps the temperature 20min, and it is primary every 10min stirring with boron nitride stick during heat preservation, it obtains
To alloying metal liquid, finally alloying metal liquid is placed under subzero 30 DEG C of environment and carries out cooling treatment, obtains alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride earthenware of CXM-CVV type vacuum continuous casting equipment
In crucible, 300 DEG C of heat preservation 3h are first warming up to, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, makes temperature
Degree stops vacuumizing after rising to 800 DEG C, and argon gas is then passed through in crucible makes air pressure arrival 0.5MPa in crucible, and by temperature
It is promoted to 1300 DEG C, obtains alloying metal liquid after keeping the temperature 30min, finally continuing to be passed through argon gas reaches the air pressure in crucible
1.0MPa draws the alloy to form that diameter is 8mm size by vacuum continuous casting equipment in the way of interval cast immediately
Metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Anneal 6h under 1500 DEG C of annealing temperature, and anneal 10h under 700 DEG C of annealing temperature；
S4, rough system: first the alloying metal bar after annealing is placed under the conditions of 450 DEG C and keeps the temperature 6h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 3mm with the drawing speed of 350m/min；
S5, middle drawing: first alloy wire drawing obtained in S4 step is placed under the conditions of 550 DEG C and keeps the temperature 4h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.8mm with the drawing speed of 250m/min；
S6, thin drawing: first alloy wire drawing obtained in S5 step is placed under the conditions of 650 DEG C and keeps the temperature 2h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.1mm with the drawing speed of 150m/min；
S7, fine drawing: first alloy wire drawing obtained in S6 step is placed under the conditions of 750 DEG C and keeps the temperature 1h, is then led to again
Cross the alloy wire drawing that BF-6WDM type wire drawing machine is drawn into 0.018mm with the drawing speed of 70m/min；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
The primary sulfuric acid cleaned 30s for being 8% with volume fraction, second with alcohol-water mixed solution (by dehydrated alcohol and deionized water
According to dehydrated alcohol: deionized water=1:2 volume ratio mixes) cleaning 15s, cleans 10s with deionized water for the third time, clearly
It washes in the environment of being placed on 180 DEG C and dries, the alloy wire drawing surface scale cleaning after drying is thorough, corrosion-free phenomenon；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 13 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 14h is dried in the environment of being placed in 180 DEG C, obtains plating tin alloy drawing after drying demoulding
Silk；
Wherein, the preparation method of tin plating electrolyte are as follows: by sijna rice flour (fineness 50nm, purity 99.9) and sim alkylphenol polyoxy second
Alkene ether is dissolved in quickening liquid in succession, makes the mass fraction 1.0% of sijna rice flour, and makes Polyethylene Octylphenol Ether
Volume fraction is 15%；Immersion plating liquid needs first to shake 10min with vibrator before use；
Quickening liquid then includes the ingredient of following volumes percentage:
Surfactant is (by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: fourth two
Acid=1:1:2 volume ratio mixes) 2.0%, rosin 2.0%, phenol 0.1%, surplus is alcoholic solvent (ethyl alcohol and isopropanol
According to ethyl alcohol: isopropanol=1:1 volume ratio mixes)；
The cleaning of this step mold is most important, thus need before tin plating it is first with clear water that elongate tubular mold clean is clean,
After cleaning, ultramicroscopic observation need to be used, it is ensured that it is got lodged in die hole without remaining spot, in order to avoid influence thickness and the plating of coating
Film quality.
S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, cooperation packing box, desiccant into
Row packaging, obtains the tin plating alloy wire of bonding containing gold.
Embodiment 2:
A kind of tin plating alloy wire of bonding containing gold is present embodiments provided, which includes alloy wire ontology and package
In the tin coating of alloy wire body outer surface, wherein tin coating with a thickness of 65nm, alloy wire ontology is by following weight percent
Raw material be made:
Gold 1.2%, silver 0.006%, aluminium 0.0025%, nano silica fume 0.5%, nitride powder (average grain diameter 20nm)
1.2%, manganese 0.4%, lanthanum 0.08%, surplus is copper.
The purity of gold in above-mentioned formula, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper is required to be greater than
99.99%.
At the same time, the present embodiment additionally provides a kind of method for preparing the above-mentioned tin plating alloy wire of bonding containing gold, the party
Method the following steps are included:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper are put into K-DHM-
It in 600 type vacuum arc furnace ignitions, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Then Pa is passed through thereto
Argon gas makes the air pressure in vacuum arc furnace ignition reach 0.65MPa, is then warming up to 900 DEG C with the heating rate of 35 DEG C/min, then with
The heating rate of 55 DEG C/min is warming up to 1400 DEG C, keeps the temperature 25min, primary every 10min stirring with boron nitride stick during heat preservation,
Alloying metal liquid is obtained, finally alloying metal liquid is placed under subzero 30 DEG C of environment and carries out cooling treatment, obtains alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride earthenware of CXM-CVV type vacuum continuous casting equipment
In crucible, 400 DEG C of heat preservation 2.5h are first warming up to, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, make
Temperature stops vacuumizing after rising to 900 DEG C, and argon gas is then passed through in crucible makes the air pressure in crucible reach 0.65MPa, and will
Temperature is promoted to 1400 DEG C, obtains alloying metal liquid after keeping the temperature 25min, and finally continuing to be passed through argon gas reaches the air pressure in crucible
1.1MPa draws the alloy to form that diameter is 10mm size by vacuum continuous casting equipment in the way of interval cast immediately
Metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Anneal 8h under 1400 DEG C of annealing temperature, and anneal 18h under 600 DEG C of annealing temperature；
S4, rough system: first the alloying metal bar after annealing is placed under the conditions of 400 DEG C and keeps the temperature 8h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 4mm with the drawing speed of 380m/min；
S5, middle drawing: first alloy wire drawing obtained in S4 step is placed under the conditions of 500 DEG C and keeps the temperature 6h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 1.0mm with the drawing speed of 280m/min；
S6, thin drawing: first alloy wire drawing obtained in S5 step is placed under the conditions of 600 DEG C and keeps the temperature 4h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.2mm with the drawing speed of 180m/min；
S7, fine drawing: first alloy wire drawing obtained in S6 step is placed under the conditions of 700 DEG C and keeps the temperature 2h, is then led to again
Cross the alloy wire drawing that BF-6WDM type wire drawing machine is drawn into 0.025mm with the drawing speed of 85m/min；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
The primary sulfuric acid cleaned 25s for being 12% with volume fraction, second with alcohol-water mixed solution (by dehydrated alcohol and deionization
Water is according to dehydrated alcohol: deionized water=1:2 volume ratio mixes) cleaning 20s, 15s is cleaned with deionized water for the third time,
Cleaning is dried in the environment of being placed on 190 DEG C, and the alloy wire drawing surface scale cleaning after drying is thorough, corrosion-free phenomenon；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 14 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 13h is dried in the environment of being placed in 190 DEG C, obtains plating tin alloy drawing after drying demoulding
Silk；
Wherein, the preparation method of tin plating electrolyte are as follows: by sijna rice flour (fineness 50nm, purity 99.9) and sim alkylphenol polyoxy second
Alkene ether is dissolved in quickening liquid in succession, makes the mass fraction 1.5% of sijna rice flour, and makes Polyethylene Octylphenol Ether
Volume fraction is 18%；Immersion plating liquid needs first to shake 10min with vibrator before use；
Quickening liquid then includes the ingredient of following volumes percentage:
Surfactant is (by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: fourth two
Acid=1:1:2 volume ratio mixes) 2.5%, rosin 2.5%, phenol 0.2%, surplus is alcoholic solvent (ethyl alcohol and isopropanol
According to ethyl alcohol: isopropanol=1:1 volume ratio mixes)；
The cleaning of this step mold is most important, thus need before tin plating it is first with clear water that elongate tubular mold clean is clean,
After cleaning, ultramicroscopic observation need to be used, it is ensured that it is got lodged in die hole without remaining spot, in order to avoid influence thickness and the plating of coating
Film quality.
S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, cooperation packing box, desiccant into
Row packaging, obtains the tin plating alloy wire of bonding containing gold.
Embodiment 3:
A kind of tin plating alloy wire of bonding containing gold is present embodiments provided, which includes alloy wire ontology and package
In the tin coating of alloy wire body outer surface, wherein tin coating with a thickness of 80nm, alloy wire ontology is by following weight percent
Raw material be made:
Gold 1.5%, silver 0.009%~0.009%, aluminium 0.005%, nano silica fume 0.8%, nitride powder (average grain
Diameter 20nm) 1.5%, manganese 0.5%, lanthanum 0.1%, surplus is copper.
The purity of gold in above-mentioned formula, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper is required to be greater than
99.99%.
At the same time, the present embodiment additionally provides a kind of method for preparing the above-mentioned tin plating alloy wire of bonding containing gold, the party
Method the following steps are included:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper are put into K-DHM-
It in 600 type vacuum arc furnace ignitions, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Then Pa is passed through thereto
Argon gas makes the air pressure in vacuum arc furnace ignition reach 0.8MPa, is then warming up to 1000 DEG C with the heating rate of 40 DEG C/min, then with
The heating rate of 60 DEG C/min is warming up to 1500 DEG C, keeps the temperature 30min, primary every 10min stirring with boron nitride stick during heat preservation,
Alloying metal liquid is obtained, finally alloying metal liquid is placed under subzero 30 DEG C of environment and carries out cooling treatment, obtains alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride earthenware of CXM-CVV type vacuum continuous casting equipment
In crucible, 500 DEG C of heat preservation 2h are first warming up to, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, makes temperature
Degree stops vacuumizing after rising to 1000 DEG C, and argon gas is then passed through in crucible makes the air pressure in crucible reach 0.8MPa, and will be warm
Degree is promoted to 1500 DEG C, obtains alloying metal liquid after keeping the temperature 30min, and finally continuing to be passed through argon gas reaches the air pressure in crucible
1.2MPa draws the alloy to form that diameter is 12mm size by vacuum continuous casting equipment in the way of interval cast immediately
Metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Anneal 12h under 1300 DEG C of annealing temperature, anneals for 24 hours under 500 DEG C of annealing temperature；
S4, rough system: first the alloying metal bar after annealing is placed under the conditions of 450 DEG C and keeps the temperature 7h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 5mm with the drawing speed of 400m/min；
S5, middle drawing: first alloy wire drawing obtained in S4 step is placed under the conditions of 530 DEG C and keeps the temperature 5h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 1.3mm with the drawing speed of 300m/min；
S6, thin drawing: first alloy wire drawing obtained in S5 step is placed under the conditions of 630 DEG C and keeps the temperature 3h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.3mm with the drawing speed of 200m/min；
S7, fine drawing: first alloy wire drawing obtained in S6 step is placed under the conditions of 730 DEG C and keeps the temperature 1.5h, then again
The alloy wire drawing of 0.030mm is drawn into the drawing speed of 100m/min by BF-6WDM type wire drawing machine；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
The primary sulfuric acid cleaned 20s for being 15% with volume fraction, second with alcohol-water mixed solution (by dehydrated alcohol and deionization
Water is according to dehydrated alcohol: deionized water=1:2 volume ratio mixes) cleaning 25s, 20s is cleaned with deionized water for the third time,
Cleaning is dried in the environment of being placed on 200 DEG C, and the alloy wire drawing surface scale cleaning after drying is thorough, corrosion-free phenomenon；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 15 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 12h is dried in the environment of being placed in 200 DEG C, obtains plating tin alloy drawing after drying demoulding
Silk；
Wherein, the preparation method of tin plating electrolyte are as follows: by sijna rice flour (fineness 50nm, purity 99.9) and sim alkylphenol polyoxy second
Alkene ether is dissolved in quickening liquid in succession, makes the mass fraction 2.0% of sijna rice flour, and makes Polyethylene Octylphenol Ether
Volume fraction is 20%；Immersion plating liquid needs first to shake 10min with vibrator before use；
Quickening liquid then includes the ingredient of following volumes percentage:
Surfactant is (by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: fourth two
Acid=1:1:2 volume ratio mixes) 3.0%, rosin 3.0%, phenol 0.3%, surplus is alcoholic solvent (ethyl alcohol and isopropanol
According to ethyl alcohol: isopropanol=1:1 volume ratio mixes)；
The cleaning of this step mold is most important, thus need before tin plating it is first with clear water that elongate tubular mold clean is clean,
After cleaning, ultramicroscopic observation need to be used, it is ensured that it is got lodged in die hole without remaining spot, in order to avoid influence thickness and the plating of coating
Film quality.
S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, cooperation packing box, desiccant into
Row packaging, obtains the tin plating alloy wire of bonding containing gold.
Comparative example:
Comparative example 1~3 is to improve the conventional modification method of copper alloy wire mechanical property and surface oxidation-resistant, using the party
Method draws the copper alloy wire that diameter is 0.018mm, 0.025mm and 0.030mm respectively, specific as follows:
Comparative example 1:
The copper alloy wire includes the ingredient of following weight percent:
Calcium 0.0005%, cerium 0.0003%, antimony 0.0001%, surplus are copper
(1), alloy copper liquid is obtained, most according to melting in above-mentioned mass percent investment melting furnace by copper, calcium, cerium and antimony
Afterwards but by alloyed copper liquid cooling, alloy blank is obtained；
(2), alloy blank is added in melting furnace, is warming up at 730 DEG C and keeps the temperature 20min, is then warming up to 1380 DEG C again
Fusing, obtains alloy copper liquid；
(3), it keeps the temperature: step 2 gained alloy copper liquid is kept the temperature into 15min at 720 DEG C；
(4), continuous casting and rolling is drawn into copper alloy single line at copper alloy bar, wire drawing machine, and control lubrication temperature is not higher than 90 DEG C；
(5), copper alloy single line is sent into 350 DEG C of heat-treatment furnaces by aging strengthening model, handles 4h, is re-fed at 250 DEG C of heat
It manages in furnace, isothermal holding 3h；2h is handled finally, being sent into boiling water；
(6), tin plating: copper alloy single line, which is placed in progress chemical plating stannum processing, the temperature of chemical plating fluid in chemical plating fluid, is
65 DEG C, processing time 15min is dried in the environment of being placed on 150 DEG C；
Wherein, the formula of chemical plating fluid are as follows: stannous methanesulfonate 19g/L, sodium ethylene diamine tetracetate 180g/L, glycerol 9g/
L, suitable quantity of water add a certain amount of sulfuric acid to make the pH value 2 of plating solution.
(7), the bundled rear packaging of copper alloy single line coiling after will be tin plating, obtains the copper alloy wire that diameter is 0.018mm.
Comparative example 2:
The copper alloy wire includes the ingredient of following weight percent:
Calcium 0.0008%, cerium 0.0005%, antimony 0.00015%, surplus are copper
(1), alloy copper liquid is obtained, most according to melting in above-mentioned mass percent investment melting furnace by copper, calcium, cerium and antimony
Afterwards but by alloyed copper liquid cooling, alloy blank is obtained；
(2), alloy blank is added in melting furnace, is warming up at 730 DEG C and keeps the temperature 20min, is then warming up to 1380 DEG C again
Fusing, obtains alloy copper liquid；
(3), it keeps the temperature: step 2 gained alloy copper liquid is kept the temperature into 15min at 720 DEG C；
(4), continuous casting and rolling is drawn into copper alloy single line at copper alloy bar, wire drawing machine, and control lubrication temperature is not higher than 90 DEG C；
(5), copper alloy single line is sent into 350 DEG C of heat-treatment furnaces by aging strengthening model, handles 4h, is re-fed at 250 DEG C of heat
It manages in furnace, isothermal holding 3h；2h is handled finally, being sent into boiling water；
(6), tin plating: copper alloy single line, which is placed in progress chemical plating stannum processing, the temperature of chemical plating fluid in chemical plating fluid, is
65 DEG C, processing time 15min is dried in the environment of being placed on 150 DEG C；
Wherein, the formula of chemical plating fluid are as follows: stannous methanesulfonate 19g/L, sodium ethylene diamine tetracetate 180g/L, glycerol 9g/
L, suitable quantity of water add a certain amount of sulfuric acid to make the pH value 2 of plating solution.
(7), the bundled rear packaging of copper alloy single line coiling after will be tin plating, obtains the copper alloy wire that diameter is 0.025mm.
Comparative example 3:
The copper alloy wire includes the ingredient of following weight percent:
Calcium 0.001%, cerium 0.0007%, antimony 0.0002%, surplus are copper
(1), alloy copper liquid is obtained, most according to melting in above-mentioned mass percent investment melting furnace by copper, calcium, cerium and antimony
Afterwards but by alloyed copper liquid cooling, alloy blank is obtained；
(2), alloy blank is added in melting furnace, is warming up at 730 DEG C and keeps the temperature 20min, is then warming up to 1380 DEG C again
Fusing, obtains alloy copper liquid；
(3), it keeps the temperature: step 2 gained alloy copper liquid is kept the temperature into 15min at 720 DEG C；
(4), continuous casting and rolling is drawn into copper alloy single line at copper alloy bar, wire drawing machine, and control lubrication temperature is not higher than 90 DEG C；
(5), copper alloy single line is sent into 350 DEG C of heat-treatment furnaces by aging strengthening model, handles 4h, is re-fed at 250 DEG C of heat
It manages in furnace, isothermal holding 3h；2h is handled finally, being sent into boiling water；
(6), tin plating: copper alloy single line, which is placed in progress chemical plating stannum processing, the temperature of chemical plating fluid in chemical plating fluid, is
65 DEG C, processing time 15min is dried in the environment of being placed on 150 DEG C；
Wherein, the formula of chemical plating fluid are as follows: stannous methanesulfonate 19g/L, sodium ethylene diamine tetracetate 180g/L, glycerol 9g/
L, suitable quantity of water add a certain amount of sulfuric acid to make the pH value 2 of plating solution.
(7), the bundled rear packaging of copper alloy single line coiling after will be tin plating, obtains the copper alloy wire that diameter is 0.030mm.
Comparative example 4:
Comparative example 4 is the scheme designed according to embodiment 2, compared with Example 2, the alloy wire ontology formula of comparative example 4
In do not add nitride powder, other compositions, additive amount and preparation method are same as Example 2, and concrete scheme is as follows are as follows:
Comparative example 4 provides a kind of tin plating alloy wire of bonding containing gold, which includes alloy wire ontology and be wrapped in
The tin coating of alloy wire body outer surface, wherein tin coating with a thickness of 65nm, alloy wire ontology is by following weight percent
Raw material is made:
Gold 1.2%, silver 0.006%, aluminium 0.0025%, nano silica fume 1.7%, manganese 0.4%, lanthanum 0.08%, surplus is copper.
The purity of gold in above-mentioned formula, silver, aluminium, nano silica fume, manganese, lanthanum and copper is required to be greater than 99.99%.
At the same time, the present embodiment additionally provides a kind of method for preparing the above-mentioned tin plating alloy wire of bonding containing gold, the party
Method the following steps are included:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, manganese, lanthanum and copper are put into K-DHM-600 type vacuum electric
It in arc furnace, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Pa, being then passed through argon gas thereto makes vacuum electric
Air pressure in arc furnace reaches 0.65MPa, is then warming up to 900 DEG C with the heating rate of 35 DEG C/min, then with the liter of 55 DEG C/min
Warm speed is warming up to 1400 DEG C, keeps the temperature 25min, primary every 10min stirring with boron nitride stick during heat preservation, obtains alloying metal
Alloying metal liquid is finally placed under subzero 30 DEG C of environment and carries out cooling treatment, obtains alloy blank by liquid；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride earthenware of CXM-CVV type vacuum continuous casting equipment
In crucible, 400 DEG C of heat preservation 2.5h are first warming up to, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, make
Temperature stops vacuumizing after rising to 900 DEG C, and argon gas is then passed through in crucible makes the air pressure in crucible reach 0.65MPa, and will
Temperature is promoted to 1400 DEG C, obtains alloying metal liquid after keeping the temperature 25min, and finally continuing to be passed through argon gas reaches the air pressure in crucible
1.1MPa draws the alloy to form that diameter is 10mm size by vacuum continuous casting equipment in the way of interval cast immediately
Metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Anneal 8h under 1400 DEG C of annealing temperature, and anneal 18h under 600 DEG C of annealing temperature；
S4, rough system: first the alloying metal bar after annealing is placed under the conditions of 400 DEG C and keeps the temperature 8h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 4mm with the drawing speed of 380m/min；
S5, middle drawing: first alloy wire drawing obtained in S4 step is placed under the conditions of 500 DEG C and keeps the temperature 6h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 1.0mm with the drawing speed of 280m/min；
S6, thin drawing: first alloy wire drawing obtained in S5 step is placed under the conditions of 600 DEG C and keeps the temperature 4h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.2mm with the drawing speed of 180m/min；
S7, fine drawing: first alloy wire drawing obtained in S6 step is placed under the conditions of 700 DEG C and keeps the temperature 2h, is then led to again
Cross the alloy wire drawing that BF-6WDM type wire drawing machine is drawn into 0.025mm with the drawing speed of 85m/min；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
The primary sulfuric acid cleaned 25s for being 12% with volume fraction, second with alcohol-water mixed solution (by dehydrated alcohol and deionization
Water is according to dehydrated alcohol: deionized water=1:2 volume ratio mixes) cleaning 20s, 15s is cleaned with deionized water for the third time,
Cleaning is dried in the environment of being placed on 190 DEG C, and the alloy wire drawing surface scale cleaning after drying is thorough, corrosion-free phenomenon；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 14 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 13h is dried in the environment of being placed in 190 DEG C, obtains plating tin alloy drawing after drying demoulding
Silk；
Wherein, the preparation method of tin plating electrolyte are as follows: by sijna rice flour (fineness 50nm, purity 99.9) and sim alkylphenol polyoxy second
Alkene ether is dissolved in quickening liquid in succession, makes the mass fraction 1.5% of sijna rice flour, and makes Polyethylene Octylphenol Ether
Volume fraction is 18%；Immersion plating liquid needs first to shake 10min with vibrator before use；
Quickening liquid then includes the ingredient of following volumes percentage:
Surfactant is (by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: fourth two
Acid=1:1:2 volume ratio mixes) 2.5%, rosin 2.5%, phenol 0.2%, surplus is alcoholic solvent (ethyl alcohol and isopropanol
According to ethyl alcohol: isopropanol=1:1 volume ratio mixes)；
The cleaning of this step mold is most important, thus need before tin plating it is first with clear water that elongate tubular mold clean is clean,
After cleaning, ultramicroscopic observation need to be used, it is ensured that it is got lodged in die hole without remaining spot, in order to avoid influence thickness and the plating of coating
Film quality.S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, cooperation packing box, desiccant into
Row packaging, obtains the tin plating alloy wire of bonding containing gold.
Comparative example 5:
Comparative example 5 is the scheme designed according to embodiment 2, compared with Example 2, the alloy wire ontology formula of comparative example 5
In do not add nano silica fume, other compositions, additive amount and preparation method are same as Example 2, and concrete scheme is as follows are as follows:
Comparative example 5 provides a kind of tin plating alloy wire of bonding containing gold, which includes alloy wire ontology and be wrapped in
The tin coating of alloy wire body outer surface, wherein tin coating with a thickness of 65nm, alloy wire ontology is by following weight percent
Raw material is made:
Gold 1.2%, silver 0.006%, aluminium 0.0025%, nitride powder (average grain diameter 20nm) 1.7%, manganese 0.4%, lanthanum
0.08%, surplus is copper.
The purity of gold in above-mentioned formula, silver, aluminium, nitride powder, manganese, lanthanum and copper is required to be greater than 99.99%.
At the same time, the present embodiment additionally provides a kind of method for preparing the above-mentioned tin plating alloy wire of bonding containing gold, the party
Method the following steps are included:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nitride powder, manganese, lanthanum and copper are put into K-DHM-600 type vacuum
It in electric arc furnaces, first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Pa, being then passed through argon gas thereto makes vacuum
Air pressure in electric arc furnaces reaches 0.65MPa, is then warming up to 900 DEG C with the heating rate of 35 DEG C/min, then with 55 DEG C/min's
Heating rate is warming up to 1400 DEG C, keeps the temperature 25min, primary every 10min stirring with boron nitride stick during heat preservation, obtains alloy gold
Belong to liquid, finally alloying metal liquid is placed under subzero 30 DEG C of environment and carries out cooling treatment, obtains alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride earthenware of CXM-CVV type vacuum continuous casting equipment
In crucible, 400 DEG C of heat preservation 2.5h are first warming up to, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, make
Temperature stops vacuumizing after rising to 900 DEG C, and argon gas is then passed through in crucible makes the air pressure in crucible reach 0.65MPa, and will
Temperature is promoted to 1400 DEG C, obtains alloying metal liquid after keeping the temperature 25min, and finally continuing to be passed through argon gas reaches the air pressure in crucible
1.1MPa draws the alloy to form that diameter is 10mm size by vacuum continuous casting equipment in the way of interval cast immediately
Metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first
Anneal 8h under 1400 DEG C of annealing temperature, and anneal 18h under 600 DEG C of annealing temperature；
S4, rough system: first the alloying metal bar after annealing is placed under the conditions of 400 DEG C and keeps the temperature 8h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 4mm with the drawing speed of 380m/min；
S5, middle drawing: first alloy wire drawing obtained in S4 step is placed under the conditions of 500 DEG C and keeps the temperature 6h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 1.0mm with the drawing speed of 280m/min；
S6, thin drawing: first alloy wire drawing obtained in S5 step is placed under the conditions of 600 DEG C and keeps the temperature 4h, is then passed through again
BF-6WDM type wire drawing machine is drawn into the alloy wire drawing of 0.2mm with the drawing speed of 180m/min；
S7, fine drawing: first alloy wire drawing obtained in S6 step is placed under the conditions of 700 DEG C and keeps the temperature 2h, is then led to again
Cross the alloy wire drawing that BF-6WDM type wire drawing machine is drawn into 0.025mm with the drawing speed of 85m/min；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, the
The primary sulfuric acid cleaned 25s for being 12% with volume fraction, second with alcohol-water mixed solution (by dehydrated alcohol and deionization
Water is according to dehydrated alcohol: deionized water=1:2 volume ratio mixes) cleaning 20s, 15s is cleaned with deionized water for the third time,
Cleaning is dried in the environment of being placed on 190 DEG C, and the alloy wire drawing surface scale cleaning after drying is thorough, corrosion-free phenomenon；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by after cleaning, drying to
Alloy plating wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 14 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 13h is dried in the environment of being placed in 190 DEG C, obtains plating tin alloy drawing after drying demoulding
Silk；
Wherein, the preparation method of tin plating electrolyte are as follows: by sijna rice flour (fineness 50nm, purity 99.9) and sim alkylphenol polyoxy second
Alkene ether is dissolved in quickening liquid in succession, makes the mass fraction 1.5% of sijna rice flour, and makes Polyethylene Octylphenol Ether
Volume fraction is 18%；Immersion plating liquid needs first to shake 10min with vibrator before use；
Quickening liquid then includes the ingredient of following volumes percentage:
Surfactant is (by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: fourth two
Acid=1:1:2 volume ratio mixes) 2.5%, rosin 2.5%, phenol 0.2%, surplus is alcoholic solvent (ethyl alcohol and isopropanol
According to ethyl alcohol: isopropanol=1:1 volume ratio mixes)；
The cleaning of this step mold is most important, thus need before tin plating it is first with clear water that elongate tubular mold clean is clean,
After cleaning, ultramicroscopic observation need to be used, it is ensured that it is got lodged in die hole without remaining spot, in order to avoid influence thickness and the plating of coating
Film quality.S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, cooperation packing box, desiccant into
Row packaging, obtains the tin plating alloy wire of bonding containing gold.
Performance test:
It in order to verify the technical effects of the present invention, with Examples 1 to 3 and comparative example 1~5 is respectively subjects, to them
Carry out surface topography observation, mechanical property and electrical performance testing:
1, surface topography is observed
It is observed in Examples 1 to 3 and comparative example 1~5 respectively with scanning electron microscope (SEM, S4700, Hitachi, Japan)
The surface topography of alloy wire, as a result, it has been found that, the smooth surface of alloy wire, coating are equal in Examples 1 to 3, comparative example 4~5
It is even, fine and close, almost without flaw；And there is more rough and uneven in surface, the uniformity of coating on the surface of the alloy wire in comparative example 1~3
With compactness than Examples 1 to 3, the difference of comparative example 4~5.As it can be seen that immersion tin technology of the invention is substantially better than chemical plating stannum
Technology.
2, Mechanics Performance Testing:
Since in bonding line bonding process, the operating condition of bonding line is extremely complex, particularly with High-Speed Automatic bonding
Bonding line on machine, it is therefore desirable to which bonding line has higher Fracture Force and elongation.For bonding line, Fracture Force
It plays a crucial role with the quality of elongation percentage para-linkage line bonding, the bonding line with high Fracture Force and elongation percentage is more advantageous to key
It closes.
For the Fracture Force and elongation percentage for understanding the alloy wire in Examples 1 to 3 and comparative example 1~5, to judge their key
Close performance.This test uses YG001B type single fiber electronics strength tester, measures in Examples 1 to 3 and comparative example 1~5 respectively
The Fracture Force and elongation percentage of alloy wire, measurement result are as shown in table 1.
As can be seen from Table 1, Examples 1 to 3, the Fracture Force of alloy wire in comparative example 4~5, elongation are more than pair
Alloy wire in ratio 1~3, mechanical property is more preferable, for bonding line, there is high Fracture Force and elongation to be more advantageous to
Bonding, therefore, the alloy wire in Examples 1 to 3, comparative example 4~5 have more excellent bonding performance, and mechanical property refers to
Mark more meets application demand.
In addition, the Fracture Force and elongation percentage by the alloy wire in embodiment 2 and comparative example 4~5 can be seen that nano-silicon
The common presence of powder and nitride powder plays the role of cooperative reinforcing to the mechanical property of alloy wire, than nano silica fume or nitridation
Better modified effect is played in the exclusive use of titanium valve body, can greatly enhance the mechanical property of alloy wire.
The mechanical property and electrical performance testing result of 1 Examples 1 to 3 of table and the alloy wire in comparative example 1~3
3, electrical performance testing
According to JB/T8134-1997 and JB/T8640-1997 standard, to the alloy in Examples 1 to 3 and comparative example 1~5
The resistive performance of line is tested, and the gauge length of sample should be 1000mm, and test temperature is 20 DEG C.Using QJ-44 type direct current both arms
Electric bridge carries out resistance measurement, and is calculated by the following formula out resistivity, and measurement result is as shown in table 1.
P=RL/S=4RL/ π d2
Wherein, p is the resistivity of alloy wire, and unit is Ω m；R is the resistance of surveyed alloy wire, unit Ω；L is institute
Survey the length of alloy wire, unit m；D is alloy linear diameter, unit m.
As can be seen from Table 1, Examples 1 to 3, the resistivity of alloy wire in comparative example 4~5 are below comparative example 1~3
In alloy wire, electric property is more preferably, it is seen that alloy wire in Examples 1 to 3, comparative example 4~5 has better electric conductivity
Energy.
In addition, can be seen that nano silica fume and nitridation by the resistivity of the alloy wire in embodiment 2 and comparative example 4~5
Titanium valve body, which is used in conjunction with, influences the modified effect of alloy wire electric conductivity with the exclusive use of nano silica fume or nitride powder
Less.
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (10)
1. a kind of tin plating alloy wire of bonding containing gold, it is characterised in that: including alloy wire ontology and be wrapped in the alloy wire
The tin coating of body outer surface, the alloy wire ontology are made of the raw material of following weight percent:
Gold 0.5%~1.5%, silver 0.003%~0.009%, aluminium 0.001%~0.005%, nano silica fume 0.1%~
0.8%, nitride powder 0.8%~1.5%, manganese 0.3%~0.5%, lanthanum 0.05%~0.1%, surplus is copper.
2. a kind of tin plating alloy wire of bonding containing gold according to claim 1, it is characterised in that: the thickness of the tin coating
For 50~80nm.
3. a kind of tin plating alloy wire of bonding containing gold according to claim 1, it is characterised in that: the gold, silver, aluminium are received
The purity of rice silicon powder, nitride powder, manganese, lanthanum and copper is all larger than 99.99%.
4. a kind of method for preparing the bonding tin plating alloy wire described in claim 1 containing gold, it is characterised in that: it includes following
Step:
The preparation of S1, alloy blank: will be golden, silver, aluminium, nano silica fume, nitride powder, manganese, lanthanum and copper are put into vacuum arc furnace ignition
In, it first vacuumizes, the vacuum degree in vacuum arc furnace ignition is made to be greater than 1 × 10-2Pa, being then passed through argon gas thereto makes vacuum arc furnace ignition
Interior air pressure reaches 0.5~0.8MPa, is then warming up to 800~1000 DEG C with the heating rate of 30~40 DEG C/min, then with 50
The heating rate of~60 DEG C/min is warming up to 1300~1500 DEG C, keeps the temperature 20~30min, stirs one every 10min during heat preservation
It is secondary, alloying metal liquid is obtained, finally but by alloying metal liquid cooling, obtains alloy blank；
The preparation of S2, alloying metal bar: alloy blank is put into the boron nitride crucible of vacuum continuous casting equipment, is first warming up to
300~500 DEG C of 2~3h of heat preservation, then vacuumizing makes the vacuum degree in crucible be higher than 3 × 10-2Pa continues to heat up, and makes temperature liter
Stopping vacuumizing after to 800~1000 DEG C, argon gas is then passed through in crucible makes the air pressure in crucible reach 0.5~0.8MPa,
And temperature is promoted to 1300~1500 DEG C, alloying metal liquid is obtained after keeping the temperature 20~30min, finally continuing to be passed through argon gas makes earthenware
Air pressure in crucible reaches 1.0~1.2MPa, draws the conjunction to form that diameter is 8~12mm size by way of interval cast immediately
Golden metallic rod；
S3, annealing: under vacuum conditions making annealing treatment the alloying metal bar being prepared in S2 step, first exists
Under 1300~1500 DEG C of annealing temperature anneal 6~12h, under 500~700 DEG C of annealing temperature anneal 10~for 24 hours；
S4, rough system: 6~8h is kept the temperature under the conditions of the alloying metal bar after annealing is first placed in 400~450 DEG C, then again
The alloy wire drawing of 3~5mm is drawn by wire drawing machine；
S5, middle drawing: 4~6h is kept the temperature under the conditions of alloy wire drawing obtained in S4 step is first placed in 500~550 DEG C, then again
The alloy wire drawing of 0.8~1.3mm is drawn by wire drawing machine；
S6, thin drawing: 2~4h is kept the temperature under the conditions of alloy wire drawing obtained in S5 step is first placed in 600~650 DEG C, then again
The alloy wire drawing of 0.1~0.3mm is drawn by wire drawing machine；
S7, fine drawing: 1~2h is kept the temperature under the conditions of alloy wire drawing obtained in S6 step is first placed in 700~750 DEG C, then
The alloy wire drawing of 0.018~0.030mm is drawn by wire drawing machine again；
S8, surface clean: immediately cleaning alloy wire drawing obtained in S7 step after fine drawing three times, for the first time
20~the 30s of sulfuric acid cleaned for being 8%~15% with volume fraction cleans 15~25s with alcohol-water mixed solution for the second time, the
10~20s is cleaned with deionized water three times, cleaning is dried in the environment of being placed on 180~200 DEG C；
S9, tin plating processing: selecting the elongate tubular mold in suitable aperture according to the thickness of tin coating, by the conjunction to be plated after cleaning, drying
Golden wire drawing is interspersed in elongate tubular mold, and tin plating electrolyte is then injected elongate tubular with the speed of 13-15 μ L/min with medical needle tubing
In mold, by elongate tubular mold after filling, 12~14h is dried in the environment of being placed in 180~200 DEG C, is plated after drying demoulding
Tin alloy wire drawing；
The preparation method of the tin plating electrolyte are as follows: sijna rice flour and Polyethylene Octylphenol Ether are dissolved in quickening liquid in succession,
Make the mass fraction 1.0%~2.0% of sijna rice flour, and make the volume fraction 15% of Polyethylene Octylphenol Ether~
20%；
The quickening liquid includes the ingredient of following volumes percentage:
Surfactant 2.0%~3.0%, rosin 2.0%~3.0%, phenol 0.1%~0.3%, surplus are alcoholic solvent；
S10, packaging: being vacuum-packed after alloy wire drawing coiling after will be tin plating is bundled, obtains the bonding containing gold and plates tin alloy
Line.
5. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: S4 step
Described in rough system drawing speed be 350~400m/min.
6. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: S5 step
Described in middle drawing drawing speed be 250~300m/min.
7. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: S6 step
Described in the drawing speed carefully drawn be 150~200m/min.
8. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: S7 step
Described in the drawing speed carefully drawn be 70~100m/min.
9. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: the second
Alcohol-water mixed solution is by dehydrated alcohol and deionized water according to dehydrated alcohol: deionized water=1:2 volume ratio mixes.
10. a kind of method for preparing the tin plating alloy wire of bonding containing gold according to claim 4, it is characterised in that: described
Surfactant is by aliphatic dibasic acid, aromatic acid and succinic acid according to aliphatic dibasic acid: aromatic acid: succinic acid=1:1:2
Volume ratio mix, the alcoholic solvent is ethyl alcohol and isopropanol according to ethyl alcohol: the mixing of isopropanol=1:3 volume ratio and
At.
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| CN110607468A (en) * | 2019-09-06 | 2019-12-24 | 安徽广宇电子材料有限公司 | Production process method of copper-tin alloy bonding wire |
| CN111440965A (en) * | 2020-04-15 | 2020-07-24 | 深圳市兴鸿泰锡业有限公司 | Antioxidant alloy wire and preparation process thereof |
| CN111440965B (en) * | 2020-04-15 | 2022-01-14 | 深圳市兴鸿泰锡业有限公司 | Antioxidant alloy wire and preparation process thereof |
| CN113088837A (en) * | 2021-04-15 | 2021-07-09 | 江西富鸿金属有限公司 | Medical high-elasticity tinned alloy wire and preparation method thereof |
| CN113118234A (en) * | 2021-04-16 | 2021-07-16 | 江西富鸿金属有限公司 | Production process of tinned alloy wire for medical equipment |
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