CN113549785B - Bonding copper-silver alloy wire and preparation method and application thereof - Google Patents
Bonding copper-silver alloy wire and preparation method and application thereof Download PDFInfo
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- CN113549785B CN113549785B CN202110852786.XA CN202110852786A CN113549785B CN 113549785 B CN113549785 B CN 113549785B CN 202110852786 A CN202110852786 A CN 202110852786A CN 113549785 B CN113549785 B CN 113549785B
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- 229910001316 Ag alloy Inorganic materials 0.000 title claims abstract description 80
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052802 copper Inorganic materials 0.000 claims abstract description 34
- 239000010949 copper Substances 0.000 claims abstract description 34
- 229910052709 silver Inorganic materials 0.000 claims abstract description 20
- 239000004332 silver Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims description 100
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 63
- 238000000137 annealing Methods 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 26
- 238000004321 preservation Methods 0.000 claims description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 20
- 230000032683 aging Effects 0.000 claims description 19
- 238000007670 refining Methods 0.000 claims description 19
- 238000005266 casting Methods 0.000 claims description 18
- 238000009749 continuous casting Methods 0.000 claims description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 229910052746 lanthanum Inorganic materials 0.000 claims description 14
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 14
- 229910052727 yttrium Inorganic materials 0.000 claims description 13
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 9
- 238000007872 degassing Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 230000003647 oxidation Effects 0.000 abstract description 12
- 238000007254 oxidation reaction Methods 0.000 abstract description 12
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 229910052723 transition metal Inorganic materials 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 40
- 238000000265 homogenisation Methods 0.000 description 27
- 229910052757 nitrogen Inorganic materials 0.000 description 20
- 238000012360 testing method Methods 0.000 description 13
- 230000006698 induction Effects 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002431 foraging effect Effects 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000005457 ice water Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000035882 stress Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 3
- 230000004584 weight gain Effects 0.000 description 3
- 235000019786 weight gain Nutrition 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/003—Drawing materials of special alloys so far as the composition of the alloy requires or permits special drawing methods or sequences
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/42—Wire connectors; Manufacturing methods related thereto
- H01L24/43—Manufacturing methods
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/42—Wire connectors; Manufacturing methods related thereto
- H01L24/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
- H01L24/45—Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/43—Manufacturing methods
- H01L2224/438—Post-treatment of the connector
- H01L2224/43848—Thermal treatments, e.g. annealing, controlled cooling
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
- H01L2224/45—Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector
- H01L2224/45001—Core members of the connector
- H01L2224/45099—Material
- H01L2224/451—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof
- H01L2224/45138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/45147—Copper (Cu) as principal constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
- H01L2224/45—Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector
- H01L2224/4554—Coating
- H01L2224/45599—Material
- H01L2224/456—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof
- H01L2224/45663—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof the principal constituent melting at a temperature of greater than 1550°C
- H01L2224/4567—Zirconium (Zr) as principal constituent
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Abstract
The invention discloses a bonding copper-silver alloy wire and a preparation method thereof, and application of the bonding copper-silver alloy wire, wherein the bonding copper-silver alloy wire is prepared from a copper-silver alloy, and the copper-silver alloy comprises the following components in percentage by mass: 0.05-5% of silver, 20-199ppm of transition metal element and the balance of copper; copper is used as a main raw material, silver is used as an auxiliary material, and a transition metal element is used for modification, so that crystal grains are refined, the compactness of the alloy is enhanced, and the oxidation resistance is improved.
Description
Technical Field
The invention belongs to the field of semiconductor packaging, and particularly relates to a bonded copper-silver alloy wire and a preparation method and application thereof.
Background
In the field of semiconductor packaging, wire bonding is an important process, and is an important technique for connecting a chip and an external lead. The integration is directly influenced by the quality of the bonding effect, along with the development of microelectronic packaging technology, the semiconductor chip gradually develops towards high integration and miniaturization, the requirements on signal transmission density and safety and reliability are higher and higher, and higher requirements such as high conductivity, high elongation, thinner wire diameter and the like are also provided for the comprehensive performance of the bonding material.
The bonding lead mainly comprises a bonding alloy wire, a bonding silver wire, a bonding copper wire, a bonding aluminum wire and a series of products formed by micro-alloying, compounding, surface treatment and other measures on the basis of the bonding alloy wire, the bonding silver wire, the bonding copper wire and the bonding aluminum wire, wherein the copper wire has obvious advantages compared with the gold wire, the adoption of copper wire bonding can greatly reduce the manufacturing cost of a device and improve the competitive advantage, and the excellent material performance of the copper bonding wire accelerates the application in the electronic packaging industry.
Although the bonded copper wire has the advantages, the bonded copper wire also has some more significant disadvantages: (1) easy oxidation: the copper surface is easily oxidized at room temperature, so that the requirements of the copper wire on production and use conditions are extremely strict;
(2) the strength is low: the existing copper material has low tensile strength and high wire breakage rate in the production process, is difficult to process into a bonding lead with a smaller size, and cannot meet the requirements of high speed, high density and laminated packaging;
(3) poor heat resistance: the recrystallization temperature of the existing bonded copper wire is about 200 ℃. The larger grain size of the wire fuse balls, the longer the Heat Affected Zone (HAZ), and the increased risk of wire fracture failure during power cycling, i.e., reduced chip reliability.
Disclosure of Invention
In view of the above problems of the conventional bonded copper wire, the present invention provides a bonded copper-silver alloy wire.
The invention adopts the following technical scheme: a bonding copper-silver alloy wire is prepared from a copper-silver alloy, wherein the copper-silver alloy comprises the following components in percentage by mass: 0.05 to 5 percent of silver, 20 to 199ppm of transition metal element and the balance of copper.
Further defined, the transition metal element comprises the following components in percentage by mass: 10-99ppm of zirconium, 5-50ppm of lanthanum and 5-50ppm of yttrium.
Further limiting, the purities of the copper and the silver are respectively more than or equal to 99.999wt%, the purities of the zirconium are respectively more than or equal to 99.99wt%, and the purities of the lanthanum and the yttrium are respectively more than or equal to 99.95 wt%.
Further limited, the silver alloy is prepared from a copper-silver alloy, and the copper-silver alloy comprises the following components in percentage by mass: silver 1.0%, zirconium 30ppm, lanthanum 10ppm, zirconium 5ppm, and the balance copper.
The invention has the beneficial effects that: copper is used as a main raw material, silver is used as an auxiliary material, and a transition metal element is used for modification, so that crystal grains are refined, the compactness of the alloy is enhanced, and the oxidation resistance is improved.
The invention also provides a preparation method of the bonding copper-silver alloy wire, which comprises the following steps:
preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium, heating and melting under a vacuum condition, refining at 1300 ℃ for 25-40min under 1200-;
continuous casting: heating and melting the copper alloy cast ingot in an oxygen-free environment of 1.5-3kPa, and continuously casting the copper alloy cast ingot into a copper alloy bar with the diameter of 8.9-9.1mm after heat preservation, refining and degassing;
homogenizing heat treatment and aging heat treatment: heating the copper alloy bar to 700-800 ℃ at the heating rate of 12-17 ℃/min in an oxygen-free environment, preserving heat for 2-4h, cooling to 400-550 ℃ at the cooling rate of 8-15 ℃/min, preserving heat for 5-15h, and cooling to room temperature;
drawing and processing: repeatedly drawing the cooled copper alloy bar for multiple times to obtain a bonding copper-silver alloy wire with the diameter of 10-50 mu m;
and annealing the bonding copper-silver alloy wire in the inert gas atmosphere to obtain the bonding copper-silver alloy wire.
Further limiting, the annealing speed in the annealing treatment process is 1-3 m/s.
Further limiting, the annealing temperature in the annealing treatment process is 400-600 ℃, and the flow rate of the inert gas in the annealing treatment process is 2-10L/min.
Further limiting, in the homogenizing heat treatment and aging heat treatment processes, 5N nitrogen is adopted to keep an anaerobic environment, and the flow rate of the nitrogen is 3-5L/min;
the temperature during refining is 1250 ℃, the temperature of casting liquid during casting into ingots is 1050 ℃, the heating rate is 15 ℃/min, and the cooling rate is 10 ℃/min.
The invention has the beneficial effects that: the homogenization heat treatment and the aging heat treatment are added to the traditional process, so that the uniformity of the bonding copper-silver alloy wire is improved, and the uncontrollable performance of the bonding copper-silver alloy wire caused by harmful segregation is prevented; and the copper alloy ingot preparation, the continuous casting, the homogenization heat treatment and the aging heat treatment are all carried out under the vacuum condition and heat preservation refining is adopted in the continuous casting, so as to prevent the oxidation and the air hole inclusion of the metal.
By the preparation method, the prepared bonding copper-silver alloy wire has the following advantages:
(1) the strength is high: through the homogenization heat treatment and the aging heat treatment, silver is evenly precipitated in the copper matrix, and in the drawing process, the silver is gradually fiberized, so that the tensile strength of the bonding copper-silver alloy wire can reach more than 500MPa, the processing performance is better, the minimum diameter of the bonding copper-silver alloy wire can reach 10 mu m, the welding wire spacing is favorably shortened, and the method is more suitable for high-speed, high-density and laminated chip packaging.
(2) The oxidation resistance and the vulcanization performance are enhanced. By adding trace rare earth elements, a compact layer of 5-30nm is formed on the surface of the copper alloy, so that the corrosion resistance of elements such as O, S and the like can be effectively enhanced; the operation or processing conditions are wide, and the processing cost is reduced;
(3) the heat resistance is good. Compared with the common bonding copper wire, the recrystallization temperature is increased by 100-220 ℃, the heat affected zone is shorter, the cold and heat impact resistance is stronger, and the poor reliability of the package is greatly improved.
(4) High conductivity. The silver and the transition elements are distributed in a fibrous shape along the processing direction, so that the intensity of the bonding copper-silver alloy wire is improved, the blocking effect on current is reduced, the conductivity is better, and the bonding copper-silver alloy wire is more suitable for packaging semiconductors (such as high-power chips).
Drawings
FIG. 1 is a graph showing the results of a tensile test conducted on a bonded CuAg alloy wire obtained in examples 1 to 6 and a pure copper wire of a comparative example;
fig. 2 is a graph showing the results of an oxidation weight increase test performed on the bonded copper-silver alloy wires prepared in examples 1 to 6 and on the pure copper wires of comparative examples.
Detailed Description
In the following examples, "oxygen-free atmosphere" means an oxygen content of < 5ppm, and the oxygen-free atmosphere may be an atmosphere formed by continuously introducing 5N inert gas.
Example 1
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 0.05% of Ag, 10ppm of Zr, 5ppm of La, 5ppm of Y and the balance of copper;
the preparation method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, and vacuumizing to 10 DEG-2Pa, medium-frequency induction heating to raise temperature and melt, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots, and preparing copper alloy cast ingots.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the flow of nitrogen to be 3-5L/min, setting an automatic temperature-raising program, and performing homogenization heat treatment and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 750 ℃, the heat preservation time is 2h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 10h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper-silver alloy wire with the diameter of 15 mu m.
And S5 annealing the bonded copper-silver alloy wire: and annealing the copper-silver alloy wire in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature range is 400 ℃, and the annealing speed is 2 m/s.
Example 2
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 1.0% of Ag, 30ppm of Zr, 10ppm of La, 5ppm of Y and the balance of copper.
The manufacturing method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: push buttonUniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, and vacuumizing to 10 DEG-2Pa, medium-frequency induction heating to raise temperature and melt, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots, and preparing copper alloy cast ingots.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the flow of nitrogen to be 3-5L/min, setting an automatic temperature-raising program, and performing homogenization heat treatment and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 750 ℃, the heat preservation time is 3h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 9h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper-silver alloy wire with the diameter of 15 mu m.
And S5 annealing of the bonded copper-silver alloy wire: and annealing the bonding copper-silver alloy wire material in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature is 500 ℃, and the annealing speed is 2 m/s.
Example 3
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 2.0% of Ag, 50ppm of Zr, 5ppm of La, 10ppm of Y and the balance of copper.
The manufacturing method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, and vacuumizing to 10 DEG-2Pa, medium frequency induction heating to raise temperature and melt, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots,and (5) preparing a copper alloy ingot.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the flow of nitrogen to be 3-5L/min, setting an automatic temperature-raising program, and performing homogenization heat treatment and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 750 ℃, the heat preservation time is 3h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 8h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper-silver alloy wire with the diameter of 15 mu m.
And S5 annealing the bonded copper-silver alloy wire: and annealing the bonding copper-silver alloy wire in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature is 600 ℃, and the annealing speed is 2 m/s.
Example 4
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 3.0% of Ag, 50ppm of Zr, 30ppm of La, 10ppm of Y and the balance of copper.
The manufacturing method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, and vacuumizing to 10 DEG-2Pa, medium-frequency induction heating to raise temperature and melt, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots, and preparing copper alloy cast ingots.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the flow of nitrogen to be 3-5L/min, setting an automatic temperature-raising program, and performing homogenization heat treatment and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 700 ℃, the heat preservation time is 5h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 7h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper alloy wire with the diameter of 10 mu m.
And S5 annealing the bonded copper-silver alloy wire: and annealing the bonding copper-silver alloy wire in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature range is 400 ℃, and the annealing speed is 2 m/s.
Example 5
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 4.0% of Ag, 99ppm of Zr, 5ppm of La, 50ppm of Y and the balance of copper.
The manufacturing method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, vacuumizing to 10-2Pa, performing medium-frequency induction heating to heat and melt the mixture, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots, and preparing the copper alloy ingots.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the nitrogen flow to be 3-5L/min, setting an automatic temperature rise program, and carrying out homogenization and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 700 ℃, the heat preservation time is 2h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 6h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper-silver alloy wire with the diameter of 15 mu m.
And S5 annealing the bonded copper-silver alloy wire: and annealing the bonding copper-silver alloy wire in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature range is 500 ℃, and the annealing speed is 2 m/s.
Example 6
The bonding copper-silver alloy wire of the embodiment comprises the following components in percentage by mass: 5.0% of Ag, 99ppm of Zr, 50ppm of La, 5ppm of Y and the balance of copper.
The manufacturing method of the bonding copper-silver alloy wire comprises the following steps:
s1, preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium according to mass percent, putting the mixture into a graphite crucible, and vacuumizing to 10 DEG-2Pa, medium-frequency induction heating to raise temperature and melt, refining at 1250 ℃ for 30min, mechanically stirring for 20min, cooling to 1050 ℃, casting into ingots, and preparing copper alloy cast ingots.
S2 vacuum continuous casting: and (3) placing the copper alloy ingot in a high vacuum continuous casting furnace, vacuumizing, injecting 5N nitrogen, controlling the pressure in the furnace to be 1.5-3kPa, performing medium-frequency induction heating melting, performing heat preservation refining, degassing, and continuously casting into a copper alloy bar with the thickness of 9 +/-0.1 mm.
S3 homogenization heat treatment and aging heat treatment: placing the copper alloy bar in a vacuum heat treatment furnace at room temperature, vacuumizing, injecting 5N nitrogen for protection, controlling the nitrogen flow to be 3-5L/min, setting an automatic temperature rise program, and carrying out homogenization and aging heat treatment on the material. Wherein the heat treatment scheme is as follows: the heating rate is 15 ℃/min, the homogenization heat treatment temperature is 700 ℃, the heat preservation time is 2h, after the homogenization heat treatment is finished, the temperature is slowly reduced to 450 ℃ for aging heat treatment, the cooling rate is 10 ℃/min, the heat preservation time is 5h, after the heat treatment is finished, the copper alloy bar is quickly taken out, and the copper alloy bar is placed in ice water for cooling.
S4 drawing processing: and (3) carrying out multi-pass drawing on the copper alloy bar to obtain the bonding copper-silver alloy wire with the diameter of 15 mu m.
And S5 annealing the bonded copper-silver alloy wire: and annealing the bonding copper-silver alloy wire in a nitrogen atmosphere to eliminate the internal stress generated by processing deformation, wherein the temperature is 600 ℃, and the annealing speed is 2 m/s.
Comparative example
The bonding copper wire is prepared from pure copper on the market.
The performance of the bonding copper-silver alloy wires prepared in examples 1 to 6 and the bonding copper prepared in the comparative example was tested, and the test method and the test results were as follows:
1. tensile test
The difference in mechanical properties between examples 1-6 and the pure copper wire (comparative example) is mainly the difference in tensile strength. Tensile strength conditions corresponding to different processing deformation amounts were measured by using a tensile testing machine (the processing deformation amounts were true strains ln (a0/a), a and a0 are cross-sectional areas of the wire before and after deformation), and the results are shown in fig. 1;
as can be seen from fig. 1, the bonded cu-ag alloy wires prepared in examples 1 to 6 all had tensile strengths exceeding 500MPa when the true strain reached 12, wherein the tensile strength of the bonded cu-ag alloy wire of example 6 reached about 1.6 Gpa; and under the same deformation condition, the tensile strength of the pure copper wire is less than 400 MPa.
2. Oxidation weight gain test
The oxidation resistance of the material was measured by measuring the weight change of the pure copper wire (comparative example) and the bonded copper-silver alloy wires described in examples 1 to 6 before and after the test, respectively, by an oxidation weight increase test. The protocol is shown in (Table 1) and the results are shown in FIG. 2.
TABLE 1
| Testing instrument | Ordinary |
| Test conditions | |
| 40±1℃ | |
| Amount of material used | 15g of wire rod with diameter of 0.5mm |
| Measuring instrument | Precision balance (precision 0.1 mg) |
| Test period | 7*24h |
The bonding copper-silver alloy wire prepared in the embodiment 6 only increases the weight by 0.80g in 7 days of the test, and the oxidation resistance is greatly improved compared with that of 3.57g of a pure copper wire.
As can be seen from fig. 2, the oxidation weight gain of the pure copper wire is obvious in the experimental process, and the weight gain of the bonded copper-silver alloy wire prepared in examples 1 to 6 before and after the experiment is not obvious, so that the oxidation resistance is better.
3. Reliability test
For 7 groups of samples, namely pure copper wires and the bonding copper-silver alloy wires prepared in the embodiments 1 to 6, packaging is carried out in a TQFP packaging mode, the number of leads contained in each chip is 144, and after the packaging, high and low temperature cycle tests (TC tests) are carried out on the chips, and the test results are shown in Table 2.
TABLE 2
| Sample set | Number of cycles tested |
| Pure copper wire | 150 |
| Example 1 | 350 |
| Example 2 | 650 |
| Example 3 | 700 |
| Example 4 | 750 |
| Example 5 | 750 |
| Example 6 | 800 |
As can be seen from table 2, the reliability of the bonded cu-ag alloy wires prepared in examples 1 to 6 is significantly better than that of the pure copper wires, the chips of the pure copper wires used all failed after 150 cycles, while the chips of the bonded cu-ag alloy wires prepared in examples 1 to 6 used all exceeded 350 cycles, and the reliability was much higher than that of the pure copper wires.
Finally, it should be noted that: the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The bonding copper-silver alloy wire is characterized by being prepared from a copper-silver alloy, wherein the copper-silver alloy comprises the following components in percentage by mass: 0.05-5% of silver, 10-99ppm of zirconium, 5-50ppm of lanthanum, 5-50ppm of yttrium and the balance of copper;
the bonding copper-silver alloy wire is prepared by the following steps:
preparing a copper alloy ingot: uniformly mixing copper, silver, zirconium, lanthanum and yttrium, heating and melting under a vacuum condition, refining at 1300 ℃ for 25-40min at 1200-;
continuous casting: heating and melting the copper alloy cast ingot in an oxygen-free environment of 1.5-3kPa, and continuously casting the copper alloy cast ingot into a copper alloy bar with the diameter of 8.9-9.1mm after heat preservation, refining and degassing;
homogenizing heat treatment and aging heat treatment: heating the copper alloy bar to 700-800 ℃ at the heating rate of 12-17 ℃/min in an oxygen-free environment, preserving heat for 2-4h, cooling to 400-550 ℃ at the cooling rate of 8-15 ℃/min, preserving heat for 5-15h, and cooling to room temperature;
drawing and processing: repeatedly drawing the cooled copper alloy bar for multiple times to obtain a bonding copper-silver alloy wire with the diameter of 10-50 mu m;
and annealing the bonding copper-silver alloy wire in the inert gas atmosphere to obtain the bonding copper-silver alloy wire.
2. The bonded copper-silver alloy wire of claim 1, wherein the purity of both copper and silver is greater than or equal to 99.999wt%, the purity of zirconium is greater than or equal to 99.99wt%, and the purity of lanthanum and yttrium is greater than or equal to 99.95 wt%.
3. The bonded copper-silver alloy wire according to claim 1, comprising the copper-silver alloy, wherein the copper-silver alloy comprises the following components in percentage by mass: silver 1.0%, zirconium 30ppm, lanthanum 10ppm, yttrium 5ppm, and the balance copper.
4. The bonded copper-silver alloy wire according to claim 1, wherein the annealing rate during the annealing treatment is 1 to 3 m/s.
5. The bonding copper-silver alloy wire according to claim 4, wherein the annealing temperature during the annealing treatment is 400-600 ℃, and the flow rate of the inert gas during the annealing treatment is 2-10L/min.
6. The bonding copper-silver alloy wire according to claim 4, wherein in the homogenizing heat treatment and aging heat treatment, 5N inert gas is continuously introduced to maintain an oxygen-free environment, and the gas flow is controlled to be 3-5L/min;
the temperature during refining is 1250 ℃, the temperature of casting liquid during casting into ingots is 1050 ℃, the heating rate is 15 ℃/min, and the cooling rate is 10 ℃/min.
7. Use of the bonded copper silver alloy wire according to any one of claims 1 to 6 in the field of semiconductor packaging.
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