CN110699569A - Bonded silver wire material with stably distributed crystal grains and preparation method thereof - Google Patents
Bonded silver wire material with stably distributed crystal grains and preparation method thereof Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 71
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052709 silver Inorganic materials 0.000 claims abstract description 40
- 239000004332 silver Substances 0.000 claims abstract description 40
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052737 gold Inorganic materials 0.000 claims abstract description 16
- 239000010931 gold Substances 0.000 claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000956 alloy Substances 0.000 claims abstract description 14
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 14
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 13
- 239000011651 chromium Substances 0.000 claims abstract description 13
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 239000010949 copper Substances 0.000 claims abstract description 13
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 12
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 11
- 239000011575 calcium Substances 0.000 claims abstract description 11
- 239000011573 trace mineral Substances 0.000 claims abstract description 7
- 235000013619 trace mineral Nutrition 0.000 claims abstract description 7
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052738 indium Inorganic materials 0.000 claims abstract description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 4
- 239000011669 selenium Substances 0.000 claims abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims description 41
- 230000008018 melting Effects 0.000 claims description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- LJCRYLPRAFNGFA-UHFFFAOYSA-N [Au].[Ag].[Cr] Chemical compound [Au].[Ag].[Cr] LJCRYLPRAFNGFA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 230000003064 anti-oxidating effect Effects 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000009749 continuous casting Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- YSFHRHQJDPRCHZ-UHFFFAOYSA-N scandium silver Chemical compound [Sc].[Ag] YSFHRHQJDPRCHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000003575 carbonaceous material Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 150000002739 metals Chemical class 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RZVXOCDCIIFGGH-UHFFFAOYSA-N chromium gold Chemical compound [Cr].[Au] RZVXOCDCIIFGGH-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910021654 trace metal Inorganic materials 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
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- 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
- B21C1/02—Drawing metal wire or like flexible metallic material by drawing machines or apparatus in which the drawing action is effected by drums
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- 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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
- C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
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- 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
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4885—Wire-like parts or pins
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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
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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
- H01L2224/43—Manufacturing methods
- H01L2224/432—Mechanical processes
- H01L2224/4321—Pulling
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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
- H01L2224/43—Manufacturing methods
- H01L2224/438—Post-treatment of the connector
- H01L2224/43848—Thermal treatments, e.g. annealing, controlled cooling
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- H—ELECTRICITY
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- 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
- H01L2224/45139—Silver (Ag) as principal constituent
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Abstract
The invention belongs to the technical field of bonding wire materials, and relates to a bonding silver wire material with stably distributed crystal grains and a preparation method thereof. The material comprises 98% + -0.2% of silver, 0.5% + -0.04% of chromium, 0.5% + -0.03% of gold, 0.45% + -0.04% of scandium, 0.45% + -0.02% of palladium, 0.01% + -0.001% of calcium, 0.01% + -0.004% of lanthanum and 0.01% + -0.001% of copper, and further comprises 0.001% + -0.0001% of other trace elements, wherein the trace elements comprise one or more of indium, cerium, yttrium and selenium; the inside of the material is in a relatively stable and stable crystal grain shape, metal crystal grains can be fully and uniformly distributed in the preparation process, the full coincidence of the crystal grains of all components in the synthesis process of the bonding silver wire material is improved, the crystal grain shape after the synthesis of all metals is optimized, and the chemical stability and the mechanical property of the alloy wire material are improved.
Description
Technical Field
The invention belongs to the technical field of bonding wire materials, and particularly relates to a bonding silver wire material with stably distributed crystal grains and a preparation method thereof.
Background
In recent years, the application of silver in the electronic field is more and more emphasized, and with the development of the semiconductor and electronic industries, the performance requirement on the bonding wire material is higher and higher.
In the current research progress of bonding wire materials, the development of bonding copper wire products is good, although the price of the bonding copper wire products is superior, the problems that the oxidation resistance is poor, the mechanical property is not excellent enough and the like exist, the stability and the working efficiency of used elements are influenced, the production cost and the use cost are increased, the chip is damaged due to high hardness, and the yield is influenced.
The metal silver has the characteristic of excellent conductivity, the resistivity of the metal silver is 1.586 mu omega cm, the metal silver is the smallest in all metals, and the metal silver also has better heat dissipation performance, but the pure silver is easy to oxidize in the atmosphere, when the pure silver is melted into balls, the surfaces of the balls are not smooth, so the service life of the balls is not long, the mechanical properties of the pure silver are poorer, the ductility of the pure silver is poorer, and the like.
Although the existing silver-based bonding wire material has the advantages of good oxidation resistance, mechanical strength and the like, the bonding performance and the use of the bonding wire material are caused by uneven distribution of crystal grains in most materials.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a check silver wire material with stable grain distribution and a preparation method thereof, such that metallic silver is better used for synthesizing a bonding wire material, advantages of metallic silver are fully exerted, gold usage is reduced, cost is reduced, and a bonding silver wire material with excellent bonding performance is synthesized by adding rare metals and trace metal elements.
The invention comprises the following steps:
a bonded silver wire material with stably distributed crystal grains comprises 98% +/-0.2% of silver, 0.5% +/-0.04% of chromium, 0.5% +/-0.03% of gold, 0.45% +/-0.04% of scandium, 0.45% +/-0.02% of palladium, 0.01% +/-0.001% of calcium, 0.01% +/-0.004% of lanthanum and 0.01% +/-0.001% of copper;
the composition of the material also comprises 0.001% +/-0.0001% of other trace elements, wherein the trace elements comprise one or more of indium, cerium, yttrium and selenium;
the interior of the material forms a uniformly distributed and compact metal crystal grain shape, and the size of the crystal grain is 2-10 mu m;
the purity of each component is more than 99%.
The invention also provides a preparation method of the bonded silver wire material with stably distributed crystal grains, which comprises the following steps:
1) pretreatment: respectively cleaning silver, chromium, gold, scandium, palladium, calcium, lanthanum and copper substances by adopting argon gas, grinding into powder, sieving, preheating to 50-60 ℃, carrying out vacuum drying, simultaneously carrying out deoxidization treatment on metal substances by adopting a reducing carbon material,
2) preparing silver gold chromium melt: mixing metal silver, gold and chromium, putting the mixture into a crucible, carrying out vacuum melting, raising the melting temperature to 860-920 ℃ for 10-30 minutes, raising the temperature to 975-1030 ℃ for 10-50 minutes, raising the temperature to 1750-1830 ℃ for 20-60 minutes, wherein the temperature raising speed in the whole process is 110-350 ℃/h, and obtaining a silver-gold-chromium melt after the melting is finished;
3) preparing a silver scandium palladium melt: mixing silver, scandium and palladium, putting the mixture into a crucible, and performing vacuum melting, wherein the initial melting temperature is increased to 860-920 ℃ and maintained for 10-30 minutes, and then increased to 1480-1520 ℃ and maintained for 20-60 minutes, the temperature increase speed in the whole process is 200-350 ℃/h, and the silver, scandium and palladium melt is obtained after melting;
4) continuous casting of bonding bar material: mixing and putting metal calcium, lanthanum, copper, residual silver, gold, chromium melt and silver, scandium and palladium melt into a crucible, carrying out vacuum melting, raising the melting temperature to 800-1000 ℃ for 15-30 minutes, raising the temperature to 1460-1500 ℃ for 20-50 minutes, wherein the temperature rise speed in the whole process is 175-225 ℃/h, and the speed for continuous casting after melting is 25-50 mm/min to form a bonding rod material;
5) drawing: drawing the bonding rod material to obtain a filament, wherein the average deformation of each pass is 10-15%, and an alloy wire material with a preset wire diameter is formed;
6) annealing: annealing the filaments for 3-6 hours at the temperature of 570-620 ℃, wherein the cold machining stress of the alloy filaments can be eliminated by annealing treatment, the size of alloy crystal grains is optimized, the comprehensive performance of the alloy filaments is further improved, the surface of the annealed alloy filaments is coated with mixed alcohol for anti-oxidation treatment, and then the mixed alcohol is subjected to vacuum drying to obtain the bonding silver filaments;
the reduced carbon material in the step 1) comprises carbon monoxide and activated carbon, and can realize oxygen removal treatment in the synthesis process;
the crucible in the steps 2) to 4) is a silicon nitride crucible or a silicon carbide crucible, and the silicon nitride crucible or the silicon carbide crucible can promote the fusion bonding of alloy materials, improve the bonding property and further achieve the effect of oxidation resistance;
the vacuum pressure condition of the vacuum melting is 10-2~10-4Pa, the melting point of the metal material can be reduced by adopting vacuum, the cost is reduced, and the anti-oxidation of the material in the synthesis process is further achieved;
the operations of the steps 2) to 6) are all carried out in a hydrogen-nitrogen environment, the hydrogen-nitrogen is a mixed gas of hydrogen and nitrogen, the content of the hydrogen is more than 3.5% and less than 5%, and good anti-oxidation protection is formed;
and step 5), drawing the wire, wherein the drawing comprises rough drawing, intermediate drawing, fine drawing and fine drawing, the target diameter of the rough drawing is 1-2 mm, the target diameter of the intermediate drawing is 0.5-0.8 mm, the target diameter of the fine drawing is 0.06-0.07 mm, and the target diameter of the fine drawing is 0.01-0.05 mm.
The invention has the following beneficial effects:
compared with the prior art, the bonded silver wire material with stably distributed crystal grains has the advantages that the adopted metallic silver component with higher content is combined with the gold with lower content and other rare elements and trace elements with different proportions, so that the raw material cost is reduced, the uniformly and tightly distributed metallic crystal grain appearance is formed inside the material, the bonded silver wire material with excellent bonding performance is promoted to be formed due to the stable and stable crystal grain appearance, meanwhile, the electronic structure of the metallic chromium is optimized, the conductivity is improved, the chemical performance and the mechanical performance of the metallic scandium can be simultaneously improved, the strength of the material is improved, the shaping of the material is kept, the corrosion resistance is improved, the oxidation resistance, the corrosion resistance and the discoloration resistance of the material are improved due to the addition of the metallic palladium, and the weldability of the bonded material is improved due to the addition of the metallic lanthanum;
the preparation method of the bonding silver wire material with stably distributed crystal grains is mainly characterized in that metal components are separately fused and synthesized step by step, so that the metal crystal grains can be fully and uniformly distributed, the full coincidence of the crystal grains of the components in the synthesis process of the bonding silver wire material is improved, the appearance of the crystal grains after the synthesis of the metals is optimized, the chemical stability, the mechanical property and the like of the alloy wire material are improved, compared with the prior art, the used raw materials are low in cost, the industrial production can be met, and the performance requirements of high-end circuit products such as IC integrated circuits, semiconductor discrete devices, LEDs and the like can be met.
Drawings
FIG. 1 is a grain morphology diagram of a bonded silver wire material of the present invention;
fig. 2 is a crystal grain morphology diagram of a bonding wire material of metal silver, gold and copper.
Detailed Description
The present invention is described in further detail in the following description of specific embodiments and the accompanying drawings, it is to be understood that these embodiments are merely illustrative of the present invention and are not intended to limit the scope of the invention, which is defined by the appended claims, and modifications thereof by those skilled in the art after reading this disclosure that are equivalent to the above described embodiments.
All the raw materials and reagents of the invention are conventional market raw materials and reagents unless otherwise specified.
Example 1
A preparation method of a bonded silver wire material with stably distributed crystal grains comprises the following steps:
1) pretreatment: respectively cleaning silver, chromium, gold, scandium, palladium, calcium, lanthanum and copper substances by adopting argon gas, grinding into powder, sieving, preheating to 50-60 ℃, carrying out vacuum drying, simultaneously carrying out deoxidization treatment on the metal substances by adopting activated carbon,
2) preparing silver gold chromium melt: mixing 20% +/-0.2% of metallic silver, 0.5% +/-0.03% of gold and 0.5% +/-0.04% of chromium, putting the mixture into a silicon carbide crucible, adopting vacuum melting, raising the melting temperature to 860-920 ℃ at the beginning and maintaining the temperature for 10-30 minutes, raising the temperature to 975-1030 ℃ and maintaining the temperature for 10-50 minutes, raising the temperature to 1750-1830 ℃ and maintaining the temperature for 20-60 minutes, wherein the temperature raising speed in the whole process is 110-350 ℃/h, and obtaining a silver-gold-chromium melt after the melting is finished;
3) preparing a silver scandium palladium melt: mixing 20% +/-0.2% of metallic silver, 0.45% +/-0.04% of scandium and 0.45% +/-0.02% of palladium, putting the mixture into a silicon carbide crucible, adopting vacuum melting, raising the melting temperature to 860-920 ℃ at the beginning, maintaining the temperature for 10-30 minutes, raising the temperature to 1480-1520 ℃ and maintaining the temperature for 20-60 minutes, wherein the temperature raising speed in the whole process is 200-350 ℃/h, and completing melting to obtain a silver-scandium-palladium melt;
4) continuous casting of bonding bar material: mixing 0.01% + -0.001% of metallic calcium, 0.01% + -0.004% of lanthanum, 0.01% + -0.001% of copper, 0.001 + -0.0001% of indium and/or cerium, 58% + -0.2% of the rest silver, gold-chromium melt and silver-scandium-palladium melt, putting the mixture into a silicon carbide crucible, carrying out vacuum melting, raising the melting temperature to 800-1000 ℃ and maintaining for 15-30 minutes, raising the temperature to 1460-1500 ℃ and maintaining for 20-50 minutes, wherein the temperature raising speed in the whole process is 175-225 ℃/h, and the speed for continuous casting after melting is 25-50 mm/min to form a bonding rod material;
5) drawing: drawing the bonding rod material to obtain a filament, wherein the average deformation of each pass is 10-15%, and an alloy wire material with a preset wire diameter is formed;
6) annealing: annealing the filaments at the temperature of 570-620 ℃ for 3-6 hours, coating mixed alcohol on the surfaces of the annealed alloy filaments for anti-oxidation treatment, and then carrying out vacuum drying to obtain the bonding silver filaments;
the vacuum pressure condition of the vacuum melting is 10-2~10-4Pa;
The operations of the steps 2) to 6) are all carried out in a hydrogen-nitrogen environment, the hydrogen-nitrogen is a mixed gas of hydrogen and nitrogen, the content of the hydrogen is more than 3.5% and less than 5%, and good anti-oxidation protection is formed;
and step 5), drawing the wire, wherein the drawing comprises rough drawing, intermediate drawing, fine drawing and fine drawing, the target diameter of the rough drawing is 1-2 mm, the target diameter of the intermediate drawing is 0.5-0.8 mm, the target diameter of the fine drawing is 0.06-0.07 mm, and the target diameter of the fine drawing is 0.01-0.05 mm.
Example 2
A preparation method of a bonded silver wire material with stably distributed crystal grains comprises the following steps:
1) pretreatment: respectively cleaning silver, chromium, gold, scandium, palladium, calcium, lanthanum and copper substances by adopting argon gas, grinding into powder, sieving, preheating to 50-60 ℃, carrying out vacuum drying, simultaneously carrying out deoxidization treatment on the metal substances by adopting carbon monoxide,
2) preparing silver gold chromium melt: mixing 20% +/-0.2% of metallic silver, 0.5% +/-0.03% of gold and 0.5% +/-0.04% of chromium, putting the mixture into a silicon nitride crucible, adopting vacuum melting, raising the melting temperature to 860-920 ℃ at the beginning and maintaining the temperature for 10-30 minutes, raising the temperature to 975-1030 ℃ and maintaining the temperature for 10-50 minutes, raising the temperature to 1750-1830 ℃ and maintaining the temperature for 20-60 minutes, wherein the temperature raising speed in the whole process is 110-350 ℃/h, and obtaining a silver-gold-chromium melt after the melting is finished;
3) preparing a silver scandium palladium melt: mixing 20% +/-0.2% of metallic silver, 0.45% +/-0.04% of scandium and 0.45% +/-0.02% of palladium, putting the mixture into a silicon nitride crucible, adopting vacuum melting, raising the melting temperature to 860-920 ℃ at the beginning, maintaining the temperature for 10-30 minutes, raising the temperature to 1480-1520 ℃ and maintaining the temperature for 20-60 minutes, wherein the temperature raising speed in the whole process is 200-350 ℃/h, and completing the melting to obtain a silver-scandium-palladium melt;
4) continuous casting of bonding bar material: mixing 0.01% + -0.001% of metallic calcium, 0.01% + -0.004% of lanthanum, 0.01% + -0.001% of copper, 0.001 + -0.0001% of yttrium and/or selenium, 58% + -0.2% of the rest silver, a silver-gold-chromium melt and a silver-scandium-palladium melt, putting the mixture into a silicon nitride crucible, carrying out vacuum melting, raising the initial melting temperature to 800-1000 ℃ and maintaining the temperature for 15-30 minutes, raising the temperature to 1460-1500 ℃ and maintaining the temperature for 20-50 minutes, wherein the temperature raising speed in the whole process is 175-225 ℃/h, and the speed for continuous casting after melting is 25-50 mm/min, so as to form a bonding rod material;
5) drawing: drawing the bonding rod material to obtain a filament, wherein the average deformation of each pass is 10-15%, and an alloy wire material with a preset wire diameter is formed;
6) annealing: annealing the filaments at the temperature of 570-620 ℃ for 3-6 hours, coating mixed alcohol on the surfaces of the annealed alloy filaments for anti-oxidation treatment, and then carrying out vacuum drying to obtain the bonding silver filaments;
the vacuum pressure condition of the vacuum melting is 10-2~10-4Pa;
The operations of the steps 2) to 6) are all carried out in a hydrogen-nitrogen environment, the hydrogen-nitrogen is a mixed gas of hydrogen and nitrogen, the content of the hydrogen is more than 3.5% and less than 5%, and good anti-oxidation protection is formed;
and step 5), drawing the wire, wherein the drawing comprises rough drawing, intermediate drawing, fine drawing and fine drawing, the target diameter of the rough drawing is 1-2 mm, the target diameter of the intermediate drawing is 0.5-0.8 mm, the target diameter of the fine drawing is 0.06-0.07 mm, and the target diameter of the fine drawing is 0.01-0.05 mm.
And (3) detecting the performance of the bonded silver wire material:
the bonded silver wire materials of different thicknesses in example 1 were selected for elongation calculation and breaking load measurement, and the results are shown in table one:
watch 1
The bonded silver wire materials of different thicknesses in example 2 were selected for elongation calculation and breaking load measurement, and the results are shown in table two:
watch two
Selecting the bonded silver wire in the embodiment of the invention to perform SEM (scanning electron microscope) scanning, and observing the cross-section grain morphology of the bonded silver wire, wherein the obtained grain morphology is distributed more uniformly and tightly, so that the obtained bonded silver wire has more excellent bonding performance;
fig. 2 shows a bonding wire made of silver, gold and copper, and the size difference of the grains is relatively large and the distribution is not uniform when the bonding wire is scanned by an SEM electron microscope to observe the morphology of the grains in the cross section, which is much inferior to the bonding wire material prepared in this embodiment in terms of bonding performance, and the morphology of the grains inside the material affects the bonding and use of the bonding wire material.
Claims (10)
1. A bonded silver wire material with stably distributed crystal grains is characterized in that the material comprises 98% + -0.2% of silver, 0.5% + -0.04% of chromium, 0.5% + -0.03% of gold, 0.45% + -0.04% of scandium, 0.45% + -0.02% of palladium, 0.01% + -0.001% of calcium, 0.01% + -0.004% of lanthanum and 0.01% + -0.001% of copper.
2. The bonded silver wire material of claim 1, wherein the composition of the material further comprises 0.001% ± 0.0001% of other trace elements, and the trace elements comprise one or more of indium, cerium, yttrium, and selenium.
3. The bonded silver wire material of claim 1 or 2, wherein the interior of the material forms a uniformly distributed and dense morphology of metal grains having a grain size of 2 ~ 10 μm.
4. The bonded silver wire material of claim 1 or 2, wherein the purity of each constituent component is greater than 99%.
5. A preparation method of a bonded silver wire material with stable grain distribution is characterized by comprising the following steps:
1) pre-treating, namely cleaning silver, chromium, gold, scandium, palladium, calcium, lanthanum and copper substances by adopting argon respectively, grinding the cleaned substances into powder, sieving the powder, preheating the powder to 50 ~ 60 ℃ for vacuum drying, simultaneously deoxidizing the metal substances by adopting a reducing carbon material,
2) preparing silver-gold-chromium melt, namely mixing silver, gold and chromium, putting the mixture into a crucible, carrying out vacuum melting, raising the melting temperature to 860 ~ 920 ℃ and maintaining the temperature for 10 ~ 30 minutes, raising the temperature to 975 ~ 1030 ℃ and maintaining the temperature for 10 ~ 50 minutes, raising the temperature to 1750 ~ 1830 ℃ and maintaining the temperature for 20 ~ 60 minutes, wherein the temperature raising speed in the whole process is 110 ~ 350 ℃/h, and obtaining the silver-gold-chromium melt after the melting is finished;
3) preparing a silver scandium palladium melt, namely mixing metal silver, scandium and palladium, putting the mixture into a crucible, adopting vacuum melting, raising the melting temperature to 860 ~ 920 ℃ at the beginning, maintaining the temperature for 10 ~ 30 minutes, raising the temperature to 1480 ~ 1520 ℃ at the beginning, maintaining the temperature for 20 ~ 60 minutes, and finishing the melting at the temperature raising speed of 200 ~ 350 ℃/h in the whole process to obtain the silver scandium palladium melt;
4) taking metal calcium, lanthanum, copper, residual silver, silver-gold-chromium melt and silver-scandium-palladium melt, mixing and putting into a crucible, adopting vacuum melting, raising the melting temperature to 800 ~ 1000 ℃ at the beginning, maintaining the temperature for 15 ~ 30 minutes, raising the temperature to 1460 ~ 1500 ℃ and maintaining the temperature for 20 ~ 50 minutes, wherein the temperature raising speed in the whole process is 175 ~ 225 ℃/h, and the speed of continuous casting after melting is 25 ~ 50mm/min, so as to form the bonding rod material;
5) drawing, namely drawing the bonding rod material to obtain a filament, wherein the average deformation of each pass is 10 ~ 15%, and forming an alloy wire material with a preset wire diameter;
6) annealing, namely annealing the filament for 3 ~ 6 hours at the temperature of 570 ~ 620 ℃, coating mixed alcohol on the surface of the annealed alloy filament for anti-oxidation treatment, and then performing vacuum drying to obtain the bonded silver filament.
6. The method of manufacturing a bonded silver wire material according to claim 5, wherein the reduced carbon material in step 1) includes carbon monoxide and activated carbon.
7. The method for preparing a bonded silver wire material according to claim 5, wherein the crucible in the step 2) to the step 4) is a silicon nitride crucible or a silicon carbide crucible.
8. The method for producing a bonded silver wire material according to claim 5 or 7, wherein the vacuum melting is performed under a vacuum pressure condition of 10-2~10-4Pa。
9. The method for preparing the bonded silver wire material according to claim 5, wherein the operations of the steps 2) to 6) are all performed in a hydrogen-nitrogen environment, the hydrogen-nitrogen is a mixed gas of hydrogen and nitrogen, and the content of the hydrogen is more than 3.5% and less than 5%.
10. The method for producing a bonded silver wire material according to claim 5 or 9, wherein the drawing in step 5) includes rough drawing, middle drawing, fine drawing and fine drawing, the rough drawing having a target diameter of 1 ~ 2mm, the middle drawing having a target diameter of 0.5 ~ 0.8mm, the fine drawing having a target diameter of 0.06 ~ 0.07.07 mm, and the fine drawing having a target diameter of 0.01 ~ 0.05.05 mm.
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CN111593223A (en) * | 2020-04-03 | 2020-08-28 | 广东佳博电子科技有限公司 | Silver-platinum bonding wire material with high platinum-containing metal and preparation process thereof |
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