CN103789568A - Alloy bonding wire, and preparation method and application thereof - Google Patents
Alloy bonding wire, and preparation method and application thereof Download PDFInfo
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- CN103789568A CN103789568A CN201410054839.3A CN201410054839A CN103789568A CN 103789568 A CN103789568 A CN 103789568A CN 201410054839 A CN201410054839 A CN 201410054839A CN 103789568 A CN103789568 A CN 103789568A
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- 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
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- H01L2224/42—Wire connectors; Manufacturing methods related thereto
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- H—ELECTRICITY
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- 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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- 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
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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
- H01L2224/4501—Shape
- H01L2224/45012—Cross-sectional shape
- H01L2224/45015—Cross-sectional shape being circular
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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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- 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
- H01L2224/45144—Gold (Au) as principal constituent
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- H01L2924/10—Details of semiconductor or other solid state devices to be connected
- H01L2924/11—Device type
- H01L2924/12—Passive devices, e.g. 2 terminal devices
- H01L2924/1204—Optical Diode
- H01L2924/12041—LED
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Abstract
The invention provides an alloy bonding wire, and a preparation method and an application thereof, wherein the alloy bonding wire is composed of, by weight percentage, 5-10% of gold, 1-5% of aluminum, 0.5-5% of nickel and the balance of silver having the purity greater than or equal to 99.999wt%. The alloy bonding wire is low in cost, excellent in bonding performance, free of breakage under a high-speed bonding condition, good in mechanical properties, and further applicable to an integrated circuit, a large-scale integrated circuit, a discrete device and an LED (Light Emitting Diode) package.
Description
Technical field
The present invention relates to a kind of alloy bonding silk, belong to packaged material technical field, the invention still further relates to preparation method and the application thereof of described alloy bonding silk.
Background technology
Bonding wire is the crucial lead material being connected with lead frame for unicircuit or transistor chip tube core.Conventional keys plying is mainly made up of proof gold material.The bonding wire of proof gold material has the preferably physical properties such as ductility and electroconductibility.But along with being growing more intense of LED and IC product market competition, production marketing price declines to a great extent, how to develop a kind of effect that can reach proof gold bonding wire, and the metallic bond plying that can significantly reduce material cost becomes the extremely urgent task of encapsulation enterprise.
Chinese patent literature CN102418011A discloses a kind of bonding gold wire, in described spun gold, add silver, also in addition element Ca, Pd, Cu, In, Sn, Ni, La, Sc, Ce one or more, wherein in bonding gold wire, the weight percentage of silver is 10%-25%, and the weight percentage of gold is about 74%-89%.This technical scheme is still take gold as base material, and the cost of bonding wire is still very high.
Chinese patent literature CN101569968B discloses the silver alloys bonding wire that a kind of packaging conductive wire is used, and the moiety of this silver alloys bonding wire comprises: the silver-colored composition that weight percent is 90.00～99.99%; Weight percent is 0.0001～9.9997% golden composition; And the weight percent copper component that is 0.0001～9.9997%.The welding effect of the silver alloys bonding wire described in this technical scheme is undesirable, easy broken string under high speed bonding conditions.
The above analysis, how to provide a kind of with low cost, bonding performance is good, the bonding wire and the production technique thereof that do not break under high speed bonding conditions are the technical barriers also not solving in prior art.
Summary of the invention
For this reason, technical problem to be solved by this invention be to provide a kind of with low cost, bonding performance is good, do not break under high speed bonding conditions, bonding wire that mechanical property is strong and preparation method thereof.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The invention provides a kind of alloy bonding silk, this alloy bonding silk comprises: golden 5-10wt%, aluminium 1-5wt%, nickel 0.5-5wt%, all the other silver that are purity >=99.999wt%.
Preferred as one, the invention provides a kind of alloy bonding silk, the composition of this alloy bonding silk and weight content are: golden 6-9wt%, aluminium 2-4wt%, nickel 1-4wt%, all the other silver that are purity >=99.999wt%.
Preferred as one, the invention provides a kind of alloy bonding silk, the composition of this alloy bonding silk and weight content are: golden 7-8wt%, aluminium 3wt%, nickel 2-3wt%, all the other silver that are purity >=99.999wt%.
Preferred as one, described alloy bonding silk also adds a kind of in Ca, Se, Rh, Be, Co, In or wherein several.
Preferred as one, described alloy bonding silk adds a kind of in Ca, Se that weight content is 1-120ppm, Rh, Be, Co, In or wherein several.
Preferred as one, described alloy bonding silk adds the Ca that weight content is 1-20ppm, the Se of 1-20ppm, the Rh of 1-20ppm, the Be of 1-20ppm, the Co of 1-20ppm, the In of 1-20ppm.
The present invention also provides a kind of method of preparing above-mentioned alloy bonding silk, and described method comprises the steps:
(1) raw metal silver, gold, aluminium, nickel are placed in smelting furnace and carry out founding, to make silver alloys ingot bar;
(2) the silver alloys ingot bar of step (1) being made carries out Wire Drawing, forms the silver alloys wire rod of predetermined wire diameter;
(3) the silver alloys wire rod of step (2) being made carries out annealing process processing, makes required alloy bonding silk.
Wherein, in described method steps (1), raw metal is: golden 5-10wt%, aluminium 1-5wt%, nickel 0.5-5wt%, all the other silver that are purity >=99.999wt%; Preferred golden 6-9wt%, aluminium 2-4wt%, nickel 1-4wt%, all the other silver that are purity >=99.999wt%; More select golden 7-8wt%, aluminium 3wt%, nickel 2-3wt%, all the other silver that are purity >=99.999wt%.
Preferred as one, in described method steps (1), also comprise and add a kind of in trace metal raw materials of Ca, Se, Rh, Be, Co, In or wherein several to carry out founding.
Preferred as one, in described method steps (1), also comprising and adding weight content is the Ca of 1-20ppm, the Se of 1-20ppm, and the Rh of 1-20ppm, the Be of 1-20ppm, the Co of 1-20ppm, the In of 1-20ppm carries out founding.
In described method steps (3), annealing process silver alloys wire rod after treatment also carries out wire winding processing.
Described wire winding silver alloys wire rod after treatment also carries out packaging process processing.
That drawing process in described step (2) comprises is rough, in draw, carefully draw, ultra tiny stretching.
Annealing process processing in described step (3) includes finished products, performance test process.
Alloy bonding silk prepared by above-mentioned any alloy bonding silk or above-mentioned any method is useful on the purposes of packaging conductive wire.
Technique scheme of the present invention has the following advantages compared to existing technology:
1. alloy bonding silk provided by the invention, take high-purity silver material as basis, add the minor elements such as gold, aluminium, nickel, also can add a kind of in micro-metals Ca, Se, Rh, Be, Co, In or wherein several, and after reasonable analysis and test of many times, select every kind of optimum content that adds element, make to interact between each element of alloy, reach optimal effectiveness.Evidence, the mechanical property of alloy bonding silk of the present invention, the conventional keys B alloy wire that physicals is all better than equal wire diameter, and the material cost of alloy bonding silk of the present invention is only 1/8 of gold wire rod, macromarketing price is only 1/5 of same specification gold thread, greatly reduces the manufacturing cost of LED and IC encapsulation.
The bonding performance of alloy bonding silk provided by the invention is good, under pure nitrogen gas protective condition, can realize any welding technique requirement, comprises that planting ball bonding connects, and meets every welding test request, and properties exceedes bonding gold wire.
Alloy bonding silk provided by the invention is difficult for fracture of wire under high speed bonding conditions, a little higher than conventional keys alloy of outage silk thread, and the mechanical property of the alloy bonding silk of the present invention of fine line diameter is equal to or is better than the conventional keys plying in thick line footpath.
The oxidation-resistance of alloy bonding silk provided by the invention is better compared to fine silver bonding wire, can realize and plant ball welding requirements.Alloy bonding silk provided by the invention is compared with bonding gold wire: price is cheaper, and disconnected Li Genggao is chosen in stable performance.
Alloy bonding silk provided by the invention can be used as packaging conductive wire, is satisfied with multiple encapsulation requirement, has both been applicable to unicircuit, the microminiaturized encapsulation of large-scale integrated circuit, is also applicable to discrete device, LED encapsulation.
2. alloy bonding silk preparation method provided by the invention, comprises raw metal silver, gold, aluminium, nickel is placed in smelting furnace and carries out founding, to make the step of silver alloys ingot bar; Silver alloys ingot bar is carried out to Wire Drawing, form the step of the silver alloys wire rod of predetermined wire diameter; The silver alloys wire rod of making is carried out to annealing process processing, make the step of required alloy bonding silk.Alloy bonding silk preparation method provided by the invention is convenient and practical.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below embodiments of the present invention are described in further detail.
Embodiment 1:
The invention provides a kind of alloy bonding silk, the composition of this alloy bonding silk and weight content are: 5N gold 5wt%, aluminium 2wt%, nickel 1wt%, 5N silver 91.99wt%, the about 0.01wt% of trace metal raw material;
It is as follows that trace metal raw material adds content:
5ppm≤calcium≤20ppm
2ppm≤rhodium≤10ppm
20ppm≤beryllium≤50ppm
5ppm≤cobalt≤10ppm
3ppm≤indium≤10ppm
5ppm≤selenium≤10ppm.
Wherein, 5N gold refers to that purity is 99.999% gold; 5N silver refers to that purity is 99.999% silver.
The present invention also provides the preparation method of above-mentioned alloy bonding silk, and the method comprises the steps:
1) mother metal of silver, gold, aluminium, nickel and micro-metals composition is placed in smelting furnace and carries out founding, to make silver alloys ingot bar;
The 1000g that always feeds intake, wherein 5N ag material, content 91.99wt%, meter 919.9g; 5N gold 5wt%, meter 50g; Aluminium 2wt%, meter 20g; Nickel 1wt%, meter 10g; Add trace metal raw material 0.01wt%, meter 0.1g;
It is as follows that trace metal raw material adds content:
5ppm≤calcium≤20ppm
2ppm≤rhodium≤10ppm
20ppm≤beryllium≤50ppm
5ppm≤cobalt≤10ppm
3ppm≤indium≤10ppm
5ppm≤selenium≤10ppm
2) the silver alloys ingot bar of step (1) being made carries out Wire Drawing, forms the silver alloys wire rod of predetermined wire diameter;
3) the silver alloys wire rod of step (2) being made carries out annealing process processing, makes required alloy bonding silk.
Wherein, in alloy bonding silk preparation method of the present invention,
Step (1) is placed in the mother metal of metallic element composition in smelting furnace and carries out founding, and described fusion-casting process can carry out under vacuum condition.
During drawing process in step (2) includes, draw, carefully draw, ultra tiny stretching, alloy wire is stretched to predetermined wire diameter.For example, after silver alloys wire rod has been cast, carry out wire diameter stretching, first stretch through the first thick wire drawing machine, wire diameter is stretched to 1mm by 8mm, draw speed is 0.1m/s, again by silver alloys wire rod sequentially through the second thin wire drawing machine, superfine wire drawing machine, and super superfine wire drawing machine stretches, wherein, the second thin wire drawing machine (SS21BC that for example Japanese SKAWA company produces) is stretched to 0.1mm by wire rod by 1mm, draw speed is 0.5m/s, superfine wire drawing machine (WSS21BC that for example Japanese SKAWA produces) is stretched to 0.05mm by wire rod by 0.1, draw speed is 1m/s, and silver alloys wire rod is further stretched as predetermined wire diameter 23 μ m by super superfine wire drawing machine (WSS21BC that for example Japanese SKAWA produces), the specific silver alloys bonding wire of 25 μ m, the speed stretching is 3-6m/s.
Annealing process processing in step (3) includes finished products, performance test treating processes.
The mechanical performance comparison of annealing is as follows
Embodiment 1 alloy bonding silk physicals:
| Alloy melting point | 1080℃ |
| Density g/cm 3 | 10.7 |
| Resistivity μ Ω cm | 2.8 |
| Hardness Hv | 35-38 |
| Annealing temperature | 400-600℃ |
| Wire color | Silvery white |
Above-mentioned alloy bonding silk is carried out to packaging process processing, and bonding packaging parameter is:
| Wire rod title | Bonding gold wire | Embodiment 1 wire rod |
| Equipment | KS | KS |
| Bonding power (W) | 160 | 165 |
| Welding pressure (N) | 95 | 95 |
| Welding fluency | OK | OK |
| Crater | pass | pass |
| Bonding wire is chosen disconnected power (cN) | ≥5cN | ≥7cN |
| Soldered ball thrust (N) | ≥30 | ≥30 |
| Whether planting ball bonding connects | Plant ball | Plant ball |
| Bonding wire broken string number of times (working 4 hours) | 1-2 time | 4-5 time |
| Aging | Without defective products | Without defective products |
| Thermal shock | Without defective products | Without defective products |
| Conclusion | OK | OK |
Embodiment 2:
Alloy bonding silk of the present invention, the 1000g that always feeds intake, 5N ag material, content 90.49wt%, meter 904.9g; 5N gold 8wt%, meter 80g; Aluminium 1wt%, meter 10g; Nickel 0.5wt%, meter 5g; Add trace metal raw material 0.01wt%, meter 0.1g; Alloy adds content and the following is:
5ppm≤calcium≤20ppm
2ppm≤rhodium≤10ppm
20ppm≤beryllium≤50ppm
5ppm≤cobalt≤10ppm
3ppm≤indium≤18ppm
The present invention also provides the preparation method of above-mentioned alloy bonding silk, and the method comprises the steps:
1) mother metal of silver, gold, aluminium, nickel and micro-metals composition is placed in smelting furnace and carries out founding, to make silver alloys ingot bar;
The 1000g that always feeds intake, the 1000g that always feeds intake, 5N ag material, content 90.49wt%, meter 904.9g; 5N gold 8wt%, meter 80g; Aluminium 1wt%, meter 10g; Nickel 0.5wt%, meter 5g; Add trace metal raw material 0.01%, meter 0.1g; Alloy adds content and the following is:
5ppm≤calcium≤20ppm
2ppm≤rhodium≤10ppm
20ppm≤beryllium≤50ppm
5ppm≤cobalt≤10ppm
3ppm≤indium≤18ppm
2) the silver alloys ingot bar of step (1) being made carries out Wire Drawing, forms the silver alloys wire rod of predetermined wire diameter;
3) the silver alloys wire rod of step (2) being made carries out annealing process processing, makes required alloy bonding silk.
The mechanical performance comparison of annealing is as follows
Embodiment 2 alloy bonding silk physicalies:
| Alloy melting point | 1100℃ |
| Density g/cm 3 | 10.9 |
| Resistivity μ Ω cm | 2.7 |
| Hardness Hv | 37-40 |
| Annealing temperature | 400-600℃ |
| Wire color | Silvery white |
Bonding packing parameter
| Wire rod title | Bonding gold wire | Embodiment 2 wire rods |
| Equipment | KS | KS |
| Bonding power (W) | 170 | 175 |
| Welding pressure (N) | 95 | 95 |
| Welding fluency | OK | OK |
| Crater | pass | pass |
| Bonding wire is chosen disconnected power (cN) | ≥5cN | ≥7cN |
| Soldered ball thrust | ≥30 | ≥30 |
| Whether planting ball bonding connects | Plant ball | Plant ball |
| Bonding wire broken string number of times (working 4 hours) | 1-2 time | 6-7 time |
| Aging | Without defective products | Without defective products |
| Thermal shock | Without defective products | Without defective products |
| Conclusion | OK | OK |
Embodiment 3:
Alloy bonding silk of the present invention, the 1000g that always feeds intake, 5N ag material, content 79.99wt%, meter 799.9g; 5N gold 10wt%, meter 100g; Aluminium 5wt%, meter 50g; Nickel 5wt%, meter 50g; Add trace metal raw material 0.01wt%, meter 0.1g; Alloy adds content and the following is:
5ppm≤calcium≤10ppm
5ppm≤rhodium≤20ppm
20ppm≤beryllium≤50ppm
10ppm≤cobalt≤20ppm
2ppm≤indium≤5ppm
The present invention also provides the preparation method of above-mentioned alloy bonding silk, and the method comprises the steps:
1) mother metal of silver, gold, aluminium, nickel and micro-metals composition is placed in smelting furnace and carries out founding, to make silver alloys ingot bar;
The 1000g that always feeds intake, 5N ag material, content 79.99wt%, meter 799.9g; 5N gold 10wt%, meter 100g; Aluminium 5wt%, meter 50g; Nickel 5wt%, meter 50g; Add trace metal raw material 0.01%, meter 0.1g; Alloy adds content and the following is:
5ppm≤calcium≤10ppm
5ppm≤rhodium≤20ppm
20ppm≤beryllium≤50ppm
10ppm≤cobalt≤20ppm
2ppm≤indium≤5ppm
2) the silver alloys ingot bar of step (1) being made carries out Wire Drawing, forms the silver alloys wire rod of predetermined wire diameter;
3) the silver alloys wire rod of step (2) being made carries out annealing process processing, makes required alloy bonding silk.
The mechanical performance comparison of annealing is as follows
Embodiment 3 alloy bonding silk physicalies:
| Alloy melting point | 1100℃ |
| Density g/cm 3 | 10.9 |
| Resistivity μ Ω cm | 2.7 |
| Hardness Hv | 37-40 |
| Annealing temperature | 400-600℃ |
| Wire color | Silvery white |
Bonding packing parameter
| Wire rod title | Bonding gold wire | Embodiment 3 wire rods |
| Equipment | KS | KS |
| Bonding power (W) | 170 | 175 |
| Welding pressure (N) | 95 | 95 |
| Welding fluency | OK | OK |
| Crater | pass | pass |
| Bonding wire is chosen disconnected power (cN) | ≥5cN | ≥7cN |
| Soldered ball thrust | ≥30 | ≥30 |
| Whether planting ball bonding connects | Plant ball | Plant ball |
| Bonding wire broken string number of times (working 4 hours) | 1-2 time | 6-8 time |
| Aging | Without defective products | Without defective products |
| Thermal shock | Without defective products | Without defective products |
| Conclusion | OK | OK |
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being extended out thus or variation are still among protection scope of the present invention.
Claims (14)
1. an alloy bonding silk, is characterized in that: this alloy bonding silk comprises: golden 5-10wt%, aluminium 1-5wt%, nickel 0.5-5wt%, all the other silver that are purity >=99.999wt%.
2. alloy bonding silk according to claim 1, is characterized in that: described alloy bonding silk comprises: golden 6-9wt%, aluminium 2-4wt%, nickel 1-4wt%, all the other silver that are purity >=99.999wt%.
3. alloy bonding silk according to claim 1, is characterized in that: the composition of described alloy bonding silk and content are: golden 7-8wt%, aluminium 3wt%, nickel 2-3wt%, all the other silver that are purity >=99.999wt%.
4. according to the alloy bonding silk described in claim 1-3 any one, it is characterized in that: described alloy bonding silk also adds a kind of in Ca, Se, Rh, Be, Co, In or wherein several.
5. according to the alloy bonding silk described in claim 1-4 any one, it is characterized in that: described alloy bonding silk adds a kind of in Ca, Se that weight content is 1-120ppm, Rh, Be, Co, In or wherein several.
6. according to the alloy bonding silk described in claim 1-5 any one, it is characterized in that: described alloy bonding silk adds the Ca that weight content is 1-20ppm, the Se of 1-20ppm, the Rh of 1-20ppm, the Be of 1-20ppm, the Co of 1-20ppm, the In of 1-20ppm.
7. a method of preparing alloy bonding silk described in claim 1-6 any one, is characterized in that: described method comprises the steps:
(1) raw metal silver, gold, aluminium, nickel are placed in smelting furnace and carry out founding, to make silver alloys ingot bar;
Wherein, described raw metal comprises: golden 5-10wt%, aluminium 1-5wt%, nickel 0.5-5wt%, all the other silver that are purity >=99.999wt%;
(2) the silver alloys ingot bar of step (1) being made carries out Wire Drawing, forms the silver alloys wire rod of predetermined wire diameter;
(3) the silver alloys wire rod of step (2) being made carries out annealing process processing, makes required alloy bonding silk.
8. alloy bonding silk preparation method according to claim 7, is characterized in that: in described method steps (1), also comprise and add a kind of in trace metal raw materials of Ca, Se, Rh, Be, Co, In or wherein several to carry out founding.
9. according to the alloy bonding silk preparation method described in claim 7 or 8, it is characterized in that: in described method steps (1), also comprising and adding weight content is the Ca of 1-20ppm, the Se of 1-20ppm, the Rh of 1-20ppm, the Be of 1-20ppm, the Co of 1-20ppm, the In of 1-20ppm carries out founding.
10. according to the alloy bonding silk preparation method described in claim 7-9 any one, it is characterized in that: in described method steps (3), annealing process silver alloys wire rod after treatment also carries out wire winding processing.
11. alloy bonding silk preparation methods according to claim 10, is characterized in that: described wire winding silver alloys wire rod after treatment also carries out packaging process processing.
12. according to the alloy bonding silk preparation method described in claim 7-11 any one, it is characterized in that: the drawing process in described step (2) comprise rough, in draw, carefully draw, ultra tiny stretching.
13. according to the alloy bonding silk preparation method described in claim 7-12 any one, it is characterized in that: the annealing process processing in described step (3) includes finished products, performance test process.
The alloy bonding silk that described in alloy bonding silk described in 14. claim 1-6 any one or claim 7-13 any one prepared by method can be used for the purposes of packaging conductive wire.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410054839.3A CN103789568B (en) | 2014-02-18 | 2014-02-18 | A kind of alloy bonding silk and preparation method and application |
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