CN108122877A - Thin gold copper line and its manufacturing method - Google Patents

Thin gold copper line and its manufacturing method Download PDF

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Publication number
CN108122877A
CN108122877A CN201711394116.8A CN201711394116A CN108122877A CN 108122877 A CN108122877 A CN 108122877A CN 201711394116 A CN201711394116 A CN 201711394116A CN 108122877 A CN108122877 A CN 108122877A
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palladium
plating
cored wire
gold
annealing
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CN108122877B (en
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周振基
周博轩
麦宏全
彭政展
陈怡廷
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Shantou Junma Kaisa Coltd
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Shantou Junma Kaisa Coltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/49—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions wire-like arrangements or pins or rods
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0607—Wires
    • 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 at least one potential-jump barrier or surface barrier, e.g. 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
    • H01L21/4889—Connection or disconnection of other leads to or from wire-like parts, e.g. wires

Abstract

A kind of thin gold copper line, it is characterised in that including cored wire, the palladium pre-plating layer being coated on outside cored wire and the golden clad being coated on outside palladium pre-plating layer；The cored wire is by weight containing Pd 0.1 3%, and 1 300 ppm of trace additives, surplus is copper；The trace additives are combinations more than one kind or two of which in Ca, In, Co, Be, Ga, Mg, Ce, Ni, Pt and Al；The thickness of the palladium pre-plating layer is 1 40 nm, and the thickness of golden clad is 1 30 nm.The present invention also provides a kind of manufacturing methods of above-mentioned thin gold copper line.The thin gold copper line of the present invention has excellent workability and reliability, and cost is relatively low, and long lifespan after opening.

Description

Thin gold copper line and its manufacturing method
Technical field
The present invention relates to the bonding wires of IC, LED encapsulation, and in particular to a kind of thin gold copper line and its manufacturing method.
Background technology
Bonding wire（Bonding wire, also known as bonding line）It is connection chip and outer enclosure substrate（substrate）It is and/or more Sandwich circuit board（PCB）Main connection mode.The development trend of bonding wire, from the line of production, mainly line footpath is made fine, is high The workshop service life（floor life）And high spool length；Chemically on ingredient, mainly there is copper wire（Including bare copper wire, plating palladium copper Line dodges gold plating palladium copper wire）Significantly substitute gold thread in semiconductor applications, and silver wire and silver alloy wire are sealed in LED and part IC Dress applies upper substitution gold thread.Due to miniaturization of electronic products and the demand for development of thin thinning, semicon industry passes through chip thickness (Wafer thinning), encapsulation is thinned using chip stack (Die stacking), flip-chip (flip chip), wafer Grade encapsulation（wafer level packaging）, 2.5D and 3D the methods of encapsulating tackle, however traditional bonding packaging （wire bonding）It is still mainstream packing forms.
A kind of existing plating palladium gold-plated copper wires, including cored wire, the palladium pre-plating layer being coated on outside cored wire and to be coated on palladium pre- Golden clad outside coating, cored wire are made of fine copper.This plating palladium gold-plated copper wires are in order to ensure good workability and can By property, it is necessary to coat the thicker palladium pre-plating layer of thickness and golden clad, the wherein thickness of palladium pre-plating layer is 50-120nm, and gold coats The thickness of layer is 35-60nm, so that manufacture cost is excessively high, lacks the market competitiveness.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of thin gold copper line and this thin gold copper line Manufacturing method, this thin gold copper line has excellent workability and reliability, and cost is relatively low.The technical solution of use is such as Under：
A kind of thin gold copper line, it is characterised in that including cored wire, the palladium pre-plating layer being coated on outside cored wire and be coated on palladium Golden clad outside pre-plating layer；The cored wire is by weight containing Pd 0.1-3%, trace additives 1-300 ppm, surplus For copper；The trace additives are more than one kind or two of which in Ca, In, Co, Be, Ga, Mg, Ce, Ni, Pt and Al Combination；The thickness of the palladium pre-plating layer is 1-40 nm, and the thickness of golden clad is 1-30 nm.
It is preferred that the thickness of above-mentioned palladium pre-plating layer is 5-15 nm, the thickness of golden clad is 10-20 nm.
In general, above-mentioned palladium pre-plating layer is the palladium layers that purity is more than 99%（Such as the ingredient of palladium pre-plating layer is that purity is 99- 99.99% palladium）, golden clad is the layer gold that purity is more than 99%（Such as the ingredient of golden clad is that purity is 99-99.99% Gold）.
In the thin gold copper line of the present invention, the palladium of content 0.1-3% is added in cored wire（Pd）, wire rod can be effectively improved Anti-oxidant and sulfuration resistant performance, and improve reliability of the encapsulating products in thermal shock test；Suitable trace additives To improve the mechanical performance of wire rod, wherein Ca, In, Ga, Mg, Ce, Ni can effectively promote the bonding wire workability of billon, can increase The adhesion property of strong wire rod and chip and substrate, is promoted and trusts performance；Co, Be, Pt, Al etc. can improve tying again for billon wire rod Brilliant temperature promotes wire rod fatigue durability in a high temperauture environment, effectively reduces the probability of neck broken string.Since wire surface coats There is golden clad, can effectively promote wire rod and chip and the joint capacity of substrate, effectively promote reliability.It is in cored wire and Jin Bao Palladium pre-plating layer between coating is a good adhesive layer, is tightly engaged into wire rod, and promotes aging ability.
The present invention also provides a kind of manufacturing methods of above-mentioned thin gold copper line, it is characterised in that comprises the following steps：
（1）Founding：Pd and trace additives are added in copper raw material in proportion, continuously draw casting by vacuum melting and orientation Technique obtains core wires 6-8 millimeters a diameter of；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 50-280um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, N is used in annealing process2Or nitrogen Hydrogen gaseous mixture comes as annealing atmosphere, and annealing furnace effective length is 600-1000mm, and annealing temperature is 300-600 DEG C, annealing speed Rate is 60-120m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Micron）Core Line；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 1-40 nm （It is preferred that 5-15 nm）, obtain plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 1-30 nm（It is preferred that 10-20 nm）, obtain plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and N is used in annealing process2Or Nitrogen and hydrogen mixture comes as annealing atmosphere, and annealing furnace effective length is 600-1000mm, and annealing temperature is 300-600 DEG C, annealing Rate is 60-120m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 20-30 DEG C, obtains required thin gold copper line. Step（5）The palladium coating of formation forms the palladium pre-plating layer in thin gold copper line, step（5）The gold plate of formation forms Bao Jintong Golden clad in alloy wire.
It is preferred that above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition immerses the acetone ethanol mixed liquor that temperature is 70-150 DEG C In, it is 1.4-8 seconds to immerse the time, the organic matter on removing cored wire surface；The weight of acetone and ethyl alcohol in the acetone ethanol mixed liquor Amount ratio is 1:5-10；
（5-2）Remove oxide process：It is 70-150 DEG C, weight percent by temperature is immersed by the cored wire of removing organic matter processing Specific concentration is in the nitric acid of 30-50%, and it is 1.4-8 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：It is 70-150 DEG C, weight percent by temperature is immersed by the cored wire of removing oxide process Concentration is in the sulfuric acid of 10-30%, and it is 1.4-8 seconds to immerse the time, and surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, in the condition that electroplating current is 0.2-0.8A Lower plating palladium, it is 1-40 nm that thickness is formed on the surface of cored wire（It is preferred that 5-15 nm）Palladium coating, the palladium coating is by cored wire bag It covers；
（5-5）Cleaning：Using pure water as cleaning solution, ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife；
When being electroplated, with the continuous release steps of the speed of 5-30m/min（4）The cored wire of acquisition, cored wire is successively by above-mentioned de- After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
It is preferred that above-mentioned steps（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, The concentration of middle palladium sulfate is 1-4g/L, and the concentration of ammonium chloride is 1-4g/L, and the concentration of ammonium sulfate is 1-4g/L.Ammonium chloride and sulfuric acid Ammonium is as conductive agent.
It is preferred that above-mentioned steps（5-5）In, using pure water as cleaning solution, twice Supersonic is carried out to the cored wire for being coated with palladium coating Ripple cleans.
It is preferred that above-mentioned steps（5-6）In, air knife air-flow is N2, flow velocity 5-20L/min.
It is preferred that above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 2-4g/L, is in electroplating current Gold-plated under conditions of 0.2-0.8A, it is 1-30 nm that thickness is formed on the surface of plating palladium line（It is preferred that 10-20 nm）Gold plate, The gold plate coats palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife；
When being electroplated, with the continuous release steps of the speed of 5-30m/min（5）The plating palladium line of acquisition, plating palladium line is successively by upper After stating gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
It is preferred that above-mentioned steps（6-1）In, the gold plating liquid of use is potassium auricyanide solution.
It is preferred that above-mentioned steps（6-2）In, using pure water as cleaning solution, twice are carried out to the plating palladium line for being coated with gold plate and are surpassed Sound wave cleans.
It is preferred that above-mentioned steps（6-3）In, air knife air-flow is N2, flow velocity 5-20L/min.
It is preferred that above-mentioned steps（3）And step（7）The nitrogen and hydrogen mixture of use by 5% (volume) H2With 95% (volume) N2Composition.
The thin gold copper line of the present invention compared with prior art, has the advantages that：
（1）Palladium and trace additives are uniformly distributed in Copper base material in cored wire, and palladium atom can be in routing and reliability processing procedure Even diffusion makes thin gold copper line have excellent workability（CUP (Circuit Under Pad) electrode lower circuit will not It breaks or punctures）And reliability；
（2）There are relatively low wire rod hardness, HAZ（Heat affected area）Length down to 50 um, can significantly reduce the camber of routing；
（3）Preferable is inhibited to copper-aluminium Jie metallic compound；
（4）Good zygosity can be provided, effectively aqueous vapor is prevented to immerse interface, gold goal under IC hot and humid environments can be improved It comes off（ball lift）Problem；
（5）Cost is relatively low, and cost 10-20% can be reduced compared with plating palladium gold-plated copper wires, and reliability is then with plating palladium gold-plated copper wires phase When, may replace plating palladium gold-plated copper wires；
（6）The thin gold copper line of the present invention is sealed off（Dismantle the outer packing of wire rod）Long lifespan afterwards.
Specific embodiment
Embodiment 1
The thin gold copper line of the present embodiment includes cored wire, the palladium pre-plating layer being coated on outside cored wire and is coated on palladium pre-plating layer The golden clad of outside；The cored wire is by weight containing Pd 1.5%, Ca 30ppm, Be 25 ppm, In 30ppm, surplus For copper；The thickness of the palladium pre-plating layer is 10 nm, and the thickness of golden clad is 12nm.
The manufacturing method of above-mentioned thin gold copper line comprises the following steps：
（1）Founding：Pd, Ca, Be and In are added in copper raw material in proportion, continuously draw foundry work by vacuum melting and orientation Skill obtains a diameter of 6 millimeters of core wires；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 150um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, N is used in annealing process2Come as Annealing atmosphere, annealing furnace effective length are 800mm, and annealing temperature is 500 DEG C, annealing rate 80m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Such as 20um）'s Cored wire；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 10nm, is obtained To plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 12nm, obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and N is used in annealing process2To do For annealing atmosphere, annealing furnace effective length is 800mm, and annealing temperature is 500 DEG C, annealing rate 80m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 25 DEG C, obtains required thin gold copper line.
Above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition is immersed in the acetone ethanol mixed liquor that temperature is 120 DEG C, It is 4 seconds to immerse the time, the organic matter on removing cored wire surface；The weight ratio of acetone and ethyl alcohol is in the acetone ethanol mixed liquor 1:6；
（5-2）Remove oxide process：It is 120 DEG C, weight percent by temperature is immersed by the cored wire of removing organic matter processing Concentration is in 40% nitric acid, and it is 4 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：The cored wire immersion temperature that removing oxide process will be passed through is 120 DEG C, weight percent is dense It spends in the sulfuric acid for 20%, it is 4 seconds to immerse the time, and surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, is plated under conditions of electroplating current is 0.5A Palladium, forms the palladium coating that thickness is 10nm on the surface of cored wire, which coats cored wire；
This step（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, wherein palladium sulfate Concentration is 2g/L, the concentration 3g/L of ammonium chloride, the concentration 1g/L of ammonium sulfate；
（5-5）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife（Air knife air-flow is N2, flow velocity 10L/ min）；
When being electroplated, with the continuous release steps of the speed of 15m/min（4）The cored wire of acquisition, cored wire pass through above-mentioned removing successively After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
Above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 3g/L（The gold plating liquid of use is cyanogen Change golden potassium solution）, it is gold-plated under conditions of electroplating current is 0.5A, the gold plating that thickness is 12nm is formed on the surface of plating palladium line Layer, the gold plate coat palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife（Air knife air-flow is N2, flow velocity 10L/ min）；
When being electroplated, with the continuous release steps of the speed of 15m/min（5）The plating palladium line of acquisition, plating palladium line is successively by above-mentioned After gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
Embodiment 2
The thin gold copper line of the present embodiment includes cored wire, the palladium pre-plating layer being coated on outside cored wire and is coated on palladium pre-plating layer The golden clad of outside；The cored wire is by weight containing Pd 0.5%, 25 ppm of Mg 80 ppm, Ca 60ppm, Ce, surplus For copper；The thickness of the palladium pre-plating layer is 8 nm, and the thickness of golden clad is 15 nm.
The manufacturing method of above-mentioned thin gold copper line comprises the following steps：
（1）Founding：Pd, Mg, Ca and Ce are added in copper raw material in proportion, continuously draw foundry work by vacuum melting and orientation Skill obtains a diameter of 8 millimeters of core wires；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 280um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, N is used in annealing process2Come as Annealing atmosphere, annealing furnace effective length are 1000mm, and annealing temperature is 300 DEG C, annealing rate 80m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Such as 20um）'s Cored wire；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 8 nm, is obtained To plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 15nm, obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and N is used in annealing process2To do For annealing atmosphere, annealing furnace effective length is 1000mm, and annealing temperature is 600 DEG C, annealing rate 120m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 30 DEG C, obtains required thin gold copper line.
Above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition is immersed in the acetone ethanol mixed liquor that temperature is 150 DEG C, It is 1.4 seconds to immerse the time, the organic matter on removing cored wire surface；The weight ratio of acetone and ethyl alcohol in the acetone ethanol mixed liquor For 1:5；
（5-2）Remove oxide process：It is 150 DEG C, weight percent by temperature is immersed by the cored wire of removing organic matter processing Concentration is in 30% nitric acid, and it is 1.4 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：The cored wire immersion temperature that removing oxide process will be passed through is 150 DEG C, weight percent is dense It spends in the sulfuric acid for 30%, it is 1.4 seconds to immerse the time, and surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, is plated under conditions of electroplating current is 0.2A Palladium, forms the palladium coating that thickness is 8 nm on the surface of cored wire, which coats cored wire；
This step（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, wherein palladium sulfate Concentration is 4g/L, the concentration 4g/L of ammonium chloride, the concentration 2g/L of ammonium sulfate；
（5-5）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife（Air knife air-flow is N2, flow velocity 5L/ min）；
When being electroplated, with the continuous release steps of the speed of 30m/min（4）The cored wire of acquisition, cored wire pass through above-mentioned removing successively After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
Above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 4g/L（The gold plating liquid of use is cyanogen Change golden potassium solution）, it is gold-plated under conditions of electroplating current is 0.2A, the gold plating that thickness is 15nm is formed on the surface of plating palladium line Layer, the gold plate coat palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife（Air knife air-flow is N2, flow velocity 5L/ min）；
When being electroplated, with the continuous release steps of the speed of 5m/min（5）The plating palladium line of acquisition, plating palladium line is successively by above-mentioned After gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
Embodiment 3
The thin gold copper line of the present embodiment includes cored wire, the palladium pre-plating layer being coated on outside cored wire and is coated on palladium pre-plating layer The golden clad of outside；The cored wire is by weight containing Pd 2%, and Ni 20 ppm of 20 ppm, Co, surplus is copper；The palladium The thickness of pre-plating layer is 12 nm, and the thickness of golden clad is 18 nm.
The manufacturing method of above-mentioned thin gold copper line comprises the following steps：
（1）Founding：Pd, Ni and Co are added in copper raw material in proportion, continuously draw casting process by vacuum melting and orientation, Obtain a diameter of 6 millimeters of core wires；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 60um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, is mixed in annealing process using nitrogen hydrogen Gas comes as annealing atmosphere, and annealing furnace effective length is 600mm, and annealing temperature is 400 DEG C, annealing rate 60m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Such as 20um）'s Cored wire；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 12 nm, is obtained To plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 18nm, obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and is mixed in annealing process using nitrogen hydrogen It closes gas to come as annealing atmosphere, annealing furnace effective length is 900mm, and annealing temperature is 500 DEG C, annealing rate 100m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 20 DEG C, obtains required thin gold copper line.
Above-mentioned steps（3）And step（7）The nitrogen and hydrogen mixture of use by 5% (volume) H2With the N of 95% (volume)2Group Into.
Above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition is immersed in the acetone ethanol mixed liquor that temperature is 80 DEG C, It is 7 seconds to immerse the time, the organic matter on removing cored wire surface；The weight ratio of acetone and ethyl alcohol is in the acetone ethanol mixed liquor 1:8；
（5-2）Remove oxide process：The cored wire immersion temperature that will be handled by removing organic matter is 80 DEG C, weight percent is dense It spends in the nitric acid for 50%, it is 7 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：It is 80 DEG C, weight percent concentration by temperature is immersed by the cored wire of removing oxide process It is 7 seconds in 10% sulfuric acid, to immerse the time, surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, is plated under conditions of electroplating current is 0.8A Palladium, forms the palladium coating that thickness is 12nm on the surface of cored wire, which coats cored wire；
This step（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, wherein palladium sulfate Concentration is 1g/L, the concentration 2g/L of ammonium chloride, the concentration 3g/L of ammonium sulfate；
（5-5）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife（Air knife air-flow is N2, flow velocity 20L/ min）；
When being electroplated, with the continuous release steps of the speed of 20m/min（4）The cored wire of acquisition, cored wire pass through above-mentioned removing successively After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
Above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 2g/L（The gold plating liquid of use is cyanogen Change golden potassium solution）, it is gold-plated under conditions of electroplating current is 0.8A, the gold that thickness is 18 nm is formed on the surface of plating palladium line Coating, the gold plate coat palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife（Air knife air-flow is N2, flow velocity 20L/ min）；
When being electroplated, with the continuous release steps of the speed of 20m/min（5）The plating palladium line of acquisition, plating palladium line is successively by above-mentioned After gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
Embodiment 4
The thin gold copper line of the present embodiment includes cored wire, the palladium pre-plating layer being coated on outside cored wire and is coated on palladium pre-plating layer The golden clad of outside；The cored wire contains Pd 3%, Ga 10ppm, Al 10ppm, Ca 20ppm by weight, and surplus is Copper；The thickness of the palladium pre-plating layer is 30 nm, and the thickness of golden clad is 2 nm.
The manufacturing method of above-mentioned thin gold copper line comprises the following steps：
（1）Founding：Pd, Ga, Al and Ca are added in copper raw material in proportion, continuously draw foundry work by vacuum melting and orientation Skill obtains a diameter of 6 millimeters of core wires；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 150um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, N is used in annealing process2Come as Annealing atmosphere, annealing furnace effective length are 900mm, and annealing temperature is 500 DEG C, annealing rate 90m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Such as 20um）'s Cored wire；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 30 nm, is obtained To plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 2 nm, obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and N is used in annealing process2To do For annealing atmosphere, annealing furnace effective length is 900mm, and annealing temperature is 500 DEG C, annealing rate 90m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 25 DEG C, obtains required thin gold copper line.
Above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition is immersed in the acetone ethanol mixed liquor that temperature is 120 DEG C, It is 3 seconds to immerse the time, the organic matter on removing cored wire surface；The weight ratio of acetone and ethyl alcohol is in the acetone ethanol mixed liquor 1: 10；
（5-2）Remove oxide process：It is 120 DEG C, weight percent by temperature is immersed by the cored wire of removing organic matter processing Concentration is in 35% nitric acid, and it is 3 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：The cored wire immersion temperature that removing oxide process will be passed through is 120 DEG C, weight percent is dense It spends in the sulfuric acid for 25%, it is 3 seconds to immerse the time, and surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, is plated under conditions of electroplating current is 0.6A Palladium, forms the palladium coating that thickness is 30 nm on the surface of cored wire, which coats cored wire；
This step（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, wherein palladium sulfate Concentration is 3g/L, the concentration 2g/L of ammonium chloride, the concentration 2g/L of ammonium sulfate；
（5-5）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife（Air knife air-flow is N2, flow velocity 15L/ min）；
When being electroplated, with the continuous release steps of the speed of 10m/min（4）The cored wire of acquisition, cored wire pass through above-mentioned removing successively After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
Above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 2.5g/L（The gold plating liquid of use is Potassium auricyanide solution）, it is gold-plated under conditions of electroplating current is 0.7A, the gold that thickness is 2 nm is formed on the surface of plating palladium line Coating, the gold plate coat palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife（Air knife air-flow is N2, flow velocity 15L/ min）；
When being electroplated, with the continuous release steps of the speed of 10m/min（5）The plating palladium line of acquisition, plating palladium line is successively by above-mentioned After gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
Embodiment 5
The thin gold copper line of the present embodiment includes cored wire, the palladium pre-plating layer being coated on outside cored wire and is coated on palladium pre-plating layer The golden clad of outside；The cored wire contains Pd 0.25%, Pt 60ppm, Co 70ppm, Mg 50ppm by weight, and surplus is Copper；The thickness of the palladium pre-plating layer is 2 nm, and the thickness of golden clad is 24 nm.
The manufacturing method of above-mentioned thin gold copper line comprises the following steps：
（1）Founding：Pd, Pt, Co and Mg are added in copper raw material in proportion, continuously draw foundry work by vacuum melting and orientation Skill obtains a diameter of 8 millimeters of core wires；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain a diameter of 180um（Micron）Cored wire；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, is mixed in annealing process using nitrogen hydrogen Gas comes as annealing atmosphere, and annealing furnace effective length is 700mm, and annealing temperature is 450 DEG C, annealing rate 80m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains a diameter of 15-40um（Such as 20um）'s Cored wire；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 2 nm, is obtained To plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface（Gold plate coats palladium coating）, The thickness of gold plate is 24 nm, obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and is mixed in annealing process using nitrogen hydrogen It closes gas to come as annealing atmosphere, annealing furnace effective length is 900mm, and annealing temperature is 500 DEG C, annealing rate 80m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 25 DEG C, obtains required thin gold copper line.
Above-mentioned steps（3）And step（7）The nitrogen and hydrogen mixture of use by 5% (volume) H2With the N of 95% (volume)2Group Into.
Above-mentioned steps（5）In electroplating technology（Plate palladium）Comprise the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition is immersed in acetone ethanol mixed liquor at a temperature of 90 °C, It is 6 seconds to immerse the time, the organic matter on removing cored wire surface；The weight ratio of acetone and ethyl alcohol is in the acetone ethanol mixed liquor 1:6；
（5-2）Remove oxide process：The cored wire immersion temperature that will be handled by removing organic matter is 90 DEG C, weight percent is dense It spends in the nitric acid for 45%, it is 6 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：It is 90 DEG C, weight percent concentration by temperature is immersed by the cored wire of removing oxide process It is 6 seconds in 20% sulfuric acid, to immerse the time, surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, is plated under conditions of electroplating current is 0.5A Palladium, forms the palladium coating that thickness is 2 nm on the surface of cored wire, which coats cored wire；
This step（5-4）In, the plating palladium liquid of use is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, wherein palladium sulfate Concentration is 2g/L, the concentration 1g/L of ammonium chloride, the concentration 4g/L of ammonium sulfate；
（5-5）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife（Air knife air-flow is N2, flow velocity 15L/ min）；
When being electroplated, with the continuous release steps of the speed of 15m/min（4）The cored wire of acquisition, cored wire pass through above-mentioned removing successively After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
Above-mentioned steps（6）In electroplating technology（It is gold-plated）Comprise the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 2.5g/L（The gold plating liquid of use is Potassium auricyanide solution）, gold-plated under conditions of electroplating current is 0.6A, it is 24 nm's that thickness is formed on the surface of plating palladium line Gold plate, the gold plate coat palladium coating；
（6-2）Cleaning：Using pure water as cleaning solution, twice ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife（Air knife air-flow is N2, flow velocity 15L/ min）；
When being electroplated, with the continuous release steps of the speed of 15m/min（5）The plating palladium line of acquisition, plating palladium line is successively by above-mentioned After gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
The thin gold copper line of 1-5 of the embodiment of the present invention is tested for the property, test method and test result are as follows：
1st, hot and humid test method and condition
A. temperature： 85℃；Humidity：85% R.H；
B. the cycle：500 it is small when small (every 24 take out one group of sample and tested)；
C. not encapsulating after routing.
It is respectively 170 to plate the total number of samples amount after palladium gold-plated copper wires and the thin gold copper line routings of embodiment 1-5, is divided into 17 Group, every group of each 10 sample, is placed in hot and humid environment, it is every 24 it is small when take out one group of sample and tested（Carry out electric current pair Voltage curve is tested and the short-circuit test that breaks, to judge whether to fail）, test result is as shown in table 1 below.It is found after being tested： Plating palladium gold-plated copper wires, embodiment 1-5 thin gold copper line routing after sample when 500 is small after still without failing. Test result shows that the ability of the high-temp resisting high-humidity resisting of thin gold copper line is suitable with plating palladium gold-plated copper wires.
Table 1
In table 1, denominator represents every group of sample number, and molecule represents every group of sample fails number.
2nd, two weldering routing operation window
The routing ability of thin gold copper line is as follows；The thin gold copper line routing parameters of embodiment 1-5 meet specification and routing is made Industry window is big（Routing carries out under the protection of nitrogen hydrogen mixeding gas, 50-90 watts of routing power, routing pressure 40-140 newton）； And without apparent aluminium extruded, electrodeless damage during routing.
3rd, hardness test
The hardness test result of the thin gold copper line of 1-5 of the embodiment of the present invention is shown：The thin gold copper line of the present invention has Relatively low wire rod hardness, between 70-90 Hv（The hardness of palladium gold-plated copper wires is plated between 95 ~ 110 Hv）, relatively low line can be played Material camber.
4th, FAB ball-types stability
A.EFO electric currents：60mA
B.N2+H2(gas flow：0.3~0.6 L/min)
The FAB balls of the thin gold copper line of the present invention, stability is identical with plating palladium gold-plated copper wires, is normal ball-type, unbiased Bulbus cordis and abnormal ball.
5、HAZ（Heat affected area）Length
It is as shown in table 2 below to the HAZ length testing results of the thin gold copper line of 1-5 of the embodiment of the present invention.Test result shows, The HAZ length of the thin gold copper line of the present invention plates the HAZ length of palladium gold-plated copper wires in 60-70 between 50-58 um Between um.
Table 2
Embodiment HAZ length（um）
Embodiment 1 50
Embodiment 2 58
Embodiment 3 54
Embodiment 4 52
Embodiment 5 55

Claims (10)

1. a kind of thin gold copper line, it is characterised in that including cored wire, the palladium pre-plating layer being coated on outside cored wire and be coated on Golden clad outside palladium pre-plating layer；The cored wire is by weight containing Pd 0.1-3%, and trace additives 1-300 ppm are remaining It measures as copper；The trace additives are more than one kind or two of which in Ca, In, Co, Be, Ga, Mg, Ce, Ni, Pt and Al Combination；The thickness of the palladium pre-plating layer is 1-40 nm, and the thickness of golden clad is 1-30 nm.
2. thin gold copper line according to claim 1, it is characterised in that：The thickness of the palladium pre-plating layer is 5-15 nm, The thickness of golden clad is 10-20 nm.
3. the manufacturing method of thin gold copper line described in claim 1, it is characterised in that comprise the following steps：
（1）Founding：Pd and trace additives are added in copper raw material in proportion, continuously draw casting by vacuum melting and orientation Technique obtains core wires 6-8 millimeters a diameter of；
（2）Wire drawing：To step（1）Obtained core wires carry out wire drawing, obtain the cored wire of a diameter of 50-280um；
（3）Intermediate annealing：Step（2）After the completion of wire drawing, intermediate annealing is carried out to cored wire, N is used in annealing process2Or nitrogen Hydrogen gaseous mixture comes as annealing atmosphere, and annealing furnace effective length is 600-1000mm, and annealing temperature is 300-600 DEG C, annealing speed Rate is 60-120m/min；
（4）To through step（3）The cored wire of intermediate annealing process continues wire drawing, obtains the cored wire of a diameter of 15-40um；
（5）Using electroplating technology in step（4）Coated with Palladium coating on the cored wire surface of acquisition, the thickness of palladium coating is 1-40 nm, Obtain plating palladium line；
（6）Using electroplating technology in step（5）Gold plate is coated on obtained plating palladium line surface, the thickness of gold plate is 1-30 Nm obtains plating palladium plating gold thread；
（7）Finally anneal：To step（6）Obtained plating palladium plating gold thread is finally annealed, and N is used in annealing process2Or nitrogen Hydrogen gaseous mixture comes as annealing atmosphere, and annealing furnace effective length is 600-1000mm, and annealing temperature is 300-600 DEG C, annealing speed Rate is 60-120m/min；
（8）Cooling：After finally annealing, plating palladium plating gold thread is cooled to 20-30 DEG C, obtains required thin gold copper line.
4. the manufacturing method of thin gold copper line according to claim 3, it is characterised in that：The step（5）In electricity Depositing process comprises the following steps：
（5-1）Remove organic matter processing：By step（4）The cored wire of acquisition immerses the acetone ethanol mixed liquor that temperature is 70-150 DEG C In, it is 1.4-8 seconds to immerse the time, the organic matter on removing cored wire surface；The weight of acetone and ethyl alcohol in the acetone ethanol mixed liquor Amount ratio is 1:5-10；
（5-2）Remove oxide process：It is 70-150 DEG C, weight percent by temperature is immersed by the cored wire of removing organic matter processing Specific concentration is in the nitric acid of 30-50%, and it is 1.4-8 seconds to immerse the time, the oxide on removing cored wire surface；
（5-3）Surface activation process：It is 70-150 DEG C, weight percent by temperature is immersed by the cored wire of removing oxide process Concentration is in the sulfuric acid of 10-30%, and it is 1.4-8 seconds to immerse the time, and surface activation process is carried out to cored wire；
（5-4）Plate palladium：Cored wire Jing Guo surface activation process is immersed in plating palladium liquid, in the condition that electroplating current is 0.2-0.8A Lower plating palladium, forms the palladium coating that thickness is 1-40 nm on the surface of cored wire, which coats cored wire；
（5-5）Cleaning：Using pure water as cleaning solution, ultrasonic cleaning is carried out to the cored wire for being coated with palladium coating；
（5-6）Drying：The water being attached on palladium coating surface is blown away using air knife；
When being electroplated, with the continuous release steps of the speed of 5-30m/min（4）The cored wire of acquisition, cored wire is successively by above-mentioned de- After organic matter processing, removing oxide process, surface activation process, plating palladium, cleaning and drying, plating palladium line and take-up are obtained.
5. the manufacturing method of thin gold copper line according to claim 4, it is characterised in that：The step（5-4）In, it adopts Plating palladium liquid is the mixed solution of palladium sulfate, ammonium chloride and ammonium sulfate, and the wherein concentration of palladium sulfate is 1-4g/L, ammonium chloride Concentration is 1-4g/L, and the concentration of ammonium sulfate is 1-4g/L.
6. the manufacturing method of thin gold copper line according to claim 4, it is characterised in that：The step（5-6）In, wind Knife air-flow is N2, flow velocity 5-20L/min.
7. the manufacturing method of thin gold copper line according to claim 3, it is characterised in that：The step（6）In electricity Depositing process comprises the following steps：
（6-1）It is gold-plated：By step（5）The plating palladium line of acquisition is immersed in the gold plating liquid that concentration is 2-4g/L, is in electroplating current It is gold-plated under conditions of 0.2-0.8A, the gold plate that thickness is 1-30 nm is formed on the surface of plating palladium line, which plates palladium Layer cladding；
（6-2）Cleaning：Using pure water as cleaning solution, ultrasonic cleaning is carried out to the plating palladium line for being coated with gold plate；
（6-3）Drying：The water being attached on gold plate surface is blown away using air knife；
When being electroplated, with the continuous release steps of the speed of 5-30m/min（5）The plating palladium line of acquisition, plating palladium line is successively by upper After stating gold-plated, cleaning and drying, plating palladium plating gold thread and take-up are obtained.
8. the manufacturing method of thin gold copper line according to claim 7, it is characterised in that：The step（6-1）In, it adopts Gold plating liquid is potassium auricyanide solution.
9. the manufacturing method of thin gold copper line according to claim 7, it is characterised in that：The step（6-3）In, wind Knife air-flow is N2, flow velocity 5-20L/min.
10. the manufacturing method of thin gold copper line according to claim 3, it is characterised in that：The step（3）And step （7）The nitrogen and hydrogen mixture of use by 5% (volume) H2With the N of 95% (volume)2Composition.
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CN109637993A (en) * 2018-11-22 2019-04-16 汕头市骏码凯撒有限公司 The coated copper bonding wire in surface and its manufacturing method
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CN109457143A (en) * 2018-10-30 2019-03-12 深圳粤通应用材料有限公司 A kind of pure nickel plating palladium high-temperature electric conduction silk and preparation method thereof
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