CN1949492A - Bonded copper wire and preparing method thereof - Google Patents
Bonded copper wire and preparing method thereof Download PDFInfo
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- CN1949492A CN1949492A CNA2006101544855A CN200610154485A CN1949492A CN 1949492 A CN1949492 A CN 1949492A CN A2006101544855 A CNA2006101544855 A CN A2006101544855A CN 200610154485 A CN200610154485 A CN 200610154485A CN 1949492 A CN1949492 A CN 1949492A
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Abstract
The invention relates to a bonding copper wire and the preparing method thereof. And it comprises: Ca 0.0005-0.001wt%, Ce or Ti 0.0003-0.0007wt% and Cu the rest >or=99.996wt%. And its preparing method comprises the steps of: a. providing copper material; b. electro-refining and obtaining refined copper with 99.999wt% purity; c. making monorystalline horizontal metal casting and obtaining monocrystalline copper with 99.9999wt% purity; d. making intermediate alloy; e. adding in the made monocrystalline copper and intermediate alloy to make monocrystalline horizontal metal casting and making boned copper wire blank; f. stretching; g. annealing; h. split-coiling; and i. vacuum packaging. And it has better mechanical properties and oxidation resistance, assuring smooth packaging and bonding course.
Description
Technical field
The present invention relates to a kind of bonding brass wire and preparation method thereof.
Background technology
Domestic existing semiconductor package lead bonding material especially is mainly used in the bonding wire in integrated circuit and the semi-conductor discrete device, mainly is to use spun gold, and its chemical property is stable.But, because its material price of gold lattice costliness, make manufacturing cost high, in addition, along with the integrated circuit scale is increasing, packaging density is more and more higher, require need have higher intensity, low long arc degree, arc stability etc. as the bonding wire of lead, and bonding gold wire has been difficult to satisfy high like this requirement.
At present, the bonding brass wire of existing part import brand begins that partly integrated encapsulation factory enters the suitable stage in the China's Mainland, the bonding brass wire of these import brands can satisfy the requirement of modern bonding technology basically, but in use still there are a lot of problems, such as making the bonding operation frequently interrupt because copper purity is lower in the product, product second solder joint that causes really up to the mark is escaped silk (also being the silk that contracts); Because the high oxidation characteristic of product; after unpacking, must use in 10 hours; and must add nitrogen hydrogen mixeding gas protected when using; make that disperse has inflammable and explosive property gas and dangerous increasing around the production scene, install exhaust system additional and make condition such as its temperature humidity not reach standard-required etc. far away again.Therefore owing to above defective, the bonding brass wire of these import brands does not obtain high volume applications so far yet, especially at integrated circuit connection.
Summary of the invention
The purpose of this invention is to provide a kind of bonding brass wire; this bonding brass wire is with low cost; have mechanical performance and antioxygenic property preferably; avoided second solder joint to escape silk; guaranteed smooth encapsulation bonding process; especially in bonding process, can remove dangerous protective gas-hydrogen, and only use high pure nitrogen can well finish bonding process.
Another object of the present invention provides a kind of preparation method of described bonding brass wire.
A kind of bonding brass wire of the present invention, its material prescription percentage by weight is: calcium 0.0005～0.001%, cerium or titanium 0.0003～0.0007%, surplus is a copper, the content of copper 〉=99.996%.
Bonding brass wire metallographic structure of the present invention is a mono-crystalline structures.
The selection of the material prescription composition of described bonding brass wire is that calcium (Ca) mainly is the breaking load that improves bonding brass wire, and suitably reduces the camber of bonding brass wire.Cerium (Ce) mainly is a fatigue resistance of improving material, improve material surface oxidation-resistant.Titanium (Ti) also has good non-oxidizability except the mechanical strength that can improve material.In addition, calcium (Ca) and cerium (Ce), the acting in conjunction of calcium (Ca) and titanium (Ti) is to form solid solution with copper, improves the mechanical strength of bonding brass wire in the mode of solid solution reinforcement; Calcium (Ca) adds the combination of cerium (Ce) or the combination that calcium (Ca) adds titanium (Ti), has all improved the surface oxidation-resistant of material, has improved the weldability of material, therefore can avoid second solder joint to escape silk preferably.More than the common advantage of several elements be to improve the material application performance, but can not influence the conductivity of bonding brass wire, resistivity can not increase.
For metal material, purity is big more usually, and its oxidation resistance is just strong more.Bonding brass wire silk material longitudinal tissue structure metallographic is a mono-crystalline structures, can effectively reduce resistivity, the raising conductivity of material, further strengthens antioxidation.
The preparation method of the bonding brass wire that the present invention adopts, its procedure comprises: a. provides copper product, b. electrorefining gets the purification copper of 99.999wt%, and c. metal single crystal horizontal casting obtains the single crystal Cu of 99.9999wt%, and d. makes intermediate alloy, e. single crystal Cu and the intermediate alloy that makes by described bonding brass wire material prescription adition process c and d carries out the metal single crystal horizontal casting, make the bonding brass wire blank, f. stretches, g. annealing, h. bundling, the i. vacuum packaging; Wherein, Faradaic current 0.5～3A, 40～60 ℃ of electrolyte temperatures; Metal single crystal horizontal casting temperature is 1100～1250 ℃, and casting speed is 10～20mm/min, and 10
-2Carry out under the Pa vacuum degree; Intermediate alloy comprises copper-calcium intermediate alloy, copper-cerium or copper-titanium intermediate alloy, and its manufacture method is: the single crystal Cu of c step is provided, and calcium or cerium or titanium feed intake, 10
-4Melting 15～20min under the Pa vacuum degree, casting, pickling; Calcium or cerium or the titanium percentage by weight in copper is 0.53～0.57% in the described intermediate alloy; Annealing temperature is 320～510 ℃, and carries out in 99.999% high pure nitrogen protection.
Make calcium or cerium or titanium material purity 〉=99.99wt% in the intermediate alloy step, be the market sell goods.Described intermediate alloy smelting temperature is 1215～1245 ℃, and under this temperature, the intermediate alloy metal material melts fully.
Mould elongation in the described drawing process is 5～18%.
The wrapping wire tension force of described bundling process is 5～30g, and wire winding speed is 500～750rpm.
It is the disclosed method of patent application of CN 1810416A (open day is 2006.08.02) that described metal single crystal horizontal continuous casting method adopts publication number; Make when feeding intake at described intermediate alloy, calcium or cerium or titanium are placed in the middle of the single crystal Cu.
Compared with prior art, the advantage of bonding brass wire of the present invention is: 1. have good oxidization resistance, product still can normally use opening in vacuum-packed back 15 days.2. safe and reliable, successfully removed hydrogen shield gas and only kept nitrogen as burning ball protection gas.3. the cost of material is low, has outstanding mechanical performance, hardness and welding performance, can not produce second solder joint and escape a problem, can substitute common bonding gold wire fully.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.Below listed designing requirement system specification requirement is formulated according to external like product standard and with reference to domestic correspondent.
Embodiment 1
Electrorefining copper: copper product that will electrolysis melts (adding vacuum protection) in intermediate frequency furnace after; be cast into 150mm * 60mm * 10mm rectangular blocks and bore the hole of 5mm diameter as anode top; (platinized platinum, size are generally 150mm * 60mm * 0.5mm) get ready to cathode sheets.In electrolysis tank, add copper-bath (analyzing the alcohol level) and, the anode blister cake is hung on the electrolysis tank upper left side by contact rod, guarantee that 95% volume of each anode block immerses in the electrolyte, the anode conducting rod is received on the positive pole of rectifier power source as electrolyte; Cathode sheets is hung on the electrolysis tank upper right side by contact rod, guarantees that 95% volume of each cathode sheets immerses in the electrolyte, cathode collector bar is received on the negative pole of rectifier power source.Open rectifier power source, regulate about direct voltage to 0.6～0.7V, about electric current 2-2.5A, the beginning electrolysis, the control electrolyte temperature is adjusted temperature to replenish new electrolyte between 40～60 ℃, when treating that the purification copper (99.999wt%) that adsorbs on the cathode sheets reaches about 1 kilogram of left and right sides, change cathode sheets, purification copper is rinsed out the acid on surface earlier with high purity water (resistivity 10～15M Ω), after using watery hydrochloric acid (5～10wt% concentration) treatment surface impurity again, again rinse well with high purity water, dry up with clean compressed air again.
The single crystal Cu of preparation 99.9999wt%: the continuous casting chamber of a horizontal casting metal single crystal in argon gas atmosphere is provided, behind the purification copper of adding 99.999wt%, is evacuated to 10
-2Pa carries out heating in medium frequency and melting under 1100～1250 ℃.After finishing fusing, refining and degasification, molten metal is injected into the middle liquid storage tank of continuous casting chamber, the horizontal continuous casting of single crystal of molten metal is finished in insulation in keeping the continuous casting chamber of 2～5 liters of/minute purification of argon flows, obtain the single crystal Cu of 99.9999wt%.
The preparation intermediate alloy: purity is that the single crystal Cu of 99.9999wt% is got (2000 ± 0.5 gram) ready, and element calcium (purity 99.99wt%) weighing 11 ± 0.5 grams are got ready.The percentage by weight of calcium in copper is 0.55 ± 0.02%.Earlier 100 gram high purity coppers are put into the silica crucible bottom, more load weighted calcium is put into this part copper above, again remaining high purity copper is placed on calcium above, build bell, vacuumize, when vacuum degree reaches 0.1 * 10
-3Begin to heat and note observing the fusing situation of material during Pa, when temperature in the stove during at 1215～1245 ℃, metal melts fully, keep this temperature, refining 15～20 minutes, treat calcium constituent fully mix observe simultaneously begin after metallic solution begins to bleach the casting, rotating crucible is slowly injected graphite casting die with metal liquid carefully, stops heating after casting finishes, keep vacuum, cool down fully in stove, the intermediate alloy of making is taken out in blow-on, alloy surface is handled clean with watery hydrochloric acid, with clean compressed air alloy surface is dried up after rinsing out surperficial diluted acid with high purity water again, obtain copper-calcium intermediate alloy.
Prepare copper-cerium intermediate alloy with quadrat method.
Preparation bonding brass wire blank: the continuous casting chamber that a horizontal casting metal single crystal in argon gas atmosphere is provided, add 0.024kg copper-calcium intermediate alloy, 0.018kg copper-cerium intermediate alloy, the single crystal Cu of 19.958kg99.9999wt%, be evacuated to 10-2Pa, carry out heating in medium frequency and melting under 1100～1250 ℃.After finishing fusing, refining and degasification, molten metal is injected into the middle liquid storage tank of continuous casting chamber, be incubated, finish the horizontal continuous casting of single crystal of molten metal in keeping the continuous casting chamber of 2～5 liters of/minute purification of argon flows, obtaining specification is the bonding brass wire blank of Ф 8mm.
Stretching and annealing process are: Ф 8mm → Ф 1.5mm, mould elongation 18%, draw speed 5～30m/min, annealing, pickling; Ф 1.5mm → Ф 0.1mm, mould elongation 12%, draw speed 100～240m/min, annealing, pickling; Ф 0.1mm → Ф 0.08mm, mould elongation 9%, draw speed 200～360m/min, annealing, pickling; Ф 0.08mm → Ф 0.015mm, mould elongation 6%, draw speed 6～15m/s, annealing, pickling.Annealing temperature all is 320～510 ℃, and all is to carry out in 99.999% high pure nitrogen protection.
Bundling: with 500 meters be a monovolume length, control wrapping wire tension force is 5～30g, wire winding speed is 500～750rpm.
Vacuum-packed: as to adopt bread and cheese level vacuum degree packing.
The performance test parameter of the product of this gained bonding brass wire is listed in table 1.
Embodiment 2
Repeat the method for embodiment 1 by each constituent content of appointment in the following table 1, but replace cerium, in table 1, listed the performance test parameter with titanium.
Embodiment 3
Press the method for each constituent content repetition embodiment 1 of appointment in the following table 2, in table 2, listed the performance test parameter.
Embodiment 4
Press the method for each constituent content repetition embodiment 2 of appointment in the following table 2, in table 2, listed the performance test parameter.
Embodiment 5
Press the method for each constituent content repetition embodiment 1 of appointment in the following table 3, in table 3, listed the performance test parameter.
Embodiment 6
Press the method for each constituent content repetition embodiment 2 of appointment in the following table 3, in table 3, listed the performance test parameter.
Table 1
| Designing requirement | Formula for a product constituent content (percentage by weight) | ||
| Embodiment 1: calcium 0.00065%+ cerium 0.0005%, surplus are copper | Embodiment 2: calcium 0.00065%+ titanium 0.0005%, surplus are copper | ||
| Tensile strength | ＞200N/mm 2(MPa) | 222.3N/mm 2(MPa) | 228.1N/mm 2(MPa) |
| Yield strength | ＞120N/mm 2(MPa) | 146.9N/mm 2(MPa) | 150.3N/mm 2(MPa) |
| Wire rod hardness | 100±10HV 0.01 | 108HV 0.01 | 110HV 0.01 |
| Copper ball hardness | 60-80HV 0.01 | 60-75HV 0.01 | 63-75HV 0.01 |
| Resistivity | ＜1.700×10 -8Ωm | 1.666-1.689×10 -8Ωm | 1.665-1.689×10 -8Ωm |
| Blowout current | The maximum 8.0A of minimum 0.45A | The maximum 8.73A of minimum 0.37A | The maximum 8.68A of minimum 0.39A |
| The camber scope | 120-220μm | 115-225μm | 115-225μm |
| The arc length scope | Maximum 275mil | Maximum 280mil | Maximum 285mil |
Table 2
| Designing requirement | Formula for a product constituent content (percentage by weight) | ||
| Embodiment 3: calcium 0.0005%+ cerium 0.0007%, surplus are copper | Embodiment 4: calcium 0.0005%+ titanium 0.0007%, surplus are copper | ||
| Tensile strength sigma b | ＞200N/mm 2(MPa) | 218.83N/mm 2(MPa) | 223.15N/mm 2(MPa) |
| Yield strength σ s | ＞120N/mm 2(MPa) | 155.2N/mm 2(MPa) | 152.7N/mm 2(MPa) |
| Wire rod hardness | 100±10HV 0.01 | 112HV 0.01 | 124HV 0.01 |
| Copper ball hardness | 60-80HV 0.01 | 58-73HV 0.01 | 60-78HV 0.01 |
| Resistivity | ＜1.700×10 -8Ωm | 1.672-1.680×10 -8Ωm | 1.681-1.691×10 -8Ωm |
| Blowout current | The maximum 8.0A of minimum 0.45A | The maximum 8.63A of minimum 0.41A | The maximum 8.92A of minimum 0.39A |
| The camber scope | 120-220μm | 110-222μm | 110-220μm |
| The arc length scope | Maximum 275mil | Maximum 282mil | Maximum 290mil |
Table 3
| Designing requirement | Formula for a product constituent content (percentage by weight) | ||
| Embodiment 5: calcium 0.0009%+ cerium 0.0003%, surplus are copper | Embodiment 6: calcium 0.0009%+ titanium 0.0003%, surplus are copper | ||
| Tensile strength sigma b | ＞200N/mm 2(MPa) | 225.01N/mm 2(MPa) | 230.22N/mm 2(MPa) |
| Yield strength σ s | ＞120N/mm 2(MPa) | 160.3N/mm 2(MPa) | 158.6N/mm 2(MPa) |
| Wire rod hardness | 100±10HV 0.01 | 111HV 0.01 | 121HV 0.01 |
| Copper ball hardness | 60-80HV 0.01 | 66-76HV 0.01 | 66-79HV 0.01 |
| Resistivity | ＜1.700×10 -8Ωm | 1.667-1.688×10 -8Ωm | 1.669-1.689×10 -8Ωm |
| Blowout current | The maximum 8.0A of minimum 0.45A | The maximum 8.68A of minimum 0.43A | The maximum 8.95A of minimum 0.42A |
| The camber scope | 120-220μm | 115-228μm | 115-230μμm |
| The arc length scope | Maximum 275mil | Maximum 288mil | Maximum 293mil |
Annotate: 1). in the blowout current data, minimum value, its p-wire footpath Ф 18 μ m, line length 10mm.
Maximum, its p-wire footpath Ф 50 μ m, line length 0.6mm.
2). during the wire rod hardness test, the elongation of wire rod is 4.5-6.5%.
3). during resistivity measurement, gauge or diameter of wire is 0.2mm, and length is 1 meter, and wire rod is the full annealing state.
4). during the tensile strength test, the elongation of wire rod is 4.5-6.5%.
The performance test parameter of table 1,2,3 each embodiment illustrates that all bonding brass wire of the present invention can reach designing requirement.
More than the final products of 6 embodiment through bonding test, all reached client's specification requirement fully, solved a problem of escaping of second solder joint, and successfully removed hydrogen shield gas and only kept nitrogen as burning ball protection gas; The surface oxidation-resistant test, in opening vacuum-packed back 15 days of product, product still can normally be used.
Claims (7)
1, a kind of bonding brass wire, its material prescription percentage by weight is: calcium 0.0005～0.001%, cerium or titanium 0.0003～0.0007%, surplus is a copper, the content of copper 〉=99.996%.
2, bonding brass wire according to claim 1 is characterized in that described bonding brass wire metallographic structure is a mono-crystalline structures.
3, a kind of preparation method of bonding brass wire, its procedure comprises: a. provides copper product, b. electrorefining gets the purification copper of 99.999wt%, and c. metal single crystal horizontal casting obtains the single crystal Cu of 99.9999wt%, and d. makes intermediate alloy, e. single crystal Cu and the intermediate alloy that makes by described bonding brass wire material prescription adition process c and d carries out the metal single crystal horizontal casting, make the bonding brass wire blank, f. stretches, g. annealing, h. bundling, the i. vacuum packaging; Wherein, Faradaic current 0.5～3A, 40～60 ℃ of electrolyte temperatures; Metal single crystal horizontal casting temperature is 1100～1250 ℃, and casting speed is 10～20mm/min, and carries out under 10-2Pa vacuum degree; Intermediate alloy comprises copper-calcium intermediate alloy, copper-cerium or copper-titanium intermediate alloy, and its manufacture method is: the single crystal Cu of c step is provided, and calcium or cerium or titanium feed intake, 10
-4Melting 15～20min under the Pa vacuum degree, casting, pickling; Calcium or cerium or the titanium percentage by weight in copper is 0.53～0.57% in the described intermediate alloy; Annealing temperature is 320～510 ℃, and carries out in 99.999% high pure nitrogen protection.
4, the preparation method of bonding brass wire according to claim 3 is characterized in that calcium or cerium or titanium material purity 〉=99.99wt% in the described making intermediate alloy step.
5,, it is characterized in that the smelting temperature in the described making intermediate alloy step is 1215～1245 ℃ according to the preparation method of claim 3 or 4 described bonding brass wires.
6, the preparation method of bonding brass wire according to claim 3 is characterized in that the mould elongation in the described drawing process is 5～18%.
7, the preparation method of bonding brass wire according to claim 3, the wrapping wire tension force that it is characterized in that described bundling process is 5～30g, wire winding speed is 500～750rpm.
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