CN103608910A - Copper strand for bonding wire and method for producing copper strand for bonding wire - Google Patents
Copper strand for bonding wire and method for producing copper strand for bonding wire Download PDFInfo
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- CN103608910A CN103608910A CN201280028930.7A CN201280028930A CN103608910A CN 103608910 A CN103608910 A CN 103608910A CN 201280028930 A CN201280028930 A CN 201280028930A CN 103608910 A CN103608910 A CN 103608910A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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Abstract
This copper strand for a bonding wire is a copper strand for forming a bonding wire having a wire diameter of 180 [mu]m or less. The strand diameter of the copper strand is between 0.15 and 3.0 mm. The copper strand is formed from one or more additional elements selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti, and rare earth elements such that the total content is within a range between 0.0001 and 0.01 mass%, and copper and inevitable impurities as the balance. The copper strand has a specific grain boundary ratio (L[sigma]/L), which is the ratio of the length of a specific grain boundary L[sigma] to the total length L of the crystal grain boundary, that is 50% or greater as determined by EBSD.
Description
Technical field
The present invention relates to a kind of closing line using when wire diameter is the closing line below 180 μ m that produces and with copper wires and closing line, use the manufacture method of copper wires.
The application advocates based on July 22nd, 2011 in the priority of No. 2011-161036, the Japanese patent application of Japanese publication, and its content is applied to this.
Background technology
Conventionally, be equipped with in the semiconductor device of semiconductor element, by above-mentioned closing line, connect semiconductor element and lead-in wire.In the past, as closing line, from viewpoints such as stringiness and conductivity, mainly used Au line.Yet Au is expensive, the closing line that therefore instead this Au line is used, provides Cu closing line processed.
At this, compare with Au, therefore Cu is harder, exists the sphere that is formed at line front end can destroy the risk of the Al distribution tunicle that is for example formed at Si semiconductor component surfaces while engaging.And, to compare with Au, the percentage elongation of Cu is lower, therefore has the problem of the wire loop shape that cannot remain suitable.
For this reason, for example in patent documentation 1,2, proposing there is the purity utilized is the Cu closing line processed of ultrahigh-purity coppers (6NCu) more than 99.9999 quality %.In addition, in patent documentation 3, propose have indium addition to have the Cu closing line processed of Ti, Zr, Hf, V, Cr and B.
But, as recorded in patent documentation 1,2, while utilizing purity to be ultrahigh-purity coppers (6NCu) more than 99.9999 quality %, in order to obtain ultrahigh-purity copper (6NCu), need to carry out purification processes operation.Therefore the problem that, exists manufacturing cost significantly to increase.
In addition, in the closing line of recording in patent documentation 3, compare still hard and percentage elongation is also lower with Au.Therefore,, as the substitute product of Au line, characteristic is also insufficient.
And in recent years, the graph thinning of the closing line that requirement consists of Cu line, for closing line copper wires, also required can not occur the processability of broken string.
Patent documentation 1: Japanese kokai publication sho 62-111455 communique
Patent documentation 2: Japanese kokai publication hei 04-247630 communique
Patent documentation 3: Japanese Patent Publication 04-012623 communique
Summary of the invention
The present invention completes in view of afore-mentioned, its object be to provide a kind of hardness is lower and percentage elongation is higher and also the closing line of excellent in workability with copper wires and closing line the manufacture method by copper wires.
In order to solve above-mentioned problem, the related closing line of a mode of the present invention is to be used to form the copper wires that wire diameter is the closing line below 180 μ m by copper wires, wherein, gauge or diameter of wire is below the above 3.0mm of 0.15mm, and there is following composition, with total scope below 0.01 quality % more than 0.0001 quality %, contain and be selected from Mg, Ca, Sr, Ba, Ra, Zr, the interpolation element of more than one in Ti and rare earth element, and surplus is copper and inevitable impurity, and special grain boundary ratio (L σ/L) is more than 50%, described special grain boundary ratio is that the length L σ of the special grain boundary measured with EBSD method is with respect to the ratio of the length L of whole crystal boundaries.
This closing line is with in copper wires, there is following composition, to amount to more than the 0.0001 quality % scope below 0.01 quality %, contain more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element, and surplus is copper and inevitable impurity.Therefore the S and the above-mentioned element reaction that, are contained in copper form compound.Thus, the impact of S reduces, and can reduce recrystallization temperature, and can reduce hardness.
And special grain boundary ratio (L σ/L) is more than 50%, described special grain boundary ratio is that the length L σ of the special grain boundary measured with EBSD method is with respect to the ratio of the length L of whole crystal boundaries.Therefore, can improve percentage elongation and processability lower in the situation that hardness is maintained.
In addition, by utilizing an EBSD determinator for emission-type scanning electron microscopy, crystal boundary, special grain boundary are carried out specific, calculate the length L of whole crystal boundaries and the length L σ of special grain boundary.By these length, can obtain the special grain boundary ratio (L σ/L) in the manner.
Crystal boundary is defined as follows, the result of observing through two-dimensional section, and the misorientation between two adjacent crystallizations becomes 15 ° of borders between this crystallization when above.
In addition, special grain boundary is defined as, and meets corresponding crystal boundary (the Coincidence-Site Lattice of 3≤Σ≤29 in crystallography according to the Σ value of CSL theoretical (Kronberg et al:Trans.Met.Soc.AIME, 185,501 (1949)) definition; CSL), the intrinsic corresponding position crystal lattice orientation defect Dq and in this correspondence crystal boundary meets Dq≤15 °/Σ
1/2the crystal boundary of (D.G.Brandon:Acta.Metallurgica.Vol.14, p.1479, (1966)).
The related closing line of a mode of the present invention is with in copper wires, the adding up to below the above 0.002 quality % of 0.0003 quality % of the content of preferred described interpolation element.
Now, recrystallization temperature can be suppressed reliably for lower, and can reduce hardness.
And the content that preferably described inevitable impurity is Fe, Pb and S is, Fe is below 0.0001 quality %, and Pb is below 0.0001 quality %, and S is below 0.005 quality %.
By stipulating as described above the content of impurity, recrystallization temperature can be suppressed reliably for lower, and can reduce hardness.
The particle diameter preferably closing line described in 100g being obtained in salpeter solution by copper wires heating for dissolving is that the numbers that is not dissolved in sour residue thing more than 30 μ m is below 1000.
Now, be present in closing line less and number is less with the particle diameter of the sour residue thing of being not dissolved in of copper wires inside.Therefore the broken string producing in the time of, can being suppressed at the Wire Drawing while manufacturing closing line.
The amount that is not dissolved in sour residue thing preferably described closing line being obtained in salpeter solution by copper wires heating for dissolving is below 0.00015 quality %.
Now, be present in the ratio less that exists of the sour residue thing of being not dissolved in of copper wires inside for closing line.Therefore the broken string producing in the time of, can being suppressed at the Wire Drawing while manufacturing closing line.
The related closing line of a mode of the present invention is the manufacture method of copper wires for described closing line by the manufacture method of copper wires, possess and have: copper motlten metal generates operation, in the copper raw material more than purity is 99.99 quality % below 99.998 quality %, add more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element and generate copper motlten metal; Continuous casting operation, produces ingot bar continuously by described copper feeding molten metal to belt wheel continuous casting machine; And continuous rolling operation, in initial temperature, be the ingot bar of continuous rolling manufacturing under more than 800 ℃ conditions.
Manufacture method according to this closing line by copper wires, utilizing purity is the copper raw material of the so-called 4NCu below the above 99.998 quality % of 99.99 quality %.Therefore, compare when utilizing 6NCu, can significantly reduce the manufacturing cost of copper wires for closing line.
And, possess that to have in initial temperature be the continuous rolling operation of the ingot bar of continuous rolling manufacturing under more than 800 ℃ conditions.Therefore, the special grain boundary ratio in copper wires (L σ/L) for closing line can be made as more than 50%.
In addition, the related closing line of other modes of the present invention is the manufacture method of copper wires for described closing line by the manufacture method of copper wires, possess and have: copper motlten metal generates operation, in the copper raw material more than purity is 99.99 quality % below 99.998 quality %, add more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element and generate copper motlten metal; Casting process, injects mold by described copper motlten metal and produces ingot bar; Extrusion process, is, under more than 800 ℃ conditions, resulting ingot bar is carried out to extrusion process in initial temperature, thereby produces extruding wire rod; Processing/annealing operation, for resulting extruding wire rod, repeatedly implements any in rolling processing or Wire Drawing and anneals; And light rolling process, with rolling rate, more than 5% below 25%, be rolled, making final wire diameter is below the above 3.0mm of 0.15mm.
Manufacture method according to this closing line by copper wires, utilizing purity is the copper raw material of the so-called 4NCu below the above 99.998 quality % of 99.99 quality %.Therefore, compare when utilizing 6NCu, can significantly reduce the manufacturing cost of copper wires for closing line.
And, possess and have: processing/annealing operation, for extruding wire rod, repeatedly implement any in rolling processing or Wire Drawing and anneal; And light rolling process, with rolling rate, more than 5% below 25%, be rolled, making final wire diameter is below the above 3.0mm of 0.15mm.Therefore, the special grain boundary ratio in copper wires (L σ/L) for closing line can be made as more than 50%.
According to a mode of the present invention, can provide that a kind of hardness is lower and percentage elongation is higher and also the closing line of excellent in workability with copper wires and closing line the manufacture method by copper wires.
Accompanying drawing explanation
Fig. 1 manufactures the key diagram that one embodiment of the present invention is the continuous casting rolling device that uses during by copper wires of closing line.
Fig. 2 is that one embodiment of the present invention is the flow chart of the manufacture method of copper wires for closing line.
Fig. 3 is that another embodiment of the present invention is the flow chart of the manufacture method of copper wires for closing line.
Fig. 4 means the chart of the evaluation result that is not dissolved in sour residue thing in the inventive example 1.
Embodiment
Below, the related closing line of one embodiment of the present invention is described by the manufacture method of copper wires with copper wires and closing line.
The related closing line of present embodiment is below 180 μ m by copper wires as manufacturing wire diameter, raw material when more preferably wire diameter is the closing line below the above 180 μ m of 20 μ m.
In addition, the related closing line of present embodiment is below the above 3.0mm of 0.15mm with the gauge or diameter of wire of copper wires.
This closing line has following composition by copper wires, to amount to more than the 0.0001 quality % scope below 0.01 quality %, contain more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element, and surplus is copper and inevitable impurity.Be preferably selected from more than one the adding up to below the above 0.002 quality % of 0.0003 quality % of content of interpolation element in Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element.
And the content that described inevitable impurity is Fe, Pb and S is, Fe is below 0.0001 quality %, and Pb is below 0.0001 quality %, and S is below 0.005 quality %.
Wherein, rare earth element is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
This closing line is more than 50% with the special grain boundary ratio (L σ/L) of copper wires.Wherein, the length L σ that special grain boundary ratio is special grain boundary is with respect to the ratio of the length L of whole crystal boundaries.By utilizing an EBSD determinator for emission-type scanning electron microscopy, crystal boundary, special grain boundary are carried out specific, calculate the length L of whole crystal boundaries and the length L σ of special grain boundary.The length calculating from this can obtain special grain boundary ratio.That is, as the closing line of present embodiment, use in copper wires, special grain boundary exists more than general crystal boundary.
Crystal boundary is defined as follows, the result of observing through two-dimensional section, and the misorientation between two adjacent crystallizations becomes 15 ° of borders between this crystallization when above.
In addition, special grain boundary is defined as, in crystallography according to theoretical (the Kronberg et al:Trans.Met.Soc.AIME of CSL, 185,501 (1949)) the corresponding crystal boundary of satisfied 3≤Σ≤29 of the Σ value of definition, and the intrinsic corresponding position crystal lattice orientation defect Dq in this correspondence crystal boundary meets Dq≤15 °/Σ
1/2the crystal boundary of (D.G.Brandon:Acta.Metallurgica.Vol.14, p.1479, (1966)).
In addition, using the closing line as present embodiment of 100g, with the particle diameter that copper wires heating for dissolving obtains in salpeter solution, be that the more than 30 μ m number that is not dissolved in sour residue thing is below 1000.And the above-mentioned ratio that exists that is not dissolved in sour residue thing is below 0.00015 quality %.
Implement to be not dissolved in the following order the evaluation of sour residue thing.
First, from the sample test portion of scheduled volume (100g) of copper wires for the closing line of clean surface, heating for dissolving is in the salpeter solution having heated.Lysate is cooled to after room temperature, with filter, filters, thus trapping residue thing.
To trapping the filter of residue thing, weigh, measure the residue quality of residue thing.And, calculate the amount (residue quality) of residue thing with respect to the ratio (quality %) of the amount of test portion (closing line copper wires).By more than, measure the amount (having ratio) that is not dissolved in sour residue thing that closing line is obtained in salpeter solution by copper wires heating for dissolving.
Then, by scanning electron microscope, observe the filter that traps residue thing, take SEM photo.SEM photo is carried out to graphical analysis, measure size and the number of residue thing.And obtaining particle diameter is the number of residue things more than 30 μ m.By more than, measuring the particle diameter that 100g closing line is obtained in salpeter solution by copper wires heating for dissolving is the numbers that is not dissolved in sour residue thing more than 30 μ m.
Then, the closing line as present embodiment is described by the manufacture method of copper wires.
The special grain boundary overall length L σ of special grain boundary is that more than 50% closing line is manufactured by the extruding method of continuous casting milling method or ingot bar by copper wires with respect to the ratio (L σ/L) of the crystal boundary overall length L of crystal boundary.
In present embodiment, to utilize the example of the continuous casting rolling device 10 shown in Fig. 1 to describe.
Continuous casting rolling device 10 shown in Fig. 1 has melting furnace 11, keeps stove 12, casts conduit 13, belt wheel continuous casting machine 30, continuous rolling device 15 and up-coiler 18.
In present embodiment, utilize the shaft furnace with cylindrical furnace main body as melting furnace 11.In the bottom of furnace main body, a plurality of burners (omit diagram) to circumferencial direction be equipped with and up and down direction with multistage shape, be equipped with.And, from the top charging feedstock of furnace main body, be cathode copper.Cathode copper melts by the burning of described burner, continuously manufactured copper motlten metal.
Keeping stove 12, to the fine copper motlten metal of manufacturing in melting furnace 11, under the state keeping with predetermined temperature, temporarily accumulate, and the copper motlten metal of constant basis is delivered to casting conduit 13.
The element that is provided with the copper motlten metal interpolation element to being transferred in funnel 20 adds member 21.And the flow direction end side of the copper motlten metal of funnel 20 disposes pouring nozzle 22.Copper motlten metal in funnel 20 is supplied to belt wheel continuous casting machine 30 via this pouring nozzle 22.
Belt wheel continuous casting machine 30 has outer peripheral face and is formed with the cast wheel 31 of groove and carries out around mobile endless belt 32 in the mode that the part of the outer peripheral face with this cast wheel 31 contacts.To be formed at space between described groove and endless belt 32 inject the copper motlten metal of supplying with via pouring nozzle 22 and carry out cooling, thereby cast bar-shaped ingot bar 40 continuously.
And this belt wheel continuous casting machine 30 is linked to continuous rolling device 15.The bar-shaped ingot bar 40 that these continuous rolling device 15 continuous rollings produce from belt wheel continuous casting machine 30, thus produce the copper cash base 50 of predetermined outer diameter.The copper cash base 50 producing from continuous rolling device 15 is wound onto up-coiler 18 via cleaning cooling device 16 and crack detector 17.
Then, utilize Fig. 1, Fig. 2 to utilizing the closing line of this belt wheel continuous casting machine 30 to describe by the manufacture method of copper wires.
First, to melting furnace 11, dropping into purity is more than 99.99 quality % copper raw material below 99.998 quality % (so-called 4NCu) melt to obtain copper motlten metal (melting operation S01).This melts in operation S01, and the air-fuel ratio of adjusting a plurality of burners of shaft furnace makes the inside of melting furnace 11 become reducing atmosphere.
The copper motlten metal obtaining by melting furnace 11 is via keeping stove 12 and casting conduit 13 to be transferred to funnel 20.
Wherein, by being stirred by aforementioned agitating member by the copper motlten metal of the casting conduit 13 of inert gas or reducibility gas sealing.Thus, promote reacting of copper motlten metal and inert gas or reducing gas.
Then, by element, add member (device) 21 and be selected from more than one the element (element add operation S02) in Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element to the copper motlten metal continuous adding in funnel 20.Thus, more than one the content of element that generation is selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element is adjusted into add up to below the above 0.01 quality % of 0.0001 quality %, more preferably the copper motlten metal below the above 0.002 quality % of 0.0003 quality %.
The copper motlten metal of so adjusted composition is supplied to belt wheel continuous casting machine 30 via pouring nozzle 22, produces continuously bar-shaped ingot bar 40(continuous casting operation S03).Wherein, in continuous casting operation S03, be formed at the groove of cast wheel 31 and the space between endless belt 32 and be trapezoidal.Therefore producing cross section is roughly trapezoidal bar-shaped ingot bar 40.
This bar-shaped ingot bar 40 is supplied to continuous rolling device 15 and imposes the processing of rolling system, thereby produces the copper cash base 50(continuous rolling operation S04 of predetermined outer diameter (being diameter 8mm in present embodiment)).In this continuous rolling operation S04, the scopes of 400～900 ℃, implement rolling.In present embodiment, the initial temperature of rolling is made as more than 800 ℃.The initial temperature of rolling is preferably 800 ℃ above below 1050 ℃.
The copper cash base 50 producing from continuous rolling device 15 is wound in up-coiler 18 via cleaning cooling device 16 and crack detector 17.Cleaning cooling device 16 cleans the surface of the copper cash base 50 producing from continuous rolling device 15 and carries out cooling with cleaning agents such as alcohol.And crack detector 17 is surveyed from cleaning the damage of the copper cash base 50 of cooling device 16 conveyings.
Then, resulting copper cash base 50 is implemented to Wire Drawing, making final wire diameter is the above 3.0mm of 0.15mm following (being diameter 0.9mm in present embodiment) (Wire Drawing operation S05).
And, after above-mentioned Wire Drawing operation S05, with 150 ℃ above 250 ℃, carry out below recrystallization heat treatment (final heat treatment step S06).In present embodiment, with 220 ℃ of atmosphere heat treatments of implementing 2 hours.
By as above step, produce the closing line copper wires as present embodiment.
As the closing line copper wires of present embodiment, further implementing stretch process and become diameter is the fine rule below 180 μ m, as closing line.
According to the closing line copper wires with the present embodiment of this feature, there is following composition, to amount to more than the 0.0001 quality % scope below 0.01 quality %, contain more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element, and surplus is copper and inevitable impurity.More preferably the content of above-mentioned interpolation element adds up to below the above 0.002 quality % of 0.0003 quality %.Therefore the S and the above-mentioned interpolation element that, are contained in copper form compound.Therefore, the impact of S reduces, so can reduce recrystallization temperature and reduce hardness.
And, as the closing line of present embodiment, with the special grain boundary ratio (L σ/L) of copper wires, be more than 50%.In addition, by utilizing an EBSD determinator for emission-type scanning electron microscopy, crystal boundary, special grain boundary are carried out specific, calculate the length L of whole crystal boundaries and the length L σ of special grain boundary.And the length calculating from this can obtain special grain boundary ratio.The matching degree of the crystal boundary of this special grain boundary ratio compare Gao Shi， organized whole is improved, and is difficult to accumulate dislocation.Therefore, can improve percentage elongation and processability lower in the situation that hardness is maintained.
In addition, using the closing line as present embodiment of 100g, with the particle diameter that copper wires heating for dissolving obtains in salpeter solution, be that the more than 30 μ m number that is not dissolved in sour residue thing is below 1000.And the amount (having ratio) that is not dissolved in sour residue thing is below 0.00015 quality %.
So, be not dissolved in that the particle diameter of sour residue thing is less and number is less, and it exists ratio to be also suppressed.Therefore, can be suppressed at broken string when closing line is become to closing line by copper wires Wire Drawing.
In addition, the manufacture method according to the closing line as present embodiment by copper wires, using purity is the copper raw material of the so-called 4NCu below the above 99.998 quality % of 99.99 quality %.Therefore, compare when utilizing 6NCu, can significantly reduce the manufacturing cost of copper wires for closing line.
And possessing has the continuous casting operation S03 that utilizes belt wheel continuous casting machine 30 to produce continuously bar-shaped ingot bar 40 and is the continuous rolling operation S04 of the bar-shaped ingot bar 40 of continuous rolling manufacturing under more than 800 ℃ conditions in initial temperature.Therefore, the closing line of manufacturing can be made as more than 50% with the special grain boundary ratio (L σ/L) of copper wires.
Above, embodiments of the present invention are illustrated, but the invention is not restricted to this, in the scope that does not depart from technological thought of the present invention, can suitably change.
In present embodiment, utilize belt wheel continuous casting machine to manufacture closing line and be illustrated by copper wires, but be not limited to this.
For example, as shown in Figure 3, also can produce special grain boundary ratio (L σ/L) by enforcement copper motlten metal generation operation S11, casting process S12, hot extrusion operation S13, processing/annealing operation S14 and light rolling process S15 is more than 50% closing line copper wires.
Copper motlten metal generates in operation S11, and more than one the interpolation unit that in the copper raw material more than purity is 99.99 quality % below 99.998 quality % (so-called 4NCu), interpolation is selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element usually obtains copper motlten metal.
In casting process S12, copper poured with molten metal is obtained to the ingot bar that diameter is 200mm～400mm to mold.
In hot extrusion operation S13, in initial temperature, be that under more than 800 ℃ conditions, extrusion process ingot bar obtains pushing wire rod.More than the initial temperature of extrusion process is preferably 800 ℃, below 1050 ℃.
In processing/annealing operation S14, extruding wire rod is repeatedly implemented any in rolling processing or Wire Drawing and annealed.Whenever becoming 80%, cross section slip implements annealing when above.
In light rolling process S15, with rolling rate, more than 5% below 25%, be rolled, making final wire diameter is below the above 3.0mm of 0.15mm.
Embodiment
(embodiment 1)
Below, the result for the aforesaid evaluation test of evaluating by copper wires as the closing line of present embodiment is described.
By the method shown in the flow chart of Fig. 2, produce the closing line copper wires of the inventive example 1～5 and comparative example 1,2.Specifically the interpolation unit, recording in interpolation table 1 in 4NCu usually obtains copper motlten metal.By copper poured with molten metal to belt wheel continuous casting machine and cast rolling continuously.Further implement Wire Drawing and final heat treatment, thereby produce the closing line copper wires that diameter is 0.9mm.
By the method shown in the flow chart of Fig. 3, produce the closing line copper wires of the inventive example 6～10 and comparative example 3,4.Specifically the interpolation unit, recording in interpolation table 1 in 4NCu usually obtains copper motlten metal.Utilize copper motlten metal to produce the ingot bar that diameter is 240mm.The 800 ℃ of hot extrusions of take are processed this ingot bar and are produced the extruding wire rod that diameter is 8mm.This extruding wire rod is rolled and anneals to produce the copper wires that wire diameter is 1mm repeatedly.Afterwards, this copper wires is implemented the rolling of rolling rate 10%.Then, carry out final heat treatment with 220 ℃, thereby produce the closing line copper wires that diameter is 0.9mm.
Produce by the following method the closing line copper wires of conventional example.First, the Zr that adds 0.0030 quality % at 4NCu obtains copper motlten metal.Utilize copper motlten metal to produce the ingot bar that diameter is 240mm.The 800 ℃ of hot extrusions of take are processed this ingot bar and are produced the extruding wire rod that diameter is 8mm.This extruding wire rod is implemented to Wire Drawing.Then, carry out final heat treatment with 220 ℃, thereby produce the closing line copper wires that diameter is 0.9mm.
In addition, the closing line of the resulting inventive example 1～10, comparative example 1～4 and conventional example is implemented to Wire Drawing by copper wires and produce the closing line that diameter is 180 μ m.
(special grain boundary ratio)
Closing line copper wires to the resulting inventive example 1～10, comparative example 1～4 and conventional example, measures special grain boundary ratio (L σ/L) by the following method.
To each test portion, utilize waterproof abrasive paper and diamond abrasive to carry out mechanical lapping.Then, utilize cataloid solution to carry out smooth grinding.
And, by EBSB determinator (S4300-SEM processed of HITACHI company, the OIM Data processed Collection of EDAX/TSL company) and analysis software (the OIM Data processed Analysis ver.5.2 of EDAX/TSL company), crystal boundary, special grain boundary are carried out specific, calculate the length L of whole crystal boundaries and the length L σ of special grain boundary.Average thus the analysis of crystallization particle diameter and special grain boundary length ratio.The detailed content of assay method is below shown.
First, utilize scanning electron microscope to irradiate electron ray to each measuring point in the measurement range on test portion surface, make electron ray two-dimensional scan to test portion surface.By utilizing the orientation analysis of Electron Back-Scattered Diffraction, the misorientation between adjacent measuring point becomes between 15 ° of above measuring points as crystal boundary.
To the crystal boundary overall length of the crystal boundary in measurement range (all length of crystal boundary), L measures.And, determine that adjacent crystal grain boundary is the crystal boundary position of special grain boundary, and measure crystal boundary overall length (length of all special grain boundaries) the L σ of special grain boundary.And, obtain ratio L σ/L of the crystal boundary overall length L of the crystal boundary that the length L σ of special grain boundary goes out with respect to said determination, and be made as special grain boundary ratio (L σ/L).
(hardness test)
Then,, to copper wires and the closing line that produced by copper wires by these closing lines for the closing line of the inventive example 1～10, comparative example 1～4 and conventional example, measure hardness.
In addition, hardness test is utilized AKASHI micro-vickers hardness testing machine processed MVK-700 and is implemented according to JIS Z2241.
(percentage elongation)
Then,, to copper wires and the closing line that produced by copper wires by these closing lines for the closing line of the inventive example 1～10, comparative example 1～4 and conventional example, utilize AKASHI AMSLER formula processed longitudinal type cupping machine implement tension test and evaluate percentage elongation.
(processability)
The closing line of the resulting inventive example 1～10, comparative example 1～4 and conventional example is further implemented to Wire Drawing by copper wires and make the line that diameter is 87 μ m, 50 μ m or 20 μ m.Broken string number of times while evaluating Wire Drawing.
The result that shown in table 1, the broken string number of times during by special grain boundary ratio (L σ/L), hardness and the percentage elongation of wire rod, the hardness of closing line and percentage elongation and Wire Drawing is evaluated to closing line.
In the inventive example 1～10, confirming special grain boundary ratio (L σ/L) becomes more than 50%.On the other hand, in comparative example 1～4 and conventional example, special grain boundary ratio (L σ/L) is less than 50%.If the contrast inventive example 6～10 and conventional example, can confirm, by implement the processing of rolling rate 10% before implementing final heat treatment to having the wire rod of final wire diameter, can increase special grain boundary ratio (L σ/L).
Special grain boundary ratio (L σ/L) is in more than 50% inventive example 1～10, and confirming in wire diameter is that under the state of closing line of 180 μ m, hardness is low to moderate below 40Hv.
And confirm, compare with comparative example, in the inventive example 1～10, broken string during wire drawing is suppressed, can the extremely thin footpath of wire drawing.
(embodiment 2)
Then, utilize the closing line of the inventive example 1～10 with copper wires evaluation, to be not dissolved in level of residue and the particle size distribution of sour residue thing.
With nitric acid, test portion is carried out to etch processes, remove and be attached to surperficial impurity.Then, take the test portion of 100g.By this test portion heating for dissolving in salpeter solution.Heating-up temperature is made as 60 ℃.Repeatedly carry out this operation.
Then, be cooled to room temperature, and filter to trap residue with filter.
At this, utilize polycarbonate filter (aperture is 0.4 μ m) to filter.In clean room, critically weigh the polycarbonate filter that has trapped residue thing, measure the residue quality of residue thing.
And, measure the particle size distribution that is not dissolved in sour residue thing.Described in observing by scanning electron microscope, trap the filter of residue thing, and taken SEM image.Image is read in to computer, with software for graphical analysis (WinRoof software), image is carried out to the analysis of binary conversion treatment.And the projected area of mensuration residue thing, calculates the diameter of a circle (equivalent circle diameter) with the area identical with this projected area.Particle diameter by this equivalent circle diameter as residue thing.Measure size (equivalent circle diameter) and the number of residue thing.In addition, the data by the inventive example 1 make particle size distribution chart.The results are shown in Fig. 4.
The graphical analysis results verification of WinRoof software arrives, and by the test portion of the inventive example of 100g 1～10 (closing line copper wires) heating for dissolving, when the salpeter solution, particle diameter is that the numbers that is not dissolved in sour residue thing more than 30 μ m is below 1000.And the results verification of measuring the residue quality of residue thing with said method arrives, the mass ratio that is not dissolved in sour residue thing in the test portion of the inventive example 1～10 is below 0.00015 quality %.
Utilizability in industry
The closing line of present embodiment is lower and percentage elongation is higher by the hardness of copper wires, and excellent in workability.Therefore, the copper wires of present embodiment can be applicable to being applicable to replacing the manufacturing process of the Cu closing line that Au line uses.
Symbol description
30-belt wheel continuous casting machine.
Claims (7)
1. a closing line copper wires, it is to be used to form the copper wires that wire diameter is the closing line below 180 μ m, it is characterized in that,
Gauge or diameter of wire is below the above 3.0mm of 0.15mm,
And there is following composition, to amount to more than the 0.0001 quality % scope below 0.01 quality %, contain more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element, and surplus is copper and inevitable impurity,
Special grain boundary ratio L σ/L is more than 50%, and described special grain boundary ratio is that the length L σ of the special grain boundary measured with EBSD method is with respect to the ratio of the length L of whole crystal boundaries.
2. closing line copper wires according to claim 1, is characterized in that,
Adding up to below the above 0.002 quality % of 0.0003 quality % of the content of described interpolation element.
3. closing line copper wires according to claim 1 and 2, is characterized in that,
The content that described inevitable impurity is Fe, Pb and S is, Fe is below 0.0001 quality %, and Pb is that the following and S of 0.0001 quality % is below 0.005 quality %.
4. according to the closing line copper wires described in any one in claim 1～3, it is characterized in that,
The particle diameter that closing line described in 100g is obtained in salpeter solution by copper wires heating for dissolving is that the numbers that is not dissolved in sour residue thing more than 30 μ m is below 1000.
5. according to the closing line copper wires described in any one in claim 1～4, it is characterized in that,
The amount that is not dissolved in sour residue thing that described closing line is obtained in salpeter solution by copper wires heating for dissolving is below 0.00015 quality %.
6. a manufacture method for copper wires for closing line, is characterized in that, it is the manufacture method that in claim 1～5, the closing line described in any one is used copper wires, possesses:
Copper motlten metal generates operation, adds more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element and generate copper motlten metal in the copper raw material more than purity is 99.99 quality % below 99.998 quality %;
Continuous casting operation, produces ingot bar continuously by described copper feeding molten metal to belt wheel continuous casting machine; And
Continuous rolling operation is the ingot bar of continuous rolling manufacturing under more than 800 ℃ conditions in initial temperature.
7. a manufacture method for copper wires for closing line, is characterized in that, it is the manufacture method that in claim 1～5, the closing line described in any one is used copper wires, possesses:
Copper motlten metal generates operation, and the copper raw material more than purity is 99.99 quality % below 99.998 quality % adds more than one the interpolation element being selected from Mg, Ca, Sr, Ba, Ra, Zr, Ti and rare earth element and generates copper motlten metal;
Casting process, injects mold by described copper motlten metal and produces ingot bar;
Extrusion process, is, under more than 800 ℃ conditions, resulting ingot bar is carried out to extrusion process in initial temperature, thereby produces extruding wire rod;
Processing and annealing operation, for resulting extruding wire rod, repeatedly implement any in rolling processing or Wire Drawing and anneal; And
Light rolling process, more than 5% is rolled below 25% with rolling rate, and making final wire diameter is below the above 3.0mm of 0.15mm.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2011161036 | 2011-07-22 | ||
| JP2011-161036 | 2011-07-22 | ||
| PCT/JP2012/068090 WO2013015154A1 (en) | 2011-07-22 | 2012-07-17 | Copper strand for bonding wire and method for producing copper strand for bonding wire |
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| CN103608910A true CN103608910A (en) | 2014-02-26 |
| CN103608910B CN103608910B (en) | 2016-03-02 |
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| JP (1) | JP5344070B2 (en) |
| KR (1) | KR101926215B1 (en) |
| CN (1) | CN103608910B (en) |
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| CN106119597A (en) * | 2016-08-30 | 2016-11-16 | 芜湖楚江合金铜材有限公司 | The different in nature copper wires of a kind of environment-friendly and high-performance and processing technique thereof |
| CN106947881A (en) * | 2017-05-05 | 2017-07-14 | 三门峡宏鑫有色金属有限公司 | Multielement rare earth high conductivity Cu alloy material and preparation method thereof |
| CN108603251A (en) * | 2016-04-06 | 2018-09-28 | 三菱综合材料株式会社 | superconducting line and superconducting coil |
| CN111279002A (en) * | 2017-10-30 | 2020-06-12 | 三菱综合材料株式会社 | Superconducting stabilizing material, superconducting wire, and superconducting coil |
| CN111656501A (en) * | 2018-01-30 | 2020-09-11 | 拓自达电线株式会社 | Bonding wire |
| CN111661953A (en) * | 2020-06-16 | 2020-09-15 | 包头稀土研究院 | Method for separating fluorine and phosphorus in mixed rare earth alkaline wastewater and application |
| US10964453B2 (en) | 2015-01-07 | 2021-03-30 | Mitsubishi Materials Corporation | Superconducting stabilization material, superconducting wire, and superconducting coil |
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| JP6175932B2 (en) * | 2013-06-24 | 2017-08-09 | 三菱マテリアル株式会社 | Drawing copper wire, drawing copper wire manufacturing method and cable |
| KR101519075B1 (en) * | 2013-12-03 | 2015-05-21 | (주)신동 | Electromagnetic wave shielding Fe-Cu wire, rod and Manufacturing method for the same |
| JP2022103567A (en) | 2020-12-28 | 2022-07-08 | 日立金属株式会社 | Rough drawing wire production method and rough drawing wire production device |
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- 2012-07-17 MY MYPI2014700100A patent/MY171026A/en unknown
- 2012-07-17 WO PCT/JP2012/068090 patent/WO2013015154A1/en active Application Filing
- 2012-07-18 TW TW101125791A patent/TWI586448B/en active
- 2012-07-20 JP JP2012161473A patent/JP5344070B2/en active Active
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| US10964453B2 (en) | 2015-01-07 | 2021-03-30 | Mitsubishi Materials Corporation | Superconducting stabilization material, superconducting wire, and superconducting coil |
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| US10971278B2 (en) | 2016-04-06 | 2021-04-06 | Mitsubishi Materials Corporation | Superconducting wire and superconducting coil |
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| CN106947881A (en) * | 2017-05-05 | 2017-07-14 | 三门峡宏鑫有色金属有限公司 | Multielement rare earth high conductivity Cu alloy material and preparation method thereof |
| CN111279002A (en) * | 2017-10-30 | 2020-06-12 | 三菱综合材料株式会社 | Superconducting stabilizing material, superconducting wire, and superconducting coil |
| TWI775976B (en) * | 2017-10-30 | 2022-09-01 | 日商三菱綜合材料股份有限公司 | Superconductivity stabilizing material, superconducting wire, and superconducting coil |
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| US11613794B2 (en) | 2017-10-30 | 2023-03-28 | Mitsubishi Materials Corporation | Superconductivity stabilizing material, superconducting wire and superconducting coil |
| CN111656501A (en) * | 2018-01-30 | 2020-09-11 | 拓自达电线株式会社 | Bonding wire |
| CN111661953A (en) * | 2020-06-16 | 2020-09-15 | 包头稀土研究院 | Method for separating fluorine and phosphorus in mixed rare earth alkaline wastewater and application |
Also Published As
| Publication number | Publication date |
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| MY171026A (en) | 2019-09-23 |
| JP2013048225A (en) | 2013-03-07 |
| CN103608910B (en) | 2016-03-02 |
| JP5344070B2 (en) | 2013-11-20 |
| KR20140050630A (en) | 2014-04-29 |
| WO2013015154A1 (en) | 2013-01-31 |
| TWI586448B (en) | 2017-06-11 |
| TW201323104A (en) | 2013-06-16 |
| KR101926215B1 (en) | 2018-12-06 |
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