CN103031464B - 铜接合线 - Google Patents
铜接合线 Download PDFInfo
- Publication number
- CN103031464B CN103031464B CN201210252443.0A CN201210252443A CN103031464B CN 103031464 B CN103031464 B CN 103031464B CN 201210252443 A CN201210252443 A CN 201210252443A CN 103031464 B CN103031464 B CN 103031464B
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- China
- Prior art keywords
- copper
- bonding wire
- quality ppm
- wire
- soft
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010949 copper Substances 0.000 title claims abstract description 153
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 150
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000000956 alloy Substances 0.000 claims abstract description 36
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 25
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 9
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 30
- 229910052760 oxygen Inorganic materials 0.000 claims description 30
- 239000001301 oxygen Substances 0.000 claims description 30
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 25
- 239000005864 Sulphur Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 abstract description 24
- 239000012535 impurity Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 description 142
- 239000010410 layer Substances 0.000 description 48
- 238000000137 annealing Methods 0.000 description 44
- 239000010936 titanium Substances 0.000 description 33
- 238000004519 manufacturing process Methods 0.000 description 28
- 239000013078 crystal Substances 0.000 description 19
- 238000005096 rolling process Methods 0.000 description 17
- 239000002245 particle Substances 0.000 description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 13
- 238000005491 wire drawing Methods 0.000 description 13
- 238000005098 hot rolling Methods 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 230000006378 damage Effects 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 229910000881 Cu alloy Inorganic materials 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000004020 conductor Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000010931 gold Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000013081 microcrystal Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 239000007859 condensation product Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 206010021143 Hypoxia Diseases 0.000 description 3
- 230000006399 behavior Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005097 cold rolling Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 208000018875 hypoxemia Diseases 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000009749 continuous casting Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 241001124569 Lycaenidae Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000014987 copper Nutrition 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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Abstract
本发明的目的是提供具有高抗拉强度、伸长,并且硬度小的铜接合线。作为解决本发明课题的方法涉及一种铜接合线,其特征在于,由软质低浓度铜合金材料构成,所述软质低浓度铜合金材料包含选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素且其余部分为铜和不可避免的杂质,所述铜接合线的晶体组织从至少表面向内部直至线径的20%的深度为止的平均晶粒尺寸为20μm以下。
Description
技术领域
本发明涉及具有高抗拉强度、伸长率,并且硬度小的新的铜接合线。
背景技术
一直以来,在将半导体元件的电极与外部引线连接的接合线中,使用了Au线或Al合金线。特别是,在树脂模类型的半导体元件中,从连接可靠性的观点出发,使用了φ0.025mm左右的Au线。此外,近年来,作为汽车用功率模块的接合线,使用了φ0.3mm左右的Al线。
Au线具有优异的导电性、耐蚀性、软质性,另一方面成本非常高。因此,提出了将铜(Cu)作为原材料的接合线。
专利文献1中已知通过电解精炼和区域熔炼法(zone melting法)而高纯度化成纯度99.999质量%以上的接合用铜细线。
专利文献2中显示了一种铜接合线,其使用反复纯化而使不可避免的杂质为10ppm以下的无氧铜,由包含选自由Ti、Zr、Hf、V、Cr、Mn和B所组成的组中的添加元素且其余部分为铜的铜合金构成,热轧、冷轧后,利用200~300℃、1~2秒的光亮热处理而制造成直径25μm。
专利文献3中显示了Hv为41.1~49.5的铜接合线,其使用反复纯化而使不可避免的杂质为10ppm以下的无氧铜,由包含选自由Mg、Ca、Be、Ge和Si所组成的组中的添加元素且其余部分为铜的铜合金构成,热轧、冷轧后,利用200~300℃、1~2秒的光亮热处理而制造成直径25μm。
专利文献4~7中显示了使用反复纯化而使不可避免的杂质为5ppm以下或10ppm以下的无氧铜,由包含选自由S、Se、Te、Ag所组成的组中的添加元素且其余部分为铜的铜合金构成,热轧、冷轧后,专利文献4中利用250~350℃、0.5~1.5秒的光亮热处理而制造成直径25μm的铜接合线,专利文献5中利用300~400℃、1~2秒的光亮热处理而制造成直径25μm的铜接合线,专利文献6中利用300~400℃、1~2秒的光亮热处理而制造成直径25μm的铜接合线,专利文献7中利用250~380℃、1.5秒的光亮热处理而制造成直径25μm的铜接合线。
专利文献8中显示了一种半导体集成电路元件配线用接合线,其在纯度99.99质量%以上且小于99.999质量%的铜芯材上以整体的30~70体积%被覆有99.999质量%以上的铜。
现有技术文献
专利文献
专利文献1:日本特开昭60-244054号公报
专利文献2:日本特开昭61-259558号公报
专利文献3:日本特开昭61-258463号公报
专利文献4:日本特开昭62-22469号公报
专利文献5:日本特开昭61-224443号公报
专利文献6:日本特开昭62-2645号公报
专利文献7:日本特开昭62-94969号公报
专利文献8:日本特开昭63-236338号公报
发明内容
发明要解决的课题
专利文献1中的由纯度99.99质量%水平的OFC构成的接合线由比Au硬的Cu构成,因此如果使用该接合线,例如,与半导体元件(作为一例,硅芯片)上设置的作为电极焊盘的铝焊盘接合,则对铝焊盘带来破坏。
为了减少对铝焊盘的破坏,如果对铝焊盘施加过剩的热能使得OFC进一步软质化,则由于接合线的硬度与接合线的伸长、抗拉强度处于消长的关系,因此虽然接合线的硬度减少,但同时接合线的伸长降低,此外,随着接合线的晶体组织(尺寸)粗大化,抗拉强度也降低。
即,如果接合线的伸长降低,则接合线本身的变形能力降低,因此有可能由于由线接合后树脂密封之后接合线与密封树脂材的热膨胀差所产生的应力而损害接合线与接合对象物之间的连接可靠性,并且有可能从线轴向接合部供给线时易于发生所谓线卷曲等卷曲行为,操作特性降低。
此外,另一方面,如果接合线的抗拉强度降低,则在进行接合的情况下,有时在接合时形成的熔融球的正上部(球颈部)的接合线发生强度降低,导致断裂。此外如果接合线的抗拉强度降低,则有可能在反复经受温度循环时,由于上述的接合线与密封树脂材的热膨胀差而导致接合线断裂。即,作为接合线的疲劳特性降低。
为了解决这样的问题,专利文献2、3中,通过在99.999质量%以上的高纯度铜中添加微量(1~10ppm)的添加元素,在专利文献4~7中,通过在99.999质量%以上的高纯度铜中添加微量(几ppm)的添加元素,从而调整接合线的伸长率、抗拉强度和接合线的原材料的硬度的平衡的尝试部分地进行了,但对于将该导体原材料进行拉丝加工和退火处理后的导体本身而言,其硬度小,无法实现维持软质的特性并且兼备高伸长特性和抗拉强度的铜导体,仍有改善的余地。
另外,专利文献8中,与专利文献1同样地为由纯度99.99质量%水平的OFC构成的接合线,如果与半导体元件上设置的作为电极焊盘的铝焊盘接合,则对铝焊盘带来破坏。
本发明的目的是提供比无氧铜低成本,而且具有高导电性、抗拉强度和伸长率,并且硬度小的铜接合线。
用于解决课题的方法
本发明涉及一种铜接合线,其特征在于,是由软质低浓度铜合金材料构成的铜接合线,所述软质低浓度铜合金材料包含选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素且其余部分为铜,所述铜接合线的晶体组织从其表面向内部直至线径的20%的深度为止的平均晶粒尺寸为20μm以下。
此外,本发明的铜接合线优选包含2质量ppm以上12质量ppm以下的硫、超过2质量ppm且为30质量ppm以下的氧、和4质量ppm以上55质量ppm以下的钛。
此外,本发明的铜接合线优选具有与实施了退火处理的无氧铜线相同或其以下的硬度,并且,伸长率的值的平均值具有比无氧铜线高1%以上的伸长率的值。
此外,优选具有与实施了上述退火处理的无氧铜线相同或其以上的抗拉强度,并且,硬度的值具有比无氧铜线低2Hv以上的值。
此外,本发明的铜接合线优选电导率为98%IACS以上,硫(S)和钛(Ti)作为TiO、TiO2、TiS或具有Ti-O-S结合的化合物、或者TiO、TiO2、TiS或具有Ti-O-S结合的化合物的凝聚物被包含,其余部分的Ti和S作为固溶体被包含。
此外,优选上述TiO、TiO2、TiS、Ti-O-S的形式的化合物或凝聚物分布在晶粒内,TiO具有200nm以下的尺寸,TiO2具有1000nm以下的尺寸,TiS具有200nm以下的尺寸,Ti-O-S的形式的化合物或凝聚物具有300nm以下的尺寸,500nm以下的粒子为90%以上。
本发明的铜接合线可以通过下述制造方法来制造,所述制造方法包括以下工序:将包含选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素的软质低浓度铜合金材料在1100℃以上1320℃以下的熔铜温度制成熔液的熔液制造工序;由上述熔液制作盘条(wire rod)的盘条制作工序;在880℃以下550℃以上的温度对上述盘条实施热轧的热轧工序;以及对经过上述热轧工序的上述盘条实施拉丝加工的拉丝加工工序。
本发明的铜接合线的制造方法中,优选上述添加元素为4质量ppm以上55质量ppm以下的Ti,上述软质低浓度铜合金材料包含2质量ppm以上12质量ppm以下的硫、和超过2质量ppm且为30质量ppm以下的氧。
本发明的铜接合线的制造方法中,优选上述软质低浓度铜合金材料的软化温度以φ2.6mm的尺寸为130℃以上148℃以下。
(铜接合线的构成)
(1)关于添加元素
本发明涉及将包含选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素且其余部分为铜和不可避免的杂质的软质低浓度铜合金材料进行拉丝加工,接着实施退火处理而成的铜接合线。
作为添加元素,选择选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的元素的理由是,这些元素为易于与其它元素结合的活性元素,特别是易于与S结合,因此可以捕集S,可以将基体的铜母材高纯度化,使原材料的硬度降低。此外,通过捕集S,还可获得可以实现高导电性这样的效果。添加元素包含1种或2种以上。此外,合金中也可以含有不会对合金的性质带来不良影响的其它元素和杂质。
(2)关于组成比率
作为添加元素,Ti、Ca、V、Ni、Mn和Cr的1种或2种以上的合计含量为4~55质量ppm,更优选为10~20质量ppm,Mg的含量为2~30质量ppm,更优选为5~10质量ppm,Zr、Nb的含量为8~100质量ppm,更优选为20~40质量ppm。
此外,在后述的优选实施方式中,氧含量超过2质量ppm且为30质量ppm以下是良好的,更优选为5~15质量ppm,可以根据添加元素的添加量和S的含量,在具备合金的性质的范围内,包含超过2质量ppm且为400质量ppm以下。
S的含量为2~12质量ppm,更优选为3~8质量ppm。
本发明的铜接合线,例如,从汽车等中使用的功率模块的小型化、和/或供给至功率模块的电流的电流密度增大的观点出发,将作为热导率比铝高的材料的铜作为主成分而构成。
例如,本发明的铜接合线使用作为满足电导率为98%IACS(万国标准软铜(International Anneld Copper Standard),将电阻率1.7241×10-8Ωm设为100%的情况下的电导率)以上、优选为100%IACS以上、更优选为102%IACS以上的软质型铜材的软质低浓度铜合金材料来构成。
在获得电导率为98%IACS以上的软质铜材的情况下,以作为基础原材料的包含不可避免的杂质的纯铜作为基础,使用包含3~12质量ppm的硫、超过2质量ppm且为30质量ppm以下的氧、和4~55质量ppm的钛的软质低浓度铜合金材料,由该软质低浓度铜合金材料来制造盘条(线坯)。
这里,在获得电导率为100%IACS以上的软质铜材的情况下,以作为基础原材料的包含不可避免的杂质的纯铜为基础,使用包含2~12质量ppm的硫、超过2质量ppm且为30质量ppm以下的氧、和4~37质量ppm的钛的软质低浓度铜合金材料。
此外,在获得电导率为102%IACS以上的软质铜材的情况下,以作为基础原材料的包含不可避免的杂质的纯铜为基础,使用包含3~12质量ppm的硫、超过2质量ppm且为30质量ppm以下的氧、和4~25质量ppm的钛的软质低浓度铜合金材料。
通常,在纯铜的工业制造中,在制造电解铜时硫进入铜中,因此难以使硫为3质量ppm以下。通用电解铜的硫浓度的上限为12质量ppm。
由于本发明的铜接合线优选含有超过2质量ppm且为30质量ppm以下的氧,因此在该实施方式中,将所谓低氧铜(LOC)作为对象。
在氧浓度低于2质量ppm的情况下,由于铜接合线的硬度不易降低,因此将氧浓度控制为超过2质量ppm的量。此外,在氧浓度高于30质量ppm的情况下,由于在热轧工序中在铜接合线的表面上易于产生损伤,因此将氧浓度控制为30质量ppm以下。
(3)关于铜接合线的晶体组织
本发明的铜接合线中,晶体组织从铜接合线的至少表面向铜接合线的内部直至线径的20%的深度为止的平均晶粒尺寸为20μm以下。优选地,表层的平均晶粒尺寸为5~15μm,其内部的平均晶粒尺寸为50~100μm。
这是因为,通过在表层上存在平均晶粒尺寸为20μm以下的微细晶粒,从而可以期待材料的抗拉强度、伸长的提高。作为其理由,认为是由于拉伸变形而导入到晶界附近的局部应变,晶体粒径变小至微细程度,促进晶界应力集中的缓和,与此相伴,晶界应力集中降低,抑制晶界断裂。
此外,本发明中,只要具有晶体组织从铜接合线的至少表面向铜接合线的内部直至线径的20%的深度为止的平均晶粒尺寸为20μm以下的本发明的效果,就不排除在超过线径的20%的深度而更接近线材的中心部的区域存在微细晶体层的形态。
(4)关于分散的物质
优选铜接合线内分散的分散粒子的尺寸小,此外,优选在铜接合线内分散粒子大量地分散。其理由是,分散粒子具有作为硫的析出位点的功能,作为析出位点,要求尺寸小、数目多。
具体而言,铜接合线所包含的硫、特别是作为添加元素的钛作为TiO、TiO2、TiS或具有Ti-O-S结合的化合物、或者TiO、TiO2、TiS或具有Ti-O-S结合的化合物的凝聚物被包含,其余部分的Ti和S作为固溶体被包含。另外,关于其它添加元素也与钛同样。
分散粒子的形成以及硫在分散粒子中的析出使铜母材的基体的纯度提高,促进材料硬度的降低。
(5)关于铜接合线的硬度、伸长率和抗拉强度
对于本发明的铜接合线用的材料,要求硬度与伸长率、抗拉强度的平衡优异。作为其理由,是因为如果线或线前端所形成的球硬,则对作为接合焊盘的Al配线膜或其下的Si半导体芯片带来破坏。此外,其原因是,如果线本身的抗拉强度、伸长率小,则难以保持适当的线环,或接合时易于发生断线不良等。
通常,由于硬度(柔软性)与伸长(的高低)、抗拉强度(的高低)形成消长的关系,因此期望平衡好地兼备这些特性。
此外,本发明的铜接合线具有与实施了退火处理的无氧铜线相同或其以下的硬度,并且,伸长率的值的平均值具有比无氧铜线高1%以上的伸长率的值。这里所谓硬度,是指材料的维氏硬度。
此外,本发明的铜接合线具有与实施了退火处理的无氧铜线相同或其以上的抗拉强度,并且,硬度的值具有比无氧铜线低2Hv以上的值。
(铜接合线的制造方法)
本发明的铜接合线的制造方法如下所述。作为例子,对添加元素选择Ti的情况进行说明。
首先,准备作为铜接合线的原料的包含Ti的软质低浓度铜合金材料(原料准备工序)。接着,将该软质低浓度铜合金材料在1100℃以上1320℃以下的熔铜温度制成熔液(熔液制造工序)。接着,由熔液制作盘条(盘条制作工序)。接着,在880℃以下550℃以上的温度对盘条实施热轧(热轧工序)。然后,对经过热轧工序的盘条实施拉丝加工和热处理(拉丝加工、热处理工序)。作为热处理方法,可以应用使用了管状炉的移动退火、利用了电阻发热的通电退火等。此外,还能够为间歇式的退火。通过这些工序来制造本发明的铜接合线。
此外,铜接合线的制造中,优选包含2质量ppm以上12质量ppm以下的硫、超过2质量ppm且为30质量ppm以下的氧、和4质量ppm以上55质量ppm以下的钛的软质低浓度铜合金材料。
因此,本发明人为了实现铜接合线的硬度的降低,研究了以下两个对策。进而,通过在铜盘条的制造中合并使用以下两个对策,从而获得了本发明的铜接合线。
首先,第1对策是,在氧浓度超过2质量ppm的量的Cu中添加了钛(Ti)的状态下,制作软质低浓度铜合金材料的熔液。认为在该熔液中,形成了TiS、钛的氧化物(例如,TiO2)和Ti-O-S粒子。
接着,第2对策是,以通过在软质低浓度铜合金材料中导入位错而使硫(S)的析出容易为目的,将热轧工序中的温度设定为比通常的铜的制造条件下的温度(即,950℃~600℃)低的温度(880℃~550℃)。通过这样的温度设定,可以使S在位错上析出或将钛的氧化物(例如,TiO2)作为核使S析出。
通过以上的第1对策和第2对策而使软质低浓度铜合金材料所包含的硫结晶并且析出,因此可以在冷拉丝加工后获得具有所期望的软质特性和所期望的电导率的铜盘条。
本发明的铜接合线使用SCR连续铸造轧制设备,表面的损伤少,制造范围宽,能够稳定生产。通过SCR连续铸造轧制,以铸块棒的加工度为90%(30mm)~99.8%(5mm)来制作盘条。作为一例,采用以加工度99.3%制造φ8mm的盘条的条件。
熔融炉内的熔铜温度优选控制为1100℃以上1320℃以下。如果熔铜的温度高,则倾向于气孔增多、损伤发生并且粒子尺寸增大,因此控制为1320℃以下。此外,控制为1100℃以上的理由是,在该温度以下时熔铜易于凝固,有时制造不稳定,但期望熔铜温度为尽可能低的温度。
热轧加工的温度优选为将最初的轧制辊的温度控制为880℃以下,并且将最终轧制辊的温度控制为550℃以上。
这些铸造条件与通常的纯铜的制造条件不同,其目的是使作为熔铜中的硫的结晶和热轧中的硫的析出的驱动力的固溶限更小。
此外,通常的热轧加工中的温度在最初的轧制辊中950℃以下,在最终轧制辊中为600℃以上,但为了使固溶限更小,本实施方式中,期望在最初的轧制辊中设定为880℃以下,在最终轧制辊中设定为550℃以上。
另外,将最终轧制辊中的温度设定为550℃以上的理由是,在低于550℃的温度下,所得的盘条的损伤增多,不能将制造的铜接合线作为制品进行操作。热轧加工时的温度优选在最初的轧制辊中控制为880℃以下的温度,在最终轧制辊中控制为550℃以上的温度,并且为尽可能低的温度。通过这样的温度设定,可以使铜接合线的基体的硬度与高纯度铜(5N以上)的硬度接近。作为硫捕集的效果,除了软化温度降低以外,可举出将基体高纯度化,硬度降低。
优选在竖炉中熔解基础材的纯铜后,以还原状态在槽中流动。即,优选在还原气体(例如,CO气体)气氛下,在控制低浓度合金的硫浓度、钛浓度和氧浓度的同时进行铸造,并且通过对材料实施轧制加工,从而稳定地制造盘条。另外,铜氧化物混入和/或粒子尺寸大于规定尺寸会使制造的铜接合线的品质降低。
如上所述,可以获得伸长特性、断裂强度、维氏硬度的平衡好的软质低浓度铜合金材料作为本发明的铜接合线的原料。
另外,也可以在软质低浓度铜合金材料的表面上形成镀层。镀层可以使用将例如钯、锌、镍、金、铂、银等贵金属作为主成分的材料,或无Pb镀层。此外,软质低浓度铜合金材料的形状没有特别的限定,可以制成截面圆形形状、棒状或扁平导体状。
此外,本实施方式中,通过SCR连续铸造轧制法制作盘条并且利用热轧制作软质材,但也可以采用双辊式连续铸造轧制法或Properzi式连续铸造轧制法。
发明的效果
根据本发明,由于包含Ti等特定的添加元素,其余部分包含铜,晶体组织从表面直至线径的20%的深度为止的平均晶粒尺寸为20μm以下,因此可以提供具有高抗拉强度和伸长率,而且可以兼有柔软性(硬度小)的铜接合线。
附图说明
图1为用于对试样的表层中的平均晶粒尺寸的测定方法进行说明的图。
图2为显示实施材1和比较材1的不同退火温度与伸长率的关系的图。
图3为显示实施材1在退火温度500℃时的径向截面照片的图。
图4为显示实施材1在退火温度700℃时的径向截面照片的图。
图5为显示比较材1在退火温度500℃时的径向截面照片的图。
图6为显示实施材2和比较材2的伸长率与硬度的关系的图。
图7为显示实施材2和比较材2的抗拉强度与硬度的关系的图。
图8为显示直径0.05mm的比较材2的接合线的宽度方向的截面照片的图。
图9为显示直径0.05mm的实施材2的接合线的宽度方向的截面照片的图。
图10为表层中的平均晶粒尺寸的测定方法的概要图。
图11为显示直径0.26mm的实施材3的宽度方向的截面照片的图。
图12为显示直径0.26mm的比较材3的宽度方向的截面照片的图。
图13为显示直径0.26mm的实施材4的宽度方向的截面照片的图。
图14为显示直径0.26mm的比较材4的宽度方向的截面照片的图。
具体实施方式
以下,说明本发明的实施方式,但下述的实施方式不限定权利要求所涉及的发明。此外,应当注意,本实施方式中所说明的特征的全部组合在用于解决本发明的课题的方法中不一定是必须的。
[实施例1]
[软质低浓度铜合金材料(2.6mm直径)的制造]
作为实验材,制作具有氧浓度7质量ppm~8质量ppm、硫浓度5质量ppm、钛浓度13质量ppm的φ8mm的铜线(盘条,加工度99.3%)。φ8mm的铜线是通过SCR连续铸造轧制法(South Continuous Rod System)实施热轧加工而制作的。关于Ti,使在竖炉中被熔解的铜熔液在还原气体气氛下在槽中流动,将槽中流动的铜熔液导入至相同还原气体气氛的铸造釜中,在该铸造釜中添加Ti后,使其通过喷嘴,利用铸造轮与环形带之间所形成的铸模而制成铸块棒。将该铸块棒进行热轧加工而制成φ8mm的铜线。接着,对各实验材实施冷拉丝加工。由此,制作φ2.6mm尺寸的铜线。
使用该φ2.6mm尺寸的铜线,验证铜接合线中使用的原材料的特性。
[关于软质低浓度铜合金材料的软质特性]
表1为将使用了无氧铜线的比较材1和使用了具有氧浓度7质量ppm~8质量ppm、硫浓度5质量ppm、钛浓度13质量ppm的软质低浓度铜合金线的实施材1作为试样,验证在不同退火温度实施了1小时退火的材料的维氏硬度(Hv)的表。根据表1,退火温度为400℃时,比较材1与实施材1的维氏硬度(Hv)为同等水平,即使退火温度为600℃也显示同等的维氏硬度(Hv)。因此可知,本发明的软质低浓度铜合金线具有充分的软质特性,并且即使与无氧铜线相比,特别是在退火温度超过400℃的区域也具备优异的软质特性。
[表1]
试样 | 20℃ | 400℃ | 600℃ |
实施材1 | 120 | 52 | 48 |
比较材1 | 124 | 53 | 56 |
(单位:HV)
[关于软质低浓度铜合金材料的晶体结构]
测定2.6mm直径的实施材1、比较材1的表层中的平均晶粒尺寸。这里,表层中的平均晶粒尺寸的测定方法中,如图1所示,测定从2.6mm直径的径向截面的表面沿深度方向以10μm间隔直至50μm的深度为止的位置的长度10mm的线上的范围的晶粒尺寸,将所得的各个实测值进行平均而得的值作为表层中的平均晶粒尺寸。
测定的结果是,比较材1的表层中的平均晶粒尺寸为100μm,与此相对,实施材1的表层中的平均晶粒尺寸为20μm。因此,在本发明中,将从表面向内部直至20%的深度为止的表层中的平均晶粒尺寸设为20μm以下。
比较材1的晶体结构中,从表面部至中央部整体上大小相等的晶粒均匀地排列,与此相对,实施材1的晶体结构中,在试样的截面方向的表面附近薄地形成的层中的晶粒尺寸与内部的晶粒尺寸相比极小。
[关于软质低浓度铜合金材料的伸长特性与晶体结构的关系]
图2为将使用了2.6mm直径的无氧铜线的比较材1和使用了在2.6mm直径的低氧铜(氧浓度7质量ppm~8质量ppm、硫浓度5质量ppm)中添加了13质量ppm的Ti的软质低浓度铜合金线的实施材1作为试样,验证在不同退火温度实施了1小时退火的材料的伸长率(%)的值的变化的图。图2所示的圆形记号表示实施材1,矩形记号表示比较材1。
如图2所示,可知与比较材1相比,实施材1在退火温度超过100℃且从130℃附近至900℃的宽范围内显示优异的伸长特性。
图3为显示在退火温度500℃时的实施材1的铜线的径向截面照片的图。如图3所示,在铜线截面整体中形成了微细的晶体组织,认为该微细的晶体组织促进了伸长特性。与此相对,在退火温度500℃时的比较材1的截面组织进行了2次再结晶,与图3的晶体组织相比,截面组织中的晶粒粗大化,因此认为伸长特性降低。
图4为显示在退火温度700℃时的实施材1的铜线的径向截面照片的图。可知铜线截面中的表层的晶粒尺寸与内部的晶粒尺寸相比极小。虽然内部的晶体组织进行了2次再结晶,但外层中的微细晶粒的层残存。实施材1中,内部的晶体组织大地生长,但表层中残存微细晶体的层,因此认为维持了伸长特性。
这样,通过调节退火温度和退火时间,可以调节线材截面中的微细晶体层所占的比例,可以根据微细晶体层所占的比例而调整线材的伸长特性。
图5为将比较材1的径向截面组织在截面照片中显示的图。如图5所示,从表面至中央整体上大致相等大小的晶粒均匀地排列,在截面组织整体中进行了2次再结晶,因此认为与实施材1相比比较材1的600℃以上的高温区域中的伸长特性降低。
根据以上的结果,与比较材1相比,使用了实施材1的制品中,柔软性、电导率提高,并且可以提高伸长特性。
以往的导体中,为了使晶体组织再结晶成实施材1那样的大小,需要高温的退火处理。然而,如果退火温度过高,则S会再固溶。此外,以往的导体中,如果进行再结晶,则有变得柔软、伸长特性降低的问题。然而,实施材1具有下述特征:由于在退火时可以不形成双晶地再结晶,因此内部的晶粒变大,变得柔软,但另一方面,由于表层残存微细晶体,因此抗拉强度和伸长特性不降低。通过在铜接合线中使用这样的原材料,可以实现柔软、具有高导电性、伸长特性优异、具备后述的优异的抗拉强度的铜接合线。
[实施例2]
[铜接合线]
到制作φ2.6mm尺寸的铜线时为止,与上述的软质低浓度铜合金材料的实施例1是同样的。对上述铜线实施拉丝加工直至φ0.9mm,利用通电退火炉一旦退火后拉丝直至φ0.05mm。接着,利用管状炉实施400℃~600℃×0.8~4.8秒的移动退火,制成实施材2的材料。作为比较,φ0.05mm的4N铜(99.99%以上,OFC(无氧铜))也在同样的加工热处理条件下制作,制成比较材2的材料。测定这些材料的机械特性(抗拉强度、伸长率、硬度)、晶粒尺寸。
表层中的平均晶粒尺寸测定从0.05mm直径的径向截面的表面沿深度方向直至10μm的深度为止的位置的长度0.025mm的范围的晶粒尺寸。
(铜接合线的软质特性、伸长率和抗拉强度)
图6和图7为对于使用了无氧铜线的比较材2的盘条、和由使低氧铜含有13质量ppm的Ti的软质低浓度铜合金线制作而成的实施材2的盘条,从φ0.9mm(退火材)进行拉丝加工直至φ0.05mm,测定通过管状炉进行移动退火(温度300℃~600℃,时间0.8~4.8秒)后的截面硬度(Hv)和机械特性(抗拉强度、伸长率)而得到的结果。
截面硬度通过研磨埋入树脂中的φ0.05mm线的横截面,测定线中央部的维氏硬度来评价。测定数为5处,取其平均值。
抗拉强度和伸长率的测定通过将φ0.05mm线在标距100mm、拉伸速度20mm/min的条件下进行拉伸试验来评价。材料断裂时的最大拉伸应力为抗拉强度,将材料断裂时的最大变形量(应变)设为伸长。
如图6所示,可知在以大致相同伸长率进行比较的情况下,实施材2的硬度与比较材2相比小10Hv左右。与OFC材料相比,可以不降低伸长特性,减小硬度,从而实施材2的铜接合线与使用无氧铜的接合线相比,可以降低接合时的焊盘破坏。
如图7所示,可知在以大致相同伸长率进行比较的情况下,实施材2的硬度与比较材2相比小10Hv左右。与无氧铜相比,可以不降低伸长的特性,减小硬度,从而例如实施例2的铜导体与使用无氧铜的接合线相比,可以降低接合时的焊盘破坏。
表2表示在图6所示的评价结果中实施材2与比较材2中硬度选择大致同等条件的数据而进行比较的结果。表2的上格的实施例表示将实施材2的盘条从φ0.9mm(退火材)进行拉丝加工直至φ0.05mm,在管状炉中进行400℃×1.2秒移动退火时的机械特性和硬度。同样地,表2的比较例表示将比较材2的盘条从φ0.9mm(退火材)进行拉丝加工直至φ0.05mm,在管状炉中进行600℃×2.4秒移动退火时的机械特性和硬度。
[表2]
如表2所示,即使为相同硬度的材料,实施材2的伸长与比较材2相比也高7%以上,因此可以大幅度促进线接合时的连接可靠性、操作特性的提高。此外,实施材2与虽为相同硬度但使用无氧铜的比较材2的接合线相比,抗拉强度高,因此可以大幅度促进连接部(球颈部)的强度可靠性。
这里的所谓线接合部的连接可靠性,是指在线接合后树脂模制后,对于由铜线与树脂材的热膨胀差而产生的应力的耐性。此外,所谓操作性,是指对于从线轴向接合部供给线时的应力的耐性、以及卷曲行为的发生难易度。
接下来,根据图7,可知以大致相同抗拉强度进行比较的情况下,实施材2的硬度与比较材2相比小10Hv左右。可以不降低抗拉强度,减小硬度,因此可以降低实施例2的接合线在接合时的焊盘破坏。
表3显示实施材2与比较材2中抗拉强度选择大致同等条件的数据而进行比较的结果。表3的上格的实施例表示将实施材2的盘条从φ0.9mm(退火材)进行拉丝加工直至φ0.05mm,在管状炉中进行500℃×4.8秒移动退火时的机械特性和硬度。同样地,表3的比较例表示将比较材2的盘条从φ0.9mm(退火材)进行拉丝加工直至φ0.05mm,在管状炉中进行600℃×2.4秒移动退火时的机械特性和硬度。
[表3]
如表3所示,即使为相同抗拉强度的材料,实施例2的伸长率与比较材2相比也高5%,因此可以大幅度促进线接合时的连接可靠性、操作特性的提高。此外,虽为相同抗拉强度的材料,但实施材2的硬度与比较例2相比也充分小,因此可以减小线接合时的焊盘破坏。
这里的所谓线接合部的连接可靠性,是指在线接合后树脂模制后,对于由铜线与树脂材的热膨胀差而产生的应力的耐性。此外,所谓操作性,是指对于从线轴向接合部供给线时的应力的耐性、以及卷曲行为的发生难易度。
硬度、伸长率、抗拉强度的平衡根据制品所要求的规格的不同而稍微不同,作为一例,根据本发明,在重视抗拉强度的情况下,能够供给抗拉强度270MPa以上、伸长率7%以上、硬度65Hv以下的线。
此外,在重视硬度小的情况下,能够供给抗拉强度210MPa以上且小于270MPa、伸长率15%以上、并且硬度63Hv以下的导体。
(关于0.05mm直径的铜接合线的晶体结构)
图8为将比较材2的铜接合线的径向截面组织在截面照片中显示的图,图9为将实施材2的铜接合线的径向截面组织在截面照片中显示的图。如图8所示,可知比较材2的晶体结构中,从表面至中央整体上大小相等的晶粒均匀地排列。另一方面,实施材2的晶体结构中,整体上晶粒的大小稀疏,在试样的截面方向的表面附近薄地形成的层中的晶粒尺寸与内部的晶粒尺寸相比极小。
本发明人认为,比较材2中未形成的在表层中出现的微细晶粒层在实施例2中具有软质特性,并且促进兼具抗拉强度和伸长特性。
通常可理解,如果进行以软质化为目的的热处理,则如比较材2那样通过再结晶而形成了均匀地粗大化的晶粒。然而,在实施材2中,即使实行在内部形成粗大晶粒的退火处理,也会在表层中残存微细晶粒层。因此,认为实施材2获得了虽为软质铜材但抗拉强度和伸长优异的软质低浓度铜合金材料。
此外,基于图8和图9所示的晶体结构的截面照片,测定比较材2和实施材2的试料的表层中的平均晶粒尺寸。
图10显示表层中的平均晶粒尺寸的测定方法的概要。如图10所示,在从0.05mm直径的宽度方向截面的表面沿深度方向以5μm间隔直至10μm的深度为止的线径的20%的深度的范围内,测定晶粒尺寸。然后,由各测定值(实测值)求出平均值,将该平均值作为平均晶粒尺寸。
测定的结果是,比较材2的表层中的平均晶粒尺寸为22μm,与此相对,实施材2的表层中的平均晶粒尺寸直至深度5μm为止的最表面层为7μm和直至其内部的5~10μm为止的表层为15μm,与比较材2的表层不同。将表层的平均晶粒尺寸细作为理由之一,认为获得了高抗拉强度和伸长。另外,如果晶粒尺寸大,则龟裂沿晶体晶界进展。然而,如果表层中的晶粒尺寸小,则龟裂的进展方向改变,因此进展被抑制。因此,认为实施材2的疲劳特性与比较材2相比优异。因此,为了实现本实施例的效果,作为表层的平均晶粒尺寸,优选为15μm以下。
所谓疲劳特性,是指经受反复应力时,直至材料断裂为止的应力施加循环数或时间。
[实施例3]
(关于0.26mm直径的铜接合线在退火温度600℃时的晶体结构)
图11显示为与实施材1同样的成分组成,使用了相对0.26mm直径的线材在退火温度600℃实施了1小时退火的材料的实施材3的试样的径向截面组织的截面照片,图12为显示比较材3的径向截面组织的截面照片的图。
如图11和图12所示,可知比较材3的晶体结构中,从表面部至中央部整体上大小相等的晶粒均匀地排列。与此相对,实施材3的晶体结构中,整体上晶粒的大小稀疏,应当特别说明的是,在试样的截面方向的表面附近薄地形成的层中的晶粒尺寸与内部的晶粒尺寸相比极小。
这在通常情况下可理解为,如果在退火温度600℃进行1小时退火处理,则如比较材3那样通过再结晶而形成了均匀地粗大化的晶粒,但在本发明的情况下,认为即使在退火温度600℃进行1小时退火处理,也会在其表层上残存微细晶粒层,因此获得了虽为软质铜材但可实现后述的铜接合线的良好的抗拉强度、伸长特性的软质低浓度铜合金材料。
而且,基于图11和图12所示的晶体结构的截面照片,测定实施材3和比较材3的试样的表层中的平均晶粒尺寸。这里,关于表层中的平均晶粒尺寸的测定方法,如图1所示,测定从2.6mm直径的宽度方向截面的表面沿深度方向以10μm间隔直至50μm的深度为止的位置的长度1mm的线上的范围的晶粒尺寸,将所得的各个实测值进行平均而得的值作为表层中的平均晶粒尺寸。
测定的结果是,比较材3的表层中的平均晶粒尺寸为50μm,与此相对,实施材3的表层中的平均晶粒尺寸为10μm,在这点上大不相同。认为由于表层的平均晶粒尺寸细,因此实现了后述的铜接合线的良好的抗拉强度、伸长特性。
[实施例4]
(关于0.26mm直径的铜接合线在退火温度400℃时的晶体结构)
图13为将实施材4的试样的宽度方向的截面组织在截面照片中显示的图,图14为将比较材4的宽度方向的截面组织在截面照片中显示的图。
实施材4为具备氧浓度7质量ppm~8质量ppm、硫浓度5质量ppm、钛浓度13质量ppm的0.26mm直径的低浓度铜合金线,在退火温度400℃经过1小时退火处理来制作。比较材4为由无氧铜(OFC)构成的0.26mm直径的线材,在退火温度400℃经过1小时退火处理来制作。
如图13和图14所示,可知比较材4的晶体结构中,从表面部至中央部整体上大小相等的晶粒均匀地排列。与此相对,实施材3的晶体结构,表层与内部的晶粒的大小有差异,与表层中的晶粒尺寸相比,内部的晶粒尺寸极大。
将铜退火而使晶体组织再结晶时,实施材4易于进行再结晶化,内部的晶粒大幅度生长。
接下来,表4显示实施材4和比较材4的电导率。
[表4]
如表4所示,实施材4的电导率比比较材4的电导率高,为大致同等的,作为接合线可以满足。
以上的本实施方式的铜接合线是由包含Ti等且其余部分包含不可避免的杂质的软质低浓度铜合金材料,其中,晶体组织从表面直至线径的20%的深度为止的表层的平均晶粒尺寸为15μm以下,其内部的平均晶粒尺寸比上述表层的平均晶粒尺寸大,从而通过铜线表层的晶粒的微细化而可以兼有高抗拉强度和伸长,因此可以提高制品的连接可靠性。
另外,与添加的Ti同样地,选自由Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素也捕集作为杂质的硫(S),因此作为基体的铜母相高纯度化,从而提高原材料的软质特性。因此,确认了可获得可以抑制接合时对硅芯片上的脆弱的铝焊盘带来破坏的效果。
另外,本实施方式的铜接合线不需要铜的高纯度化(99.999质量%以上)处理,可以通过低价的连续铸造轧制法实现高电导率,因此可以低成本化。
此外,本实施方式的铜接合线还可以适合用作车载用功率模块用途的φ0.3mm左右的Al接合线的替代品,可以避免下述问题:由于与由原材料的高热传导性所引起的线径的减少相伴的模块的小型化、由热传导性提高所引起的放热性提高,从而因为电流密度增大而使连接可靠性降低。
Claims (5)
1.一种铜接合线,其特征在于,由软质低浓度铜合金材料构成,所述软质低浓度铜合金材料包含选自由Ti、Mg、Zr、Nb、Ca、V、Ni、Mn和Cr所组成的组中的添加元素且其余部分为铜,所述铜接合线的晶体组织从至少其表面向内部直至线径的20%的深度为止的平均晶粒尺寸为20μm以下。
2.根据权利要求1所述的铜接合线,其特征在于,含有超过2质量ppm的量的氧,含有2质量ppm以上12质量ppm以下的硫。
3.根据权利要求1或2所述的铜接合线,其特征在于,抗拉强度为210MPa以上,伸长率为15%以上,以及维氏硬度为65Hv以下。
4.根据权利要求1或2所述的铜接合线,其特征在于,电导率为98%IACS以上。
5.根据权利要求1或2所述的铜接合线,其特征在于,所述添加元素为4质量ppm以上55质量ppm以下的Ti,包含超过2质量ppm且为30质量ppm以下的氧。
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