CN106471143A - 制造用于接合应用的粗铜线材的方法 - Google Patents

制造用于接合应用的粗铜线材的方法 Download PDF

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Publication number
CN106471143A
CN106471143A CN201580037653.XA CN201580037653A CN106471143A CN 106471143 A CN106471143 A CN 106471143A CN 201580037653 A CN201580037653 A CN 201580037653A CN 106471143 A CN106471143 A CN 106471143A
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China
Prior art keywords
wire rod
annealing
core
diameter
closing line
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Pending
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CN201580037653.XA
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English (en)
Inventor
E.米尔克
L.艾努茨
P.普雷诺西尔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heraeus Deutschland GmbH and Co KG
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Heraeus Precious Metals GmbH and Co KG
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Application filed by Heraeus Precious Metals GmbH and Co KG filed Critical Heraeus Precious Metals GmbH and Co KG
Publication of CN106471143A publication Critical patent/CN106471143A/zh
Pending legal-status Critical Current

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    • 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
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0006—Apparatus or processes specially adapted for manufacturing conductors or cables for reducing the size of conductors or cables
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B21C1/02—Drawing metal wire or like flexible metallic material by drawing machines or apparatus in which the drawing action is effected by drums
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
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Abstract

一种制造接合线的方法，所述接合线包括具有表面的芯，其中所述芯包含≥98.0%的铜，并具有7500至600000 µm2范围内的横截面积和40至95 N/mm2范围内的弹性极限RP0.2（屈服强度），该方法包括以下步骤：（a）提供铜芯前体；（b）拉制该前体直到达到线芯的最终直径；（c）在650至1000℃范围内的最低退火温度下在其整个横截面上使拉制的线材退火4秒至2小时的最小退火时间。

Description

制造用于接合应用的粗铜线材的方法
本发明涉及用于制造粗铜接合线的方法。
接合线用于制造在半导体器件制造过程中用于电互联集成电路和印刷电路板的半导体器件。此外，接合线用于电力电子应用以便使晶体管、二极管等与外壳的垫或引脚（pin）电连接。虽然一开始用金来制造接合线，但现在使用不那么昂贵的材料，例如铜。尽管铜线提供非常好的导电性和导热性，但是铜线的球形接合以及楔形接合具有其挑战。此外，铜线易受氧化的影响。
就线材几何形状而言，最常见的是具有圆形横截面的接合线和具有大致矩形横截面的接合带。这两种类型的线材几何形状都具有它们的优点，使其可用于特定的应用。因此，这两种类型的几何形状都具有其市场份额。例如，接合带对于给定的横截面积具有更大的接触面积。但是，带材的弯曲受限，并且当接合时必须观察带材的取向以便在带材与其所接合的元件之间达到可接受的电接触。至于接合线，则这些弯曲起来更灵活。
但是，接合涉及在接合过程中线材的焊接和更大的形变，这可能造成危害或甚至破坏接合垫以及在下方的与之接合的元件的电结构。
对本发明而言，术语接合线包括所有横截面形状。通过本发明的方法制得的接合线的尺寸关系到粗接合线。在本发明的接合线含义中，粗线被认为是横截面积为7500至600000 µm2或12000至600000 µm2的线材。在具有圆形横截面的线材的实例中，此类线材可以具有98至510 µm或125至510 µm的直径。为了实现足够的生产量和可靠性，粗接合线的机械性能和接合行为与细接合线相比包括特定的要求。
一些近来的发展涉及具有铜芯的接合线。由于高导电性，选择铜作为芯材料。已经找寻了铜材料的不同掺杂剂以优化接合性能。例如，US 7,952,028 B2描述了几种具有大量不同的掺杂剂和浓度的不同的铜基测试线。然而，就接合线本身和接合工艺而言，仍然需要进一步改进接合线技术。
因此，本发明的一个目的是提供制造改进的接合线的方法。
因此，本发明的另一目的是提供制造接合线的方法，所述接合线具有良好的加工性能，并且其在互连时没有特殊要求，由此节约了成本。
本发明的目的还在于提供制造接合线的方法，所述接合线具有优异的导电性和导热性。
本发明的再一目的是提供制造接合线的方法，所述接合线表现出改善的可靠性。
本发明的再一目的是提供制造接合线的方法，所述接合线表现出优异的可接合性。
本发明的另一目的是提供制造接合线的方法，所述接合线对于楔形接合显示出改善的可接合性。
本发明的另一目的是提供制造接合线的方法，所述接合线在接合之前显示出提高的线芯柔软度。
本发明的另一目的是提供制造接合线的方法，所述接合线具有改进的抗腐蚀性和/或抗氧化性。
令人惊讶地，已经发现通过本发明的方法制得的线材解决了上述目的中的至少一个。此外，发现包括通过本发明的方法制得的线材的系统和模块在线材与其它电元件（例如印刷电路板、垫/引脚等）之间的界面处更可靠。
本发明涉及制造接合线的方法，所述接合线包括具有表面的芯，其中所述芯包含≥98.0%的铜，并具有7500至600000 µm2范围内的横截面积和40至95 N/mm2范围内的弹性极限RP0.2（屈服强度），该方法包括以下步骤：
（a）提供铜芯前体；
（b）拉制该前体直到达到线芯的最终直径；
（c）在650至1000℃范围内的最低退火温度下在其整个横截面上使拉制的线材退火4秒至2小时、优选4秒至1小时的最小退火时间。
在一个实施方案中，退火可以作为固定式或静态退火过程来实施，最小退火时间则可以为4秒至2小时、优选4秒至1小时，而在退火动态进行（即采用移动的线材）的情况下，最小退火时间可以为4至30秒。
如果不提供其它特殊限定，组分的所有含量或份额目前均以重量份额的形式给出。特别地，以百分比给出的份额理解为重量%。以ppm（每百万份的份数）给出的份额理解为重量ppm。
通过本发明的方法制得的此类线材在其机械与接合性能方面得到优化。在本发明的一个更优选的实施方案中，线芯或线材的弹性极限RP0.2为≤ 90 N/mm2，最优选≤ 85N/mm2。弹性极限RP0.2的下限优选≥ 40 N/mm2且最优选≥ 50 N/mm2。这特别导致通过本发明的方法制得的接合线的屈服强度的优选和有利的范围。通过本发明的方法制得的接合线优选具有在范围40-95 N/mm2、50-95 N/mm2、40-90 N/mm2或50-90 N/mm2中的一个或多个内的弹性极限RP0.2。在非常优选的实施方案中，所述芯或线材的弹性极限RP0.2在65-90 N/mm2或65-85 N/mm2范围内。
所述线材或所述芯的弹性极限与屈服强度相同。对于弹性极限或屈服强度的定义，参照公知的理解。材料的“屈服强度”在工程和材料科学中定义为材料开始塑性形变时的应力。在塑性形变开始之前，材料将弹性形变，并在移除施加的应力时将返回其初始形状。目前，通过使用塑性形变的0.2%-偏移屈服点（RP0.2）来定义弹性极限或屈服强度。
弹性极限理解为以完成并包装的产品形式提供的接合线的性质。此外，要理解的是，未对该线材施加过长的储存时间、环境影响等。接合线的弹性极限以其进料至接合工具前的状态给出。
要指出的是，任何机械应力、弯曲、加热、长储存时间等可能影响线材的微观结构及其弹性极限。例如，在刚刚离开退火炉的线材与包装状态下的成品形式的相同线材的弹性极限之间通常存在显著的差异。
要理解的是，可以特别地通过相应地选择退火程序的参数来调节线材的弹性极限。根据本发明，这不一定意味着如现有技术中常见的那样使线材退火至最大伸长率值。相反，选择退火程序和线材的其它参数（铜纯度、添加剂等）以实现根据本发明的弹性极限值。
线材的芯定义为在表面下方的本体材料（bulk material）的均匀区域。由于任何本体材料从根本上具有在一定程度上性质不同的表面区域，线材的芯的性质被理解为该本体材料区域的性质。本体材料区域的表面在形貌、组成（例如氧含量）或其它特征方面可能不同。在优选的实施方案中，该表面可以是线材的外表面。在进一步的实施方案中，线芯的表面可以作为线芯与叠置在线芯上的涂层之间的界面区域来提供。
该线材是特别用于微电子学中的接合的接合线。该线材优选是一件式物体。
如果一种组分的份额超出参比材料的所有其它组分，则该组分是“主要组分”。优选地，主要组分占材料总重量的≥50%。
所述芯的铜含量为≥ 98.0%。甚至更优选地，铜含量为≥ 99%。进一步优选地，线芯由纯度≥ 99.9%的铜（3N-铜）组成。最优选地，线芯由纯度≥ 99.99%的铜（4N-铜）组成。纯铜线材通常表现出良好的传导性和良好的接合性能。在替代实施方案中，可以在线芯中提供少量附加元素。此类元素的实例包括Pd、Ag或B。
在本发明通常优选的方面中，退火后线材的伸长率值在最大伸长率值的40至92%范围内。更优选地，该伸长率值在最大伸长率值的45至85%、最优选50至80%范围内。
在又一优选的情况下，线材在比通过退火实现最大伸长率值时的温度高≥ 10℃的温度下退火。更优选地，该温度为比最大伸长率的温度高≥ 50℃，且最优选地，该温度比最大伸长率的温度高≥ 80℃。通常，该温度比最大伸长率的温度高≤ 150℃。因此，线材可以在比最大伸长率的温度高10至150℃、或50至150℃、或80至150℃的温度下退火。
最大伸长率值定义如下：在铜基接合线的一般情况下，可以通过最终退火步骤来调节线材的伸长率。“最终”在这方面是指此后不再设立对线材的形貌具有重大影响的生产步骤。当选择退火参数时，通常选择一组参数。在使线材退火的简单情况下，在给定长度的炉中调节恒定温度，其中线材以恒定速度通过该炉。这使线材的每一点暴露于该温度下持续给定的时间，这一温度和这一退火时间是该退火程序的两个相关参数。在其它情况下，可以采用炉的特定温度分布曲线，由此将其它参数添加到该系统中。
在任何情况下，可以选择其中一个参数作为变量。随后，取决于该变量的所得到的线材伸长率值产生通常具有局部最大值的图。这在本发明的含义中定义为该线材的最大伸长率值。在变量为退火温度的情况下，这样的图通常被称为“退火曲线”。
在现有技术中，相对于变量参数，通常使任何线材退火至这样的最大伸长率值，因为局部最大值的存在提供了特别稳定的制造条件。
对于本发明，令人惊讶地发现，退火至低于最大伸长率值的不同值可以获得有益的线材性质，因为可能以积极的方式影响线材形貌。如果选择退火温度作为变量参数，并将退火时间设定为恒定值，在将退火温度选择为高于最大伸长率的退火温度的值的情况下，这是特别有益的。特别地，该制造原理可用于调节线材的平均晶粒尺寸，例如向更大的晶粒尺寸调节。通过这种调节，可以以积极的方式影响其它性质，如线材柔软度、楔形接合行为等。
为了提供良好的生产量和有效的退火，可以在退火步骤（c）的过程中将所述芯在其整个横截面上加热至≥ 650℃的最低退火温度。甚至更优选地，该温度为≥ 680℃。在退火步骤（c）的过程中将所述芯在其整个横截面上加热至≤ 1000℃的退火温度。因此，在退火步骤（c）的过程中将所述芯在其整个横截面上加热至650-1000℃或680-1000℃范围内的温度。
在一个特别优选的实施方案中，通过分股退火来实施退火，分股退火能够以高再现性快速生产线材。分股退火意味着在线材移动穿过退火炉的同时动态实施退火，并在离开炉后缠绕到线轴（reel）上。
在一个优选实施方案中，线材以包装形式提供，并且该方法在步骤（c）之后进一步包括步骤（d）输送和包装所述线材，其中该线材以曲率半径Rc弯曲，其中Rc等于0.25 ∙ (1/E -1) ∙ Dr，或简化为0.25 ∙ Dr/E，其中Dr定义为在曲率半径方向上测得的线材的直径，其中E是由弯曲造成的线材的外部细丝（outer filament）的相对伸长率；并且其中E ≤0.006。在一个更优选的实施方案中，E ≤ 0.005或≤ 0.004，最优选E ≤ 0.003。通常，E≥ 0.0002。这样的程序确保不会因最终的输送、缠绕和包装过程的影响使线材的优化微观结构和由此其机械性能劣化。通过这些措施，避免了通过退火步骤（c）调节线材的微观结构之后该线材经受不利的机械应力。特别地，退火后该线材的强弯曲或其它强形变将会不利地影响其晶体的尺寸与分布。这些包括其中仅线材外部受到影响，但是该线材整体的机械性能仍在本发明的范围内的影响。
线材的细丝定义为平行于线材的几何中心线延伸并与之保持恒定距离的具有无限小直径的理论细丝。因此上述含义中的外部细丝是在具有最大曲率半径的位置处沿着线芯表面延伸的细丝。
线材弯曲的限制尤其涉及其中在线轴上提供线材的包装形式。取决于线材直径，需要根据上面给出的参数提供包装线轴的最小直径。此外，应当注意，当处理线材时不应超过所述最小弯曲半径。此类处理包括制造线材以及在接合工具中进料和输送线材的程序。
在进一步优选的实施方案中，通过本发明的方法制得的线材已经在退火步骤（c）之后直接缠绕到包装线轴上。这意味着线材在缠绕到最终的包装线轴上之前并未缠绕到中间线轴上。已表明，缠绕线材的任何程序会对其微观结构和机械性能产生影响，因为任何这样的程序均会将线材置于机械应力下。即使使用具有大直径的中间线轴，在一定程度上也会是这样的情况。
由于包装线轴的直径限定了上面解释的含义中线材的最小曲率半径，本发明还涉及提供如根据本发明所制造并包装在线轴（spool）上的线材，其中该包装线轴满足上面给出的曲率半径的参数。
对于通过本发明的方法制得的具有圆形横截面的线材，已经观察到微观结构的不寻常的性质。这些结构有可能与良好的接合性能相关。因此，对于优选的线材，该线材的第二区域（R2）的平均晶粒尺寸与该线材的第一区域（R1）的平均晶粒尺寸之比为0.05至0.8、优选0.05至0.7和更优选0.1至0.6。线材的第一区域（R1）由距线材的几何中心线具有≤线材最小直径的10%的距离的所有点来限定，并且其中线材的第二区域（R2）由距芯的表面具有≤线材最小直径的10%的距离的所有点来限定。线材的最小直径定义为垂直且穿过其几何中心线跨该线材的最短可能直径。
采用电子背散射衍射测定法（EBSD）实施平均晶粒尺寸的测量。将线材片段包埋在树脂中并研磨在其中心线方向上穿过线材的纵向截面。通过离子铣削（ion-milling）抛光并进一步预备该线材的截面区域。对线材的微观组织进行数次测量。通过这些测量来测定线材的晶粒尺寸和分布。
已令人惊讶地发现，在靠近线材表面的边界区域中的平均晶粒尺寸明显小于在线材中心线附近的中心区域中的平均晶粒尺寸。平均晶粒尺寸看起来从线材的中心开始在径向向外的方向上快速减小。此前已知的晶粒尺寸分布显示平均晶粒尺寸的均匀分布或平均晶粒尺寸随着距线材中心的距离的增加而增大。
在该方法的可能的进一步发展中，在拉制前体的步骤（b）之前或之后，提供用涂层材料涂覆铜芯的步骤（e）。涂覆方法的实例是电镀、物理气相沉积和化学气相沉积。在本发明的此类进一步发展中，使涂层叠置在芯的表面上。要理解的是，这样的涂层是通过本发明的方法制得的线材的可能但非必要的特征。为了尽量减小此类涂层的材料对接合过程的影响，涂层的厚度≤ 0.5 µm，更优选≤ 0.2 µm。通常，涂层的厚度≥ 20 nm。
在提供涂层的情况下，该层包含贵金属、Ti、Ni或Cr中的一种作为主要组分。特别优选的用于涂覆目的的贵金属的实例是Pd、Au、Pt和Ag。
术语“叠置”在本发明的含义中用于描述第一项（例如铜芯）相对于第二项（例如涂层）的相对位置。可能地，其它项（如中间层）可布置在第一项与第二项之间。优选地，第二项至少部分叠置在第一项上，例如相对于第一项的总表面的至少 30%、50%、70%或90%。第二项最优选完全叠置在第一项上。术语“中间层”在本发明的上下文中是在铜芯与涂层之间的线材区域。在该区域中，如在芯中的材料以及如在涂层中的材料组合存在。
在本发明的可能的实施方案中，作为中间层提供涂层，其中至少一个外层叠置在中间层上。在这样的情况下，外层优选包含至少一种贵金属作为主要组分。此类贵金属可以特别是Au或Pd。在最优选的组合中，中间层包含Pd且外层包含Au作为各自的主要组分。
在提供外层的情况下，中间层具有5 nm至100 nm范围内的优选厚度。
在一个优选的实施方案中，线材具有圆形横截面形状，其中穿过横截面积的最短路径与最长路径之间的比率为0.8至1.0。这样的线材被称为具有圆形横截面的线材。
在另一优选的实施方案中，线材的形状如条带，其中穿过横截面积的最短路径与最长路径之间的比率为0.02至0.5。
根据需要，本发明的方法可以进一步包括以下步骤：
（f）在步骤（c）之前将线材轧制成条带形状。这确保将圆形线材成形为条带不会影响最终线材的微观结构。
附图描述
在附图中例示了本发明的主题。但是，附图并非意在以任何方式限制本发明或权利要求的范围。
在图1中，描绘了线材1。
图2示出了线材1的横截面视图。在该横截面视图中，铜芯2在横截面视图的中间。铜芯2被涂层3包围。在铜线2的界限上，定位铜芯的表面15。在穿过线材1的中心23的线条L上，铜芯2的直径显示为线条L与表面15的交点之间的端至端距离。线材1的直径是穿过中心23的线条L与线材1的外部界限的交点之间的端至端距离。此外，描绘出了涂层3的厚度。在图2中夸大了涂层3的厚度。如果提供涂层3的话，其典型厚度与芯直径相比非常小，例如≤芯直径的1%。
要理解的是，线材1的涂层3是任选的。对于最优选的实施方案而言，在线芯上不提供涂层。
图3示出了制造根据本发明的线材的方法。
图4描绘了电器件10形式的模块，其包括两个元件11和线材1。线材1电连接两个元件11。虚线表示另外的连接或电路，其将元件11与包围元件11的包装器件（packagingdevice）的外部接线连接。元件11可包括接合垫、引线指（lead fingers）、集成电路、LED等。
图5示出了由4N-铜芯组成的不具有涂层的粗线材的退火曲线。标记了根据现有技术的一个退火窗口和根据本发明的实例的一个退火窗口。
图6示出了在穿过根据本发明制得的线材的纵向截面上的EBSD测量。该线材具有直径为300 µm的圆形横截面。
测试方法
所有测试和测量在T = 20℃和50%的相对湿度下进行。
当测量晶粒的平均晶粒尺寸时，在本文中采用电子背散射衍射测定法（EBSD）。尽管EBSD是可以测定不同晶粒的取向的方法，但是对于本发明的目的而言，该方法仅用于测量晶粒直径。
通过标准程序来进行楔形接合工艺的测量。接合线的工艺参数窗口的定义在本领域中是已知的，并广泛用于比较不同的线材。通过下文中描述的本发明的方法制得的线材的所有实施方案已经显示出优异的接合性能。
实施例
通过实施例进一步例示本发明。这些实施例用于示例性阐述本发明，而非意在以任何方式限制本发明或权利要求的范围。
实施例1
使一定量的纯度≥ 99.99%的铜材料（“4N-铜”）在坩埚中熔融。未向熔体中加入其它物质。然后由该熔体铸造线芯前体。
使用电感耦合等离子体（ICP）仪器（Perkin Elmer ICP-OES 7100DV）来控制Cu线材的化学组成。将Cu线材溶解在浓硝酸中，并将该溶液用于ICP分析。由设备制造商根据对于体相Cu适用的公知技术建立用于测试高纯Cu线材的方法学。
线芯前体随后在数个拉制步骤中进行拉制以形成具有规定直径的线芯2。该线材具有几乎圆形的横截面，其中最长和最短直径的比率（ration）为0.8至1.0。
为了证实对于不同直径的本发明的有益效果，制造一系列选择的具有不同直径的线材。下表1显示了在制造过程的不同步骤处对于不同线材直径测得的数据的列表：
编号 直径[µm] TS1[N/mm2] EL1[%] YS1[N/mm2] TS2[N/mm2] EL2[%] YS2[N/mm2]
1 500 215.6 29.06 70.8 218.8 33.88 91.2
2 400 224.2 26.41 75.0 226.6 28.9 90.7
3 300 225.3 21.2 65.2 225.5 23.05 85.6
4 125 207.5 20.58 68.0 205.8 19.04 90.2
（表1：通过本发明的方法制得的不同线材的数据）
对数据的解释：
TS1：紧接在退火炉后的线材的抗张强度；
EL1：紧接在退火炉后的线材的伸长率；
YS1：紧接在退火炉后的线材的屈服强度；
TS2：在缠绕到包装线轴上之后的线材的抗张强度；
EL2：在缠绕到包装线轴上之后的线材的伸长率；
YS2：在缠绕到包装线轴上之后的线材的屈服强度。
要注意的是，在本发明的含义中线材的屈服强度是上面数据中的“YS2”，因为这指的是成品。用输送和缠绕过程中对线材的附加机械影响来解释YS1与YS2的结果之间的显著差异。在退火程序之后该线材处理的优化可以减小本文中所见的屈服强度的增加。
在本发明的制造线材的程序中，线材在离开退火炉之后首先缠绕到中间线轴上。随后，该线材再次缠绕到包装线轴上。这进一步增加了值YS1与YS2之间的差异。在制造程序的优选变体中，线材直接缠绕到包装线轴上。
为了尽量减小由缠绕造成的机械应力，所用线轴以及所有导向辊均具有最小直径以保持线材产生的弯曲半径高于最小值。优选的最小弯曲半径或曲率半径随线材直径而增加。
曲率半径Rc等于0.25 ∙ (1/E -1) ∙ Dr，其中：
- Dr定义为在曲率半径方向上测得的线材的直径；
- E是由弯曲造成的线材的外部细丝的相对伸长率；并且
- E ≤ 0.006。
在本实施例中，E经选择小至0.002。这意味着例如对于300 µm的线材（样品编号1），线轴的直径经选择为10 cm（= 5 cm曲率半径）。这涉及参数E = 0.0015：
5 cm = 0.25 * 0.03 cm/0.0015
在制造布置中，具有最小弯曲半径的项（线轴、导向辊等）主要限定了退火后线材的机械应力。因此，优选的是所有线轴和辊具有相同的半径，并尽可能减少它们的数量。
还应注意的是，线材的抗张强度TS1、TS2在很大程度上不受本文中描述的措施的影响。无论是根据本发明的特定退火还是由退火后的包装程序造成的机械应力均没有以显著的方式改变该线材的性质。
下表2显示了用于表1的线材的分股退火的退火参数的更多细节：
编号 直径[µm] 炉温[℃] 线材速度[m/min] 炉长度[m]
1 500 800 3 0.82
2 400 800 5 0.82
3 300 800 10 0.82
4 125 700 10 0.82
（表2：表1的线材的退火参数）。
由表2变得清楚的是，采用分股退火，通过改变线材输送速度改变了退火时间。
除了退火时间之外，退火温度也发生改变。
下表3显示了不涉及本发明的对比例。在这些实施例中，以不同的退火参数使相同的线材基材退火。在各种情况下，改变退火参数直到达到最大伸长率值EL1max（其紧接在退火炉后测得）。对于这些线材，给出了紧接在退火炉后测得的值TS1和YS1（参见上面对表1的解释）。
编号 直径[µm] 炉温[℃] 线材速度[m/min] 炉长度[m] TS1 [N/mm2] EL1max [%] YS1 [N/mm2] YS2 [N/mm2]
1 500 800 5 0.82 219.7 37.61 81.0 101.5
2 400 800 10 0.82 228.6 36.11 90.9 110.5
3 300 600 10 0.82 226.6 32.93 95.1 112.3
4 125 600 10 0.82 207.9 28.6 93.7 108.2
（表3：对比例，其中以最大伸长率值为目标进行退火）。
成品的屈服强度值YS2显著高于通过本发明的方法制得的线材。对于对比线材而言，成品的屈服强度值均不低于100 N/mm2。
关于通过本发明的方法制得的线材的退火程序，参照图5。该图显示了300 µm线材的退火曲线。在该曲线中，在不同的温度下进行退火，而退火时间保持恒定。测量紧接在退火炉后的伸长率值EL1并相对于退火温度来显示。
在本发明的分股退火的方法中，由线材速度和炉长度的值计算退火时间。要理解的是，通过本发明的方法制得的线材不限于分股退火。
如在通常情况下那样，退火曲线表现出局部最大值，其位于大约600℃处。要理解的是，最大伸长率值的退火温度还取决于退火时间。
在图5中显示出两个退火窗口A和B。第一窗口A在局部最大值周围对称布置，并且指的是根据现有技术的接合线的退火。传统上使用在局部最大值处或其附近的这种类型的退火，因为其提供良好的工艺稳定性和再现性。
以来自第二退火窗口B的参数使通过本发明的方法制得的线材退火。该窗口布置在退火曲线的高端尾部附近。当伸长率降低至≤最大伸长率值EL1max的92%时，限定窗口B的温度下边界。窗口B的温度上边界仅由要获得的屈服强度的下限来限定。要指出的是，取决于退火程序后线材经受的机械应力（其有助于提高屈服强度），该温度上边界可能不同。
在其它试验中，测量和评估了通过本发明的方法制得的线材的晶体微观结构。图6显示了上述样品编号3线材（300 µm直径）的晶粒结构。将线材样品沿其中心线切片。显示出两个不同的区域R1和R2，其中第一区域R1布置在中心线周围。
第二区域R2布置在线材表面下方。各区域的径向宽度为线材直径的10%。
由所显示的晶粒结构显而易见的是，中心区域R1中的平均晶粒明显大于近表面区域R2中的平均晶粒。测量结果的评估在中心区域R1中给出了25 µm的平均晶粒尺寸。在表面区域R2中的平均晶粒尺寸为11 µm。不同区域中的这些平均晶粒尺寸之比为11 µm/25 µm =0.44。
接合测试已经表明，通过本发明的方法制得的线材显示了优异的接合性能。此外，该线材在接合工具中的处理和接合工艺稳定性因该线材的高柔软度而得以提高。
实施例2
作为本发明的第二实施例，制造条带形式的接合线。根据上述第一实施例进行所有制造步骤，除了在退火步骤之前使线芯扁平化的附加步骤。通过轧制该线材来实现线材的扁平化。所得带材的最短直径与其最长直径之比为0.1。其最短直径为100 µm，其最长直径为1000 µm，横截面积大致为100,000 µm2。
要注意的是，包装产品的退火程序和调节的YS2值对于带材与对于上述圆形线材而言相同。考虑到要遵循的最小曲率半径，带材绕其较短的直径有规律地缠绕，因此该直径是选择线轴和导向辊的直径的相关参数。

Claims (15)

1.制造接合线的方法，所述接合线包括具有表面的芯，其中所述芯包含≥98.0%的铜，并具有7500至600000 µm2范围内的横截面积和40至95 N/mm2范围内的弹性极限RP0.2（屈服强度），所述方法包括以下步骤：
（a）提供铜芯前体；
（b）拉制所述前体直到达到线芯的最终直径；
（c）在650至1000℃范围内的最低退火温度下在其整个横截面上使拉制的线材退火4秒至2小时的最小退火时间。
2.权利要求1的方法，其中所述退火是分股退火。
3.权利要求1或2的方法，其中所述线材在比最大伸长率的温度高10℃至150℃的温度下退火。
4.权利要求1、2或3的方法，在步骤（c）之后进一步包括步骤（d）输送和包装所述线材，
其中所述线材以曲率半径Rc弯曲，其中Rc等于0.25 ∙ Dr/E，
其中Dr定义为在曲率半径方向上测得的所述线材的直径；
其中E是由弯曲造成的所述线材的外部细丝的相对伸长率；并且
其中E为0.0002至0.006。
5.前述权利要求中任一项的方法，其中所述方法进一步包括以下步骤：
（e）在步骤（b）之前或之后，用涂层材料涂覆所述铜芯，以便在所述芯的表面上叠置涂层。
6.权利要求5的方法，其中所述涂层具有20 nm至0.5 µm的厚度。
7.权利要求5或6的方法，其中所述涂层包含贵金属、Ti、Ni或Cr中的一种作为主要组分。
8.权利要求5至7中任一项的方法，其中作为中间层提供所述涂层，其中至少一个外层叠置在所述中间层上。
9.权利要求8的方法，其中所述外层包含贵金属作为主要组分。
10.权利要求8或9的方法，其中所述中间层具有5 nm至100 nm的厚度。
11.前述权利要求中任一项的方法，其进一步包括以下步骤：
（f）在步骤（c）之前将所述线材轧制成条带形状。
12.权利要求1至10中任一项的方法，其中所述线材具有圆形横截面形状，其中穿过所述横截面积的最短路径与最长路径之间的比率为0.8至1.0。
13.权利要求11的方法，其中穿过所述横截面积的最短路径与最长路径之间的比率为0.02至0.5。
14.前述权利要求中任一项的方法，其中所述线材表现出0.05至0.8的所述线材的第二区域（R2）的平均晶粒尺寸与所述线材的第一区域（R1）的平均晶粒尺寸之比，
其中所述线材的第一区域（R1）由距所述线材的几何中心线具有≤线材最小直径的10%的距离的所有点来限定，并且
其中所述线材的第二区域（R2）由距所述芯的表面具有≤线材最小直径的10%的距离的所有点来限定。
15.前述权利要求中任一项的方法，其中所述线材具有最大伸长率值的40至92%的退火后的伸长率值。
CN201580037653.XA 2014-07-11 2015-04-28 制造用于接合应用的粗铜线材的方法 Pending CN106471143A (zh)

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