CN1777702A - 净化铜或镍的等离子体处理 - Google Patents

净化铜或镍的等离子体处理 Download PDF

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CN1777702A
CN1777702A CNA200480010539XA CN200480010539A CN1777702A CN 1777702 A CN1777702 A CN 1777702A CN A200480010539X A CNA200480010539X A CN A200480010539XA CN 200480010539 A CN200480010539 A CN 200480010539A CN 1777702 A CN1777702 A CN 1777702A
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米兰·莫齐蒂克
尤罗斯·克维尔巴
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Abstract

本发明涉及一种处理电子构件的方法，这些构件用铜或镍或它们相互之间或与其他材料的合金例如黄铜制成或用它们包覆，该方法包括下列步骤：将所述构件安置在一处理室内；将所述处理室抽成真空；将氧气导入到所述处理室内；确保所述处理室内压强在10－1至50mbar范围内以及借助频率高于约1MHz的高频发生器在该处理室内激发等离子体；使氧原子团作用到所述构件上，此时流到构件表面上的原子团流量大于每秒每平方米约1021个原子团；对所述处理室抽气；将氢气导入到所述处理室内；确保所述处理室内的压强在10－1至50mbar范围内以及借助频率高于约1MHz的高频发生器在该处理室内激发等离子体；使氢原子团作用到所述构件上，此时流到构件表面上的原子团流量大于每秒每平方米约1021个原子团。

Description

净化铜或镍的等离子体处理
技术领域
本发明涉及一种处理方法，尤其用于通过使用活性等离子体净化的铜或镍或它们的合金例如黄铜制成的或用它们包覆的电子构件。
背景技术
用铜或镍或它们的合金例如黄铜制成或用它们包覆的构件典型地被一污染层覆盖。往往在表面上存在至少一个天生的氧化层。这些构件还经常被不同的有机和无机污垢污染。有机污垢常常是在加工过程中施加的油或脂的残余物。无机污垢含有氧化物，还有氯化物和硫化物。在表面上无机污垢的厚度取决于构件存放的环境和温度。温度越高，无机污垢层越厚。
在构件上的污垢层应在进一步加工前，尤其在印刷、涂漆、粘接、钎焊或熔焊前去除，以保证良好的加工质量。
金属构件表面净化的传统方法包括机械加工和化学处理。机械净化往往通过刷清或喷砂实施，而化学净化通过将构件浸入化学药剂的溶液内，然后用蒸馏水淋洗并接着干燥来实现。
但是不管哪一种方法都不能保证构件理想的纯净度。还始终在表面上存在一个薄的污垢层。这对于接下来的高温加工，如熔焊和硬钎焊通常是有利的，至少是无害的。然而在微电子技术领域，期望的纯净度通常远远超过传统方法的极限；因为在电子构件中经常进行的那些低温加工如粘接、涂漆和印刷时，表面的残留污垢会影响加工质量。因此需求一更好的净化过程，以便去除所有的表面污垢以及获得一种实际上原子纯的表面。
这尤其涉及铜，这一元素现在认为是一种中间化合物质，因为铜有较小的单位电阻和比较高的电流负荷能力。然而铜很易于氧化。在存放铜时氧化是有害的，它影响在相邻层上的粘附，损害铜结构元件的电导率，以及降低整个电路的工作可靠性。因此需要一种极其有效的方法来净化在具有集成电路的设备中的铜的沉积层。
在生产具有集成电路的设备的一个或多个步骤中采用新型净化工艺。这些新型方法基于使用气体(经常是一种低压等离子体)的失衡状态，如在文章“用于电子器件制造中的等离子方法(Plasmaverfahren in derElektronikfertigung)”(J.Messelhause，mo，Jahrg.55(2001)8，33至36页)所述，或基于在活性粒子上丰富的余辉。它们被利用来去除在生产过程中在表面上形成的有机污垢和无机污垢，以及还用于净化制造室。在德国公开文件DE 19702124 A1中也介绍了一种净化工件表面的方法。据此，可为此使用不同的气体、单独或作为两种或多种成分的气体混合物来产生等离子体。DE 4034842 C2介绍了一种等离子化学净化法，用氧和氢作为彼此相继的工作气体，以及介绍了一种接下来进行的金属基质的PVD或PECVD涂层。在这里借助在微波区内的频率进行等离子体的激发，为此力求获得高的原子团和离子份额。在日本专利申请JP 62158859A中介绍了表面预处理的另一种可能性，其中，表面首先用惰性气体的离子以及然后用氢离子轰击。
在不同的引文中记载和授予专利权的包括等离子净化的铜净化法，例如作为一种在制造具有集成电路的设备过程中的加工方法而用于初步净化(US 6107192、TW 411497、FR 2801905)，用于去除侧壁、连接装置和通道上的氧化层(TW 471126、US 2001-049181、US 6323121、US 6309957、US6204192、EP-1041614、WO 00/29642)或用于去除铜连接点上的氧化层(WO02/073687、US 2002-127825)，或用于改善铜方法综合特性(Kupferverfahrensintegration)(US 6395642)，或用于净化具有集成半导体电路的设备(US 2002-042193)，集成半导体电路具有埋入的在主导体层内含铜的中间化合物。推荐用于铜净化的气体是氢气和氮气的混合气体或氨气。在专利文件TW 471126中推荐氩气和氢气组成的混合气体。这种混合气体也适用于去除含氟的苛性残留物(TW 472319)。
等离子净化作为一种在铜酸洗过程后从半导体处理室的表面去除沉积的酸洗副产品的方法也已被授予专利权(US 6352081、TW 466629、WO01/04936)。这种方法包括施加一种氧化的等离子体和一种含有活性氟酸盐的等离子体。
发明内容
本发明的目的是创造一种处理用铜或镍或它们相互组合成的合金或与其他材料组成的合金例如黄铜制成或覆盖的电子构件的方法，通过此方法净化所涉及构件的表面，以及以特别的方式为后续的具有最高质量的低温加工作好准备。
通过在权利要求1中说明的方法达到此目的。据此，按照本发明所述构件先后遭遇氧等离子体和氢等离子体，以便首先清除有机污垢以及接着消除氧化的污垢，在两个等离子体处理步骤期间遵守特殊的条件，包括有关在处理室内的压强(10-1至50mbar)、在处理室内激发等离子体的方式(借助频率高于约1MHz的高频发生器)、以及氧原子团作用到构件上的强度(流到构件表面上的原子团流量超过每平方米约1021个原子团)。由此有利于进一步加工，尤其是因为改善了接下来的粘接剂或焊料金属在表面上的粘附以及减小了连接点的电阻。这种方法可有利于保护环境地取代工业的净化过程，而这些工业净化过程当前采用湿式化学净化。
本发明提供了一种从电子构件表面去除有机和无机污垢的方法，所述构件用铜或镍或它们的合金如黄铜制成或用它们包覆。将构件置入一真空室内，该真空室优选地抽成真空度达压强为10Pa或更低。然后向真空室填充氧化气体。在一优选的实施方式中，所述氧化气体是纯氧气或是一种氩气或另一种惰性气体与氧气的混合物，以及总的压强为10至5000Pa。按另一种实施方式也可以规定加入水蒸气或氩气或另一种惰性气体与水蒸气的混合物。氩气可以用任何惰性气体代替。等离子体通过高频放电激发。在放电中产生的氧原子团与有机的表面污垢相互作用，以及将它们氧化成从表面解吸和被抽出的水和氧化碳。在氧化的等离子处理后，表面便没有有机污垢。
无机污垢(主要是氧化铜或氧化镍)通过在真空室内加入氢气或氩气和氢气的混合物去除。氩气可以用任何惰性气体代替。等离子体通过高频放电激发。在放电中产生的氢原子团与无机的表面污垢相互作用，以及将它们还原为从表面解吸和被抽出的水和其他简单的分子，如HCl、H2S、HF等。在氢等离子处理后，表面实际上没有任何污垢。
本发明的一个独特之处在于，基于这些特殊的条件，在处理过程中没有发生用高能离子轰击表面或只是极轻微地轰击表面，这业已证明是特别有利的。
采用按照本发明的方法处理用铜或镍制成或用它们包覆的电子构件有一系列明显的优点。该方法实现了良好地粘附任何沉积在表面上的材料，包括粘接剂、颜料和低温钎焊金属，保证通过构件与敷层的接触面有良好的电导率，这在生态学上是有利的，以及它的运行费用及其维护费用是最低的。本发明与此同时还兼顾到下列想法，即，通过减小构件表面上污垢含量的等离子处理，提高了相邻层的粘附能力以及减小了通过连接面形成的电阻。
按照本发明经等离子处理的表面被钝化，这导致面对空气或水腐蚀有更长期的稳定性。此外，这样一种表面实现了非常良好地粘附任何沉积在表面上的材料，包括粘接剂、颜料和钎焊金属。
附图说明
图1示意性地表示规定用于等离子净化铜或镍的一系统的例子；
图2a是俄歇电子能谱AES(Auger Elektronenspektroskopie)-深度断面图，它表示在未处理的铜试件表面上化学元素的浓度作为溅射时间的函数；
图2b是俄歇电子能谱-深度断面图，它表示在湿式化学处理后的铜试件表面上化学元素的浓度作为溅射时间的函数；
图2c是俄歇电子能谱-深度断面图，它表示在氧等离子处理后的铜试件表面上化学元素的浓度作为溅射时间的函数；
图2d是俄歇电子能谱-深度断面图，它表示在氧或氢等离子处理后的铜试件表面上化学元素的浓度作为溅射时间的函数。
具体实施方式
在图1的示意图中表示出一用于等离子处理铜或镍的系统结构的举例。该系统包括一个放电室7、一台带有一阀门2的真空泵1，一个有滤筛的收集器3、三个不同的排出阀8及三个装氧气、氢气和另一种气体(尤其惰性气体)的气瓶9，以及该系统实现有效和经济的处理加工。在酸洗过程中，等离子体参数如在放电室内原子团的剂量，通过一真空计4和两个或更多个探测器如催化探测器5和朗谬尔探测器6控制。将原子团流量调整为每秒每平方米约大于1021个原子团，优选地大于1022或更有利地大于1024个原子团。
在气态的含有一种氧化气体(优选氧气或水蒸气)的等离子体内形成原子团的速度取决于放电源的功率。此功率优选地界于每升放电容积30与1000W之间，以保证在10与5000Pa之间的压强范围内形成一种相当均匀的等离子体。气体可以是一种由氩气和氧化气体组成的混合气体，氧化气体在气体中所占的比例应允许在等离子体内有最高的氧原子团浓度。等离子体由一优选为电感式耦合的高频发生器产生。其中，频率大于约1MHz，优选地大于3MHz，由此防止离子加热。因为用高频发生器产生频率，所以频率不处于微波范围。此外，与高频发生器电感式耦合相结合还可以防止离子以超过50eV的能量撞击构件。当等离子体发生器的频率低于3MHz时，认为能量学的离子会造成构件表面材料的溅射(Sputtern)。通过氧原子团去除有机污垢认为是由原子团与有机的表面污垢可能存在的单纯的相互作用引起的。在室温下的去除速度在10与100nm/minute之间。因为有机污垢在构件上的特征厚度为10nm的数量级，所以在含氧化气体的气态等离子体内的净化时间约为1分钟。气体通过真空系统的流速优选为在每m2被处理表面100至10000sccm的大约范围内，但特别优选地换算到标准条件为大于每m2被处理表面每分钟1升(1000sccm)，由此保证快速去除反应产物。在氧等离子处理期间，在构件表面上形成一个氧化层(图2c)。
在铜或镍或其合金的表面上薄的氧化膜最好通过引入一种气态的由纯氢气或氢气与一种惰性气体优选氩气组成的混合气体形成的等离子体来还原成纯金属。在气态的含氢的等离子体内氢原子团形成的速度取决于放电源的功率。此功率优选地界于每升放电容积30与1000W之间，以保证形成一种可以说均匀的处于压强范围10与5000Pa之间的等离子体。所述气体可以是一种由氩气和氢气组成的混合气体，氢气在气体中所占的比例应允许在等离子体内氢原子团有最高的浓度。含氢的等离子体优选地通过与含氧的等离子体相同的发生器和在相同的真空系统中造成。但作为替换方案也可以通过直流辉光放电产生氢原子团。试件可以通过附加的直流电压被施以朝向放电室壁的负偏压。通过氢原子团还原氧化的污垢认为是由原子团与表面污垢可能存在的单纯的相互作用引起的。室温下的还原速度在1与10nm/minute之间。因为氧化层在构件上的特征厚度为10nm的数量级，所以在含氧化气体的气态等离子体内的净化时间为几分钟。气体通过真空系统的流速优选地界于一个每m2被处理表面100至10000sccm的大约范围内，但特别优选地换算到标准条件下大于每m2被处理表面每分钟1升，由此保证快速去除反应产物。在氢等离子处理期间氧化层完全被还原。许多其他的氧化污垢包括氯化物和硫化物同样也被还原。因此，氢等离子处理保证了一种实际上原子纯的表面(图2d)。
因此净化过程包括用氧原子团处理后用氢原子团处理。如果有机污垢的量小，可以只采用氢原子团处理。认为氢原子团也与有机污垢反应，不过反应速度比在氧原子团的情况下低。
图2a举例表示一种未经处理的铜表面。此表面被在机械加工期间留下的各种污垢污染。在薄的试件表面层内的污垢类型和浓度通过绘制AES深度断面图在真空室内基本压强小于1.3×10-7Pa的PHI545扫描-俄歇-微型探测器(PHI545-Scanning-Auger-Mikrosonde)中确定。采用一种静态的一次电子束，它的能量为3keV、电流为3.5μA和电子束直径约为40μm。电子束相对于表面平面的垂线的入射角为47度。试件使用两个对称倾斜具有动能为1keV的Ar+离子束溅射，由此保证试件的酸洗。溅射时间对应于深度，也就是1分钟相当于4nm。原子浓度根据俄歇峰对峰高度(Auger-Spitze-zu-Spitze-Hohen)通过使用元素相对灵敏度系数SCu＝0.22、SC＝0.18、So＝0.50、Ss＝0.80和SC1＝1.05而作为溅射时间的函数来量化表示。
在图2b中表示经湿式化学净化后的试件深度断面。试件用四氯乙烯净化，然后仔细地用蒸馏水淋洗。可以发现，碳膜的厚度减小了，但仍旧有一些碳继续存在于上部薄的表面层内。污垢膜的厚度从未经净化的试件上平均被减小三倍以上。
在图2c中表示遭遇每平方米约7×1024个原子团的氧等离子体后试件的AES深度断面。此试件除最外部的表面估计由于受二次污染外，几乎没有碳膜(有机污垢)。在表面上形成氧化膜。氧等离子体的活性粒子明显地与有机污垢层反应并将它们完全去除。不过在通过氧等离子体可以说是短时的作用期间形成了一层所不希望的氧化层。
首先遭遇过氧等离子体的试件，随后遭遇每平方米约2×1025个原子团的氢等离子体。图2d表示处理后的AES深度断面。除了氧、碳和硫极低的浓度以及估计是在AES分析前由于空气的作用引起的二次污垢外，在表面上几乎没有任何污垢。
电阻的测量在一系列十个试件上实施，以及测量了通过不同方法净化的铜构件的平均电阻。用湿式化学过程净化的铜构件试件的电阻下降约16％。但用由氧等离子体与氢等离子体组合净化的铜试件的电阻得到改善，因为电阻下降了约28％。净化铜表面的最有效方法是一种组合的氧-氢等离子体处理，这种组合的处理方法导致一种没有表面污垢膜的实际上无污染的表面，以及导致达两倍的被良好改善的电导率。这通过AES深度断面(图2a、图2b、图2c、图2d)以及电阻的测量已经证实。

Claims (10)

1.一种处理电子构件的方法，这些构件用铜或镍或它们相互之间或与其他材料构成的合金例如黄铜制成或用它们包覆，所述方法包括下列步骤：
将所述构件安置在一处理室内；
将所述处理室抽成真空；
将氧气导入到所述处理室内；
确保所述处理室内压强在10-1至50mbar范围内以及借助频率高于约1MHz的高频发生器在该处理室内激发等离子体；
使氧原子团作用到所述构件上，此时流到构件表面上的原子团流量大于每秒每平方米约1021个原子团；
对所述处理室抽气；
将氢气导入到所述处理室内；
确保所述处理室内的压强在10-1至50mbar范围内以及借助频率高于约1MHz的高频发生器在该处理室内激发等离子体；
使氢原子团作用到所述构件上，此时流到构件表面上的原子团流量大于每秒每平方米约1021个原子团。
2.按照权利要求1所述的方法，其中，所述氧气用一种惰性气体和氧气的混合气体来代替。
3.按照权利要求1所述的方法，其中，所述氧气用一种惰性气体与水蒸气的混合物来代替。
4.按照权利要求1所述的方法，其中，所述氢气用一种惰性气体与氢气的混合物来代替。
5.按照权利要求1所述的方法，其中，所述等离子体通过为每升放电容积提供约30至约1000W功率密度来激发。
6.按照权利要求1所述的方法，其中，在等离子体处理步骤中，使气体以每m2处理表面约100至约10000sccm的速度流过所述处理室。
7.按照权利要求1所述的方法，其中，所述高频发生器是电感式耦合的。
8.按照权利要求1所述的方法，其中，通过附加地供给直流电对所述构件施以负偏压。
9.按照权利要求1所述的方法，其中，所述氢原子团在直流辉光放电时产生。
10.一种电子构件的处理，这些构件用铜或镍或它们相互之间的合金或与其他材料例如黄铜一起制成或用它们包覆，首先包括至少一种按照权利要求1所述的处理，以及接下来将另一种材料粘接、钎焊或熔焊到所述电子构件经如此处理后的表面上。
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EP1620581A2 (de) 2006-02-01
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CN100393914C (zh) 2008-06-11
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