CN112399896B - 用于烧结管芯附接和类似应用的纳米铜膏和膜 - Google Patents

用于烧结管芯附接和类似应用的纳米铜膏和膜 Download PDF

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CN112399896B
CN112399896B CN201980042475.8A CN201980042475A CN112399896B CN 112399896 B CN112399896 B CN 112399896B CN 201980042475 A CN201980042475 A CN 201980042475A CN 112399896 B CN112399896 B CN 112399896B
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sintering
paste
powder
sintered
film
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CN112399896A (zh
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沙米克·戈萨尔
雷米亚·钱德兰
韦诺德·马诺哈兰
苏利·萨卡尔
巴瓦·辛格
拉胡尔·劳特
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Alpha Assembly Solutions Inc
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Alpha Metals Inc
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Abstract

本发明公开了一种包含铜颗粒的烧结粉末，其中：该颗粒至少部分地涂覆有包覆剂，并且该颗粒表现出大于或等于100nm的D10和小于或等于2000nm的D90。

Description

用于烧结管芯附接和类似应用的纳米铜膏和膜
本发明涉及烧结粉末、烧结膏和烧结膜。
烧结接头提供了焊接接头的替代形式。形成烧结接头的典型方法涉及将金属粉末(通常呈粉末压坯的形式)放置在待接合的两个工件之间，然后烧结金属粉末。金属原子的所产生的原子扩散形成这两个工件之间的粘结。
金属纳米粉末已在电子工业中用于形成烧结接头，并且被认为是无铅焊接的有用替代形式。纳米材料与对应块状材料之间的不同行为被认为是由于纳米材料具有更高的表面积与体积之比。当与传统焊膏相比时，通过使用金属纳米颗粒来形成两种材料之间的导电接头在其机械、电气和热可靠性方面具有许多有益效果。
包含银纳米颗粒的烧结粉末是已知的。通过银纳米颗粒的原子扩散形成的烧结接头可在比块体的熔融温度显著更低的温度下加工并且还可用于高温应用。然而，此类烧结粉末的烧结温度仍然太高，不能在大多数电子应用中有效使用。
可通过在烧结期间施加外部压力来降低烧结温度。已证实银膏的压力辅助低温烧结是作为管芯附接方法的焊料回流的可行替代方案。已证实施加高压可显著降低烧结温度，并且可在相对更快的速率下实现管芯附接的期望特性，从而在数分钟内就形成烧结接头。然而，较大外部压力会使该工艺的自动化很困难。此外，较大外部压力的施加可导致工件损坏。
由于银金属具有优异的电导率和热导率，因此银金属长期以来一直在电子工业中用于管芯附接应用。然而，银的高成本限制了银在许多领域中的广泛应用。此外，银在相对较高的温度和湿度下还面临离子迁移问题，这是另一个引起人们关注的主要原因。
铜是比银便宜得多的材料，并且还具有极高电导率(仅比Ag低6％)。除了其成本更低之外，铜还不表现出离子迁移问题，这使铜比银有优势。然而，铜纳米颗粒发生氧化的固有倾向仍然是一个主要问题。
已经有若干报告提出了各种方法，这些方法证实铜纳米颗粒在被适当保护层涂覆的情况下可在环境条件下抗氧化。这些铜纳米颗粒在用于管芯附接应用的导电管芯附接膏中的效用仍有待大量探索。因此，在电子市场中，对铜管芯附接膏有着巨大的需求，铜管芯附接膏可提供纳米银的几乎相同有益效果，但成本低得多。
WO 2014/068299涉及包含平均最长直径小于10微米的微粒的烧结粉末并且针对具有双峰粒度分布的银纳米颗粒。WO 2015/155542涉及低压烧结粉末并且也针对具有双峰粒度分布的银纳米颗粒。由于这两篇文献利用银，因此可能发生离子迁移问题。
本发明试图解决与现有技术相关联的至少一些问题或至少提供现有技术的商业上可接受的替代解决方案。
在第一方面，本发明提供了包含铜颗粒的烧结粉末，其中：
这些颗粒至少部分地涂覆有包覆剂(capping agent)，并且
这些颗粒表现出大于或等于100nm的D10和小于或等于2000nm的D90。
如本文所定义的每个方面或实施方案可与任何其他方面或实施方案组合，除非有明确的相反指示。具体地，被指示为优选或有利的任何特征可与被指示为优选或有利的任何其他特征组合。
本发明人已令人惊讶地发现，该烧结粉末表现出有利的烧结特性，同时与常规含铜烧结粉末相比还不易氧化。
有利地，该烧结粉末在烧结性能、热导率、电导率和最终接头的有利机械特性方面提供纳米银的同等或类似有益效果，但成本低得多。另外，克服了与纳米银相关联的离子迁移问题。
该烧结粉末通常是空气中稳定的且非团聚的。
此外，该烧结粉末实现了表面的通用接合，特别是诸如以下不同饰面的两个或更多个表面的通用接合：铜至铜；铜至铝；铝至铜；铝至铝；以及铜至镍。该烧结粉末特别适用于管芯附接。
如本文所用，术语“烧结粉末”可涵盖能够形成烧结接头的粉末。通过放置在待接合的两个工件之间的金属颗粒的原子扩散来形成烧结接头。术语“烧结粉末”可涵盖微粒。
该烧结粉末包含铜颗粒。这些颗粒可包括规则形状颗粒(诸如例如球体)和/或不规则形状颗粒(诸如例如晶须、板、棒或薄片)。
铜颗粒可呈例如铜金属或铜合金的形式，优选地为铜金属。
该烧结粉末可包含除铜颗粒之外的颗粒。然而，该烧结粉末中的大部分颗粒是铜颗粒，通常基本上所有颗粒铜都是铜颗粒。
这些颗粒至少部分地涂覆有包覆剂。如本文所用，术语“包覆剂”可涵盖这样的物质，其在存在于金属颗粒的表面上时会减少金属颗粒的团聚，在粉末生产期间实现粒度控制，并且减少颗粒的表面氧化或其他污染。有利地，包覆剂的使用可有助于减少颗粒的团聚。此类团聚是不利的，因为这可增加该烧结粉末的烧结温度。因此，包覆剂的使用能够在更低温度下在工件之间形成烧结接头，并且因此可有助于减少因暴露于高烧结温度而引起的对工件的损坏。另外，包覆剂的使用可有助于避免金属的降解，诸如例如因金属暴露于空气而引起的损坏。
这些颗粒通常基本上涂覆有包覆剂，更通常完全涂覆有包覆剂。
这些颗粒表现出大于或等于100nm的D10和小于或等于2000nm的D90。D90描述该分布中的90％具有更小粒度并且10％具有更大粒度的直径。D10直径具有10％更小粒度和90％更大粒度。如本领域中常规的做法，该直径对应于等效球体直径，并且该分布对应于体积分布。D10和D90可通过本领域已知的合适技术来测量，诸如例如激光衍射、动态光散射和SEM图像分析。
小于100nm的颗粒可更容易氧化。大于2000nm的颗粒可不表现出有利的烧结特性，诸如与块体相比良好的烧结性能和降低的烧结温度。因此，该烧结粉末表现出有利的烧结特性，同时能够在非惰性气氛(诸如空气)下生产、储存、操纵和使用。D90优选地小于或等于1000nm，更优选地小于或等于500nm，甚至更优选地小于或等于450nm，还甚至更优选地小于或等于400nm。更低D90值可改善有利的烧结特性。D10优选地大于或等于125nm，更优选地大于或等于150nm。更大D10值可改善抗氧化性。优选地，这些颗粒表现出大于或等于125nm的D10和小于或等于450nm的D90，更优选地这些颗粒表现出大于或等于150nm的D10和小于或等于400nm的D90。
粒度分布通常为单峰的。
优选地，该烧结粉末用于管芯附接。该烧结粉末可特别有效地用于管芯附接。
包覆剂可为无机的和/或有机的。有机包覆剂的示例包括聚合物和配体。优选地，包覆剂包含胺和/或羧酸酯官能团。此类包覆剂可与金属颗粒形成弱键。因此，可降低断开该键所需的温度，这可有助于降低烧结温度。在这方面，包含胺官能团的包覆剂是特别优选的。优选地，包覆剂包含三乙醇胺，并且更优选地，包覆剂是三乙醇胺。三乙醇胺能特别有效地减少颗粒的团聚和/或氧化，而不会不利地影响有利的烧结特性。
该烧结粉末优选地包含至多1重量％包覆剂，更优选地0.1重量％至0.5重量％包覆剂，甚至更优选地0.2重量％至0.4重量％包覆剂。更低水平的包覆剂可导致不利的团聚或使得颗粒更容易氧化。更高水平的包覆剂可导致使用包覆剂形成的烧结接头中存在更高水平的残余包覆剂。这可降低接头的机械特性，特别是管芯剪切强度。由于这些颗粒具有比常规烧结粉末更大的粒度，因此减少团聚和/或提供合适抗氧化性所需的包覆剂的量少于常规烧结粉末。这可改善通过使用该烧结粉末形成的烧结接头的机械特性，因为烧结接头中存在的残余包覆剂的量将更少。
该烧结粉末可有利地呈粉末压坯的形式。这可使得更易将该烧结粉末定位在期望烧结接头的所需位置中。
在另外一个方面，提供了包含如本文所述的烧结粉末的烧结膏。
该烧结膏提供几乎所有与纳米银膏相同的有益效果，但成本低得多。该烧结膏展示出优异的热导率和电导率。例如，该烧结膏通常表现出至少1.0×106S/m，更通常至少1.5×106S/m，例如约1.8×106S/m的电导率。有利地，该膏体在室内环境条件下稳定。
该膏体可为可印刷的和/或可分配的和/或可喷射的和/或可针转印的和/或可丝网印刷的。该膏体可具有特别有利于分配的粘度和流动特性，这意味着该膏体可用作焊料的一对一替代品。
该烧结膏还可包含例如粘结剂、活化剂、分散剂和有机溶剂中的一者或多者。这些组分通常被选择为使得它们能够在低于该烧结粉末的目标烧结温度的温度下从该膏体去除(例如通过蒸发和/或烧尽)。这可有助于促进金属颗粒的近完全烧结。当有机材料在烧结期间保留在接头中时，可发生金属颗粒的不充分烧结。这可产生弱烧结接头。
优选地，该膏体包含70重量％至90重量％的烧结粉末，更优选地70重量％至87重量％。这可允许有利烧结特性与操纵特性的有利组合。
该膏体优选地包含1重量％至5重量％的粘结剂。该粘结剂可用于将该膏体粘结在一起以使得其更易操纵并且准确地定位在期望烧结接头的位置中。
该粘结剂优选地包含聚合物。适合用作粘结剂的聚合物是本领域中已知的。优选地，该粘结剂包含环氧基树脂，更优选地环氧甲基丙烯酸酯聚氨酯。环氧基树脂可特别有效地将该膏体粘结在一起以使得该膏体更易操纵并且可更易准确地定位在期望烧结接头的位置中。此外，环氧树脂的使用可使得在烧结之前形成更强接头，这意味着不需要在烧结之前将待接合的工件保持在一起。当包覆剂包含胺官能团时，环氧树脂的使用特别有利。在这种情况下，胺充当形成交联结构的硬化剂。这可在烧结之前产生特别强的接头。
该膏体优选地包含0.5重量％至3重量％的活化剂，更优选地1重量％至3重量％。可添加活化剂以从待印刷的表面去除可存在的任何金属氧化物和/或去除可存在于该烧结粉末中的任何氧化物。芳基羧酸或烷基羧酸可用作活化剂。优选地，活化剂包含二羧酸，更优选地丙二酸。
该膏体优选地包含0.5重量％至2重量％的分散剂。该分散剂通常包含表面活性剂。可将分散剂/表面活性剂添加到该烧结膏以帮助将该烧结粉末分散于该烧结膏中。特别合适的可商购获得的分散剂/表面活性剂的示例是BYK 163。
该膏体优选地包含10重量％至15重量％的有机溶剂。该有机溶剂优选地包含单萜醇(例如，萜品醇)和/或二醇(例如，三乙二醇)和/或二醇醚。单萜醇和/或二醇可特别有效地将金属颗粒分散在该膏体内，从而使得金属颗粒均匀分布于有机组分的基质中并且减少团簇凝聚和/或团聚。单萜醇和/或二醇的使用可用于增强该烧结膏的流动性和印刷性。该有机溶剂优选地包含萜品醇作为特别有效的溶剂。
该烧结膏可包含另外的物质。例如，可添加流变改性剂以控制该膏体的粘度。合适的流变改性剂的示例包括但不限于Thixcin R和Crayvallac Super。
在一个特别优选的实施方案中，该膏体包含：
70重量％至90重量％的烧结粉末，
1重量％至3重量％的活化剂，
0.5重量％至2重量％的分散剂，
10重量％至15重量％的有机溶剂，以及
任选地，1重量％至5重量％的粘结剂。
该膏体优选地为可印刷的和/或可分配的和/或可喷射的和/或可针转印的和/或可丝网印刷的。
在另外一个方面，本发明提供了包含本文所述的烧结膏的烧结膜。
在一个优选的实施方案中，将该膜预施加到晶片。在另一个优选的实施方案中，该膜位于聚合物衬底上。在另一个优选的实施方案中，该膜是自立式的。
在另外一个方面，本发明提供了制造烧结粉末的方法，该方法包括：
提供包含铜离子和包覆剂的溶液，
使该溶液与还原剂接触以提供该烧结粉末，并且
回收该烧结粉末。
该方法产生包含铜颗粒的烧结粉末。该方法产生包含具有有利窄粒度分布、通常具有大于或等于100nm的D10和小于或等于500nm的D90的铜颗粒的烧结粉末。所得的烧结粉末可特别适合用作例如用于管芯附接的烧结粉末，并且与常规铜烧结粉末相比，可表现出改善的抗氧化性。所得的烧结粉末可为本文所述的烧结粉末。本发明的以下方面的方法的优点和优选特征同样适用于该方面。
在另外一个方面，本发明提供了制造本文所述的烧结粉末的方法，该方法包括：
提供包含铜离子和包覆剂的溶液，
使该溶液与还原剂接触以提供该烧结粉末，并且
回收该烧结粉末。
由于该烧结粉末表现出抗氧化性，因此有利地，该方法可在非惰性气氛(诸如例如空气)中进行。
可将铜离子和包覆剂顺序地或同时地添加到溶剂以形成溶液。通常，在剧烈搅拌下将包覆剂滴加到铜离子的溶液。这可确保包覆剂良好地分散于溶液中，从而有助于将粒度控制在期望的范围内。
该溶液优选地为水溶液，诸如例如脱矿质水。
通常通过混合和搅拌来使该溶液和还原剂接触。在该步骤期间，该烧结粉末的颗粒从溶液中沉淀析出。
该溶液中的铜离子：包覆剂的摩尔比率优选地为1:1至10:1，更优选地2:1至7:1，甚至更优选地4:1至6:1。此类比率可有助于提供期望粒度的颗粒。例如，更高量的包覆剂可导致形成不合要求的小颗粒，而更低量的包覆剂可导致形成不合要求的大颗粒。
该溶液中的铜离子优选地以铜盐的形式提供。铜盐优选地包含乙酸铜。乙酸铜是特别合适的盐并且成本较低。
包覆剂优选地包含三乙醇胺。
该溶液优选地具有大于7的pH。大于7的pH可例如通过将氢氧离子添加到该溶液，例如通过添加NaOH和/或KOH来实现。大于7的pH可提供更有利的还原条件，从而提高产率。此外，大于7的pH可避免铜颗粒与酸的任何不利反应。
还原剂与铜离子的摩尔比率优选地大于1:1。过量的还原剂可增加产率。
还原剂优选地包含肼(例如，水合肼)。肼是特别合适的还原剂，并且能特别有效地产生所需粒度范围内的颗粒。
包含铜离子和包覆剂的溶液优选地与还原剂接触5小时至30小时，优选地10小时至20小时。更短时间可导致产率降低和/或形成不利的小颗粒。更长时间可导致形成不利的大颗粒。
回收通常包括以下步骤中的一个或多个步骤：从该烧结粉末滗析所得溶液(“母液”)，洗涤该烧结粉末并且干燥该烧结粉末。洗涤可例如依次用水和丙酮进行。干燥可例如在超过30℃(例如35℃)的温度下进行。
该方法优选地在非惰性气氛(诸如空气)中进行。这与制备常规铜烧结粉末的方法形成对比，后者易受氧化的影响。在非惰性气氛中进行该方法可降低该方法的复杂性和/或成本。
在另外一个方面，本发明提供了制造本文所述的烧结膏的方法，该方法包括：
提供本文所述的烧结粉末，并且
将该烧结粉末与有机溶剂及任选地活化剂、分散剂、包覆剂和粘结剂中的一者或多者混合。
该方法优选地还包括例如在三辊磨中研磨该烧结膏。这可改善该膏体的均匀性。在研磨之前的混合步骤期间添加附加包覆剂可减少研磨期间团聚的发生率。
该方法优选地还包括将该烧结膏流延成膜。合适的流延方法是本领域中已知的。
在另外一个方面，本发明提供了在两个或更多个工件之间形成接头的方法，该方法包括：
提供待接合的两个或更多个工件，
在该两个或更多个工件附近提供本文所述的烧结粉末和/或本文所述的烧结膏和/或本文所述的烧结膜。
干燥该烧结粉末和/或烧结膏和/或烧结膜，并且
加热该烧结粉末和/或烧结膏和/或烧结膜以至少部分地烧结该金属。
在一个优选的实施方案中，该两个或更多个工件包括管芯和衬底。
干燥步骤在加热步骤之前进行。干燥步骤可使得能够在烧结期间施加后续压力而不驱离(“挤出”)该粉末、膏体或膜。干燥步骤还有利于“无压烧结”，在该烧结中其用于防止加热步骤期间的任何驱离。
干燥优选地在30℃至100℃、更优选地40℃至80℃、甚至更优选地50℃至70℃的温度下进行。干燥优选地进行1分钟至60分钟，更优选地5分钟至40分钟，甚至更优选地10分钟至30分钟。
至少部分烧结引起接头的形成。加热通常引起金属的基本烧结，更通常金属的完全烧结。加热优选地在140℃至300℃、更优选地180℃至280℃的温度下进行。加热优选地进行至多15分钟，更优选地1分钟至8分钟，甚至更优选地2分钟至6分钟。更低温度和更短加热时间可导致不完全烧结，从而导致最终接头的不利机械特性和/或热特性和/或电特性。更高温度和更长加热时间可导致工件损坏。
加热可在压力下或无压力下(所谓“无压烧结”)进行。当加热在压力下进行时，优选地在加热期间施加2MPa至18MPa、更优选地3MPa至15MPa、甚至更优选地5MPa至13MPa、还甚至更优选地8MPa至12MPa的压力。更高压力可有利地需要更低加热温度和/或使得因改善的颗粒间接触而形成具有更有利的机械特性和/或热特性和/或电特性的接头。然而，如果压力太高，则存在工件损坏的风险。
在一个优选的实施方案中：
将烧结膏丝网印刷到待接合的工件中的一个或多个工件上以形成丝网印刷的图案；并且
将焊料施加到丝网印刷的图案，
任选地其中在施加焊料之前通过化学镀镍浸金(ENIG)技术来涂覆丝网印刷的图案。
丝网印刷的合适技术是本领域中已知的。该丝网印刷可使用例如筛孔筛(例如筛孔尺寸70)进行。该丝网印刷在两个或更多个工件附近提供烧结膏的步骤期间进行。可使用例如标准焊膏来施加焊料。作为烧结膏的结果，该焊接可表现出有利的铺展和焊接特征。该焊接和ENIG通常在干燥步骤和加热步骤之后进行。
任选地在施加焊料之前通过化学镀镍浸金(ENIG)技术来涂覆丝网印刷的图案。合适的化学镀镍浸金技术是本领域中已知的。化学镀镍浸金(ENIG)是一种用于印刷电路板的表面镀层。其由覆盖着浸金薄层的化学镍镀层组成，该浸金薄层保护镍免于氧化。ENIG具有优于更常规(和更便宜)表面镀层诸如HASL(焊料)的若干优点，包括优异的表面平面度(对于具有大BGA封装的PCB特别有用)、良好的抗氧化性以及对于未处理的接触表面(诸如薄膜开关和接触点)的可用性。
该两个或更多个工件优选地包括半导体或其他管芯元件和衬底。该衬底可包括例如DBC(直接粘结铜)。DPC(直接镀铜)、MCPCB(金属内核PCB)、FR4、铜引线框架、柔性PCB。
在典型工艺中，将该粉末和/或膏体和/或膜放置或丝网印刷在该衬底上，然后干燥。随后通常接着是经由例如管芯粘片机或取放机的管芯放置。之后通常使用例如Carver压机进行加热。然后通常在之后进行焊接和任选地ENIG。
在另外一个方面，本发明提供了本文所述的烧结粉末和/或本文所述的烧结膏和/或本文所述的膜在选自以下的方法中的用途：管芯附接；晶片至晶片粘结；气密和近气密密封；烧结包含烧结粉末和在背衬层上的膜中形成的粘结剂的膜；分配和产生互连线。
在另外一个方面，本发明提供了使用本文所述的烧结粉末和/或本文所述的烧结膏和/或本文所述的烧结膜形成的烧结接头。
与使用常规烧结粉末形成的接头相比，该烧结接头可表现出高剪切强度。
现在将结合以下非限制性附图来描述本发明，其中：
图1示出了根据本发明的合成铜粉末的FESEM图像(×10,000)。
图2示出了根据本发明的合成铜粉末的FESEM图像(×30,000)。
图3示出了5MPa和10MPa压力下的管芯剪切的箱线图和后固化的效应。
图4示出了250℃烧结温度、不同压力下的管芯剪切的箱线图。
图5示出了使用压力烧结在250℃及不同时间和压力烧结条件下的管芯附接之后的SEM横截面图像。
图6示出了使用压力烧结在200℃及不同时间和压力烧结条件下的管芯附接之后的SEM横截面图像。
现在将结合以下非限制性示例来描述本发明。
以下实施例中使用的材料按如下购买：一水合乙酸铜(II)购自飞世尔科技公司(Fischer Scientific)；三乙醇胺(85％)购自维沃化工公司(ViVochem)；氢氧化钠、肼(85％LR)、甲醇和丙酮购自SDFCL公司；并且脱矿质水购自斯百全化学公司(SpectrumChemicals)。
以下实施例中使用的装备如下：在Dage4000 PXY中执行管芯剪切；在Pro-cast薄带流延机(TC-71LC)流延膜；并且使用Carver压机(3891CEB.4NE1001)进行烧结。
实施例1：铜纳米颗粒的合成
将乙酸铜(100g)溶解于脱矿质水(1500ml)中。在剧烈搅拌下向乙酸铜的水溶液滴加三乙醇胺(20g)，然后搅拌该溶液30分钟。随后添加氢氧化钾/氢氧化钠(20g氢氧化钾溶于100ml水)以使该溶液呈碱性(pH>7)并且再对该溶液进行30分钟的搅拌。经由滴液漏斗向该混合物添加过量水合肼溶液(150ml)。由于该反应大量放热并且发生泡腾，应采取预防措施。从而，在水浴中进行该反应，其中该反应的温度保持在20℃和25℃之间。然后搅拌所得溶液6小时。反应混合物的颜色从蓝绿色变为橙色，随后最终变为浅棕色。然后让该溶液静置1小时以便让合成的铜颗粒沉降于底部，之后滗析所得溶液(母液)。随后用过量的水彻底洗涤合成的粉末以去除非期望的反应物。然后用丙酮洗涤经洗涤的粉末。在35℃干燥该粉末。
然后通过粉末扫描电子显微镜(SEM)和粉末X射线衍射(XRD)来表征合成的粉末。通过图像分析得出的D10大于或等于100nm并且D90小于或等于500nm。图1和图2示出了合成的颗粒的场发射扫描电子显微镜(FESEM)图像。FESEM示出了这些颗粒具有不同形状并且具有在200nm至400nm范围内的窄粒度分布。不希望受理论的约束，认为铜纳米颗粒的更大粒度会使它们比常规烧结粉末中的铜纳米颗粒更抗氧化。
还使用粒度分析仪(PSA)来确定粒度，结果显示在150nm与350nm之间的范围内的非常一致且窄的粒度分布，这与SEM相符。
实施例2：铜纳米膏的制备
实施例2.1：
使用高速混合器(1000rpm，1分钟)利用环氧甲基丙烯酸酯聚氨酯(0.279g)分散上述合成的纳米铜粉末(24g)。向该分散体中添加三乙醇胺(85％，0.279g)、BYK 163(0.558g)、丙二酸(1.116g)和萜品醇(1.674g)并且使用高速混合器以1000rpm共混1分钟。然后使用EXAKT三辊磨彻底研磨所得混合物。随后在标准温度和压力(STP)下储存所收集的均匀可印刷膏体。
实施例2.2：
使用高速轨道混合器利用环氧甲基丙烯酸酯聚氨酯(0.70g)分散上述合成的纳米铜粉末(15g)。向该分散体中添加BYK(0.70g)。将丙二酸的甲醇溶液(1.41g丙二酸溶于1.41g甲醇)添加到该分散体，之后添加萜品醇(1.5g)。然后将该混合物放入高速轨道混合物中并且在三辊磨中研磨数分钟以提供均匀膏体。
实施例2.3：
使用高速轨道混合器利用环氧甲基丙烯酸酯聚氨酯(0.754g)分散上述合成的纳米铜粉末(15g)。向该分散体中添加BYK(0.754g)。将丙二酸(1.51g)添加到该分散体，之后添加萜品醇(2.64g)。然后将该混合物放入高速轨道混合物中并且在三辊磨中研磨数分钟以提供均匀膏体。
实施例2.4：
使用高速轨道混合器利用环氧甲基丙烯酸酯聚氨酯(0.754g)分散上述合成的纳米铜粉末(15g)。向该分散体中添加BYK(0.754g)。将丙二酸(1.51g)添加到该分散体，之后添加甲酸(1.511g)和萜品醇(2.64g)。然后将该混合物放入高速轨道混合物中并且在三辊磨中研磨数分钟以提供均匀膏体。
上述合成的铜膏的电导率为约1.8×106S/m。
实施例3：膜流延工艺
借助于薄带流延机在聚对苯二甲酸乙二醇酯(PET)膜上流延铜膏。膜的厚度被设定为75μm。使铜膏在100℃穿过薄带流延机。膜的流延时间为约25分钟。流延的膜的厚度为约50μm至60μm。
实施例4：管芯上膜转移工艺
使用Datacon管芯粘片机实现管芯上膜转移(DTF)工艺。3mm×3mm覆金硅管芯的冲压条件如下表1：
冲压压力(MPa) 冲压温度(℃) 冲压时间(s)
5 200-225 1-10
表1
将膜完全转移到管芯侧上而PET衬底上未留下铜膜。然后使用Tresky管芯粘片机在以下表2中的条件下将覆铜Si管芯附接到覆金/铜直接粘结铜(DBC)：
冲压压力(MPa) 冲压温度(℃) 冲压时间(s)
5-10 300 100
表2
图3中示出了从上述条件获得的管芯剪切。在图3中，后固化条件为在300℃的温度下保持30分钟。在有和没有后固化的情况下5MPa烧结压力下的管芯剪切分别为约14MPa和约20MPa。在有和没有后固化的情况下10MPa烧结压力下的管芯剪切分别为约24MPa和约30MPa。可以清楚看出，当载体以300℃后固化30分钟时，接头强度出现急剧增加。失效模式是本体失效，而不论使用的是何种条件。
实施例5：使用Carver压机对2英寸镀金硅晶片的晶片层压
将Carver压机的两个压台保持在175℃。通过使用5MPa至10MPa压力来进行硅晶片的层压。硅橡胶用作层压的缓冲效应。层压的停留时间为约3分钟。膜的冲压部分显示PET片材上没有留下膜。然后将层压的晶片安装在UV胶带上并且使用切块机进行切块。
之后使用Carver压机将切块的3mm×3mm管芯附接到覆Au/Cu的DBC。当烧结压力为5MPa时，实现约30MPa至32MPa的接头强度。而当在250℃下烧结压力为约10MPa并保持3分钟停留时间时，实现40MPa的接头强度。
图4示出了250℃烧结温度、不同压力下的管芯剪切的箱线图。在图4中，第一温度、压力和时间烧结条件分别为250℃、5MPa和3分钟。第二温度、压力和时间烧结条件分别为250℃、10MPa和3分钟。5MPa和10MPa烧结压力下的管芯剪切分别为约31MPa和约40MPa。
实施例6：用于自立式膜的工艺
使用Carver压机制备自立式铜膜。将流延膜以200℃在5MPa至10MPa压力下压制在硅晶片上方。停留时间为约2分钟。铜膜呈现硅晶片的形状并且未扩散到硅中，继而使得膜脱离聚合物衬底，得到约30μm至40μm厚度的自立式膜。当9V电池连接在纳米铜膜的两端时，该膜的导电性引起LED发光。测得该膜的电阻率为2×10-8Ω.m。
实施例7：使用压力烧结的纳米铜膏管芯附接
可通过以下方式完成半导体或其他管芯元件的附接：将纳米铜膏印刷到衬底诸如直接粘结铜(DBC)、直接镀铜(DPC)、金属内核印刷电路板(MCPCB)、FR4、铜引线框架、柔性PCB上，之后通过在60℃下加热印刷衬底20分钟来干燥印刷区域。然后该工艺之后是经由管芯粘片机或取放机的管芯放置，并且使用压力烧结在Carver压机中烧结。
使用3mm×3mm覆金硅管芯并分别使用5MPa和10MPa的烧结压力、3分钟和5分钟的烧结时间以及200℃和250℃的烧结温度在DBC上评价烧结铜接头的接头强度。在管芯放置之后，接着用铝箔覆盖整个组件，这将防止铜氧化。使用保持在硅管芯上方的0.5mm厚度的石墨片来提供缓冲效应。已观察到，与更高烧结压力和温度相比，在更低烧结压力(5MPa)和温度(烧结时间为3分钟)下，接头强度更小。
测试了不同烧结温度和压力对接头强度的影响。结果汇总于下表3中。表3示出了不同烧结温度和压力对接头强度的影响。应当注意，在更高烧结温度和时间下，大部分管芯粉碎，这揭示了接头强度太好而无法从衬底剪切管芯这一事实。此外，这还揭示了铜在两个界面上的强扩散。
烧结时间(分钟) 烧结温度(℃) 烧结压力(MPa) 管芯剪切(MPa)
3 200 5 约19
3 200 10 约29
3 250 5 约32
3 250 10 约39
5 200 5 约28
5 200 10 约43
5 250 5 约31
5 250 10 约45
表3
铜在这些界面上的扩散还得到了SEM横截面的证实，该SEM横截面显示铜纳米颗粒在烧结层内的极好致密化以及纳米颗粒在两个界面上的优异扩散，从而引起本体失效。可以清楚看出，铜纳米颗粒在10MPa的扩散和致密化比5MPa烧结压力好得多。这可以在图5和图6的SEM横截面中看出。在图5中，顶部两行横截面图像示出了界面比较；顶部行是管芯-铜层界面并且中间行是铜层-衬底界面。底部行横截面图像示出了铜层的微结构比较。每列横截面图像举例说明了不同组时间和压力烧结条件。第一列和第二列中及第三列和第四列中的烧结压力分别为5MPa和10MPa。第一列和第三列中及第二列和第四列中的烧结时间分别为3分钟和5分钟。在图6中，顶部两行横截面图像示出了界面比较；顶部行是管芯-铜层界面并且中间行是铜层-衬底界面。底部行横截面图像示出了铜层的微结构比较。每列横截面图像举例说明了不同组时间和压力烧结条件。第一列中及第二列和第三列中的烧结压力分别为5MPa和10MPa。第二列中及第一列和第三列中的烧结时间分别为3分钟和5分钟。
还可通过以下方式完成此类半导体和管芯元件的附接：由所述材料制成的管芯背面上的DTF和层压，之后是管芯放置和使用压力的烧结。
晶片层压的主要优点是消除了丝网印刷，这在机械和人力方面带来了额外优势。然后使用切块机对切块的覆铜硅晶片进行切单，并且使用Carver压机在10MPa和5MPa压力下将该覆铜硅晶片附接到DBC达3分钟。已观察到，管芯剪切分别为约30MPa至40MPa。
已观察到，在10MPa压力下，大部分硅管芯粉碎，这再次证明了管芯与衬底的优异粘结强度。不受理论的约束，认为随着烧结压力的增加，纳米颗粒逐渐彼此接触，继而增加了纳米颗粒的接触点，使得颗粒更好地融合，从而实现优异的接头强度。
实施例8：陶瓷、FR4和PET衬底上的纳米铜膏粘附力
测试了纳米铜膏在陶瓷、FR4和PET上的粘附力。使用DEK印刷机将该膏体印刷在各种衬底上，然后在箱式炉中以1700℃在氮气下固化30分钟。随后通过典型刮痕-胶带测试方法来测试印记。对陶瓷和FR4的粘附力被分类为5B，而对PET的粘附力被分类为4B。
实施例9：丝网印刷和焊接
合成的纳米铜膏还具有被丝网印刷的能力。使用筛孔筛对该膏体进行丝网印刷。使用DEK印刷机中筛孔尺寸为70的筛网来制作设计图案。
然后对丝网印刷的纳米铜图案进行化学镀镍浸金(ENIG)涂覆，之后用标准焊膏进行焊接。该焊接显示出极好的铺展但在一些地方可见片式元件间焊球。
此外，已探讨了在由合成的纳米铜膏印刷在裸露的FR4试件上的铜印记上的焊接的可能性。使用标准焊膏进行纳米铜上的焊接。在无ENIG涂覆的情况下的铜印记上的焊接也表现出良好铺展和良好焊接特征。
上述详细描述已经通过解释和说明的方式提供，并且不旨在限制所附权利要求的范围。本文示出的本发明优选实施方案的许多变型形式对于本领域的普通技术人员而言将是显而易见的，并且仍然在所附权利要求及其等同物的范围内。

Claims (61)

1.一种包含铜颗粒的烧结粉末，其中：
所述颗粒至少部分地涂覆有包覆剂，
所述颗粒表现出大于或等于100nm的D10和小于或等于2000nm的D90；并且所述包覆剂包含三乙醇胺。
2.根据权利要求1所述的烧结粉末，所述烧结粉末用于管芯附接。
3.根据权利要求1或2所述的烧结粉末，所述烧结粉末包含至多1重量％包覆剂。
4.根据权利要求1或2所述的烧结粉末，所述烧结粉末包含0.1重量％至0.5重量％包覆剂。
5.根据权利要求1或2所述的烧结粉末，所述烧结粉末包含0.2重量％至0.4重量％包覆剂。
6.根据权利要求1或2所述的烧结粉末，其中所述颗粒表现出小于或等于1000nm的D90。
7.根据权利要求1或2所述的烧结粉末，其中所述颗粒表现出小于或等于500nm的D90。
8.根据权利要求1或2所述的烧结粉末，其中所述颗粒表现出小于或等于450nm的D90。
9.根据权利要求1或2所述的烧结粉末，其中所述颗粒表现出大于或等于125nm的D10和小于或等于450nm的D90。
10.根据权利要求1或2所述的烧结粉末，其中所述颗粒表现出大于或等于150nm的D10和小于或等于400nm的D90。
11.根据权利要求1或2所述的烧结粉末，所述烧结粉末呈粉末压坯的形式。
12.一种烧结膏，所述烧结膏包含根据权利要求1至11中任一项所述的烧结粉末。
13.根据权利要求12所述的烧结膏，其中所述膏包含70重量％至90重量％的所述烧结粉末。
14.根据权利要求12或权利要求13所述的烧结膏，其中所述膏包含1重量％至5重量％的粘结剂。
15.根据权利要求14所述的烧结膏，其中所述粘结剂包含环氧甲基丙烯酸酯聚氨酯。
16.根据权利要求12或13所述的烧结膏，其中所述膏包含0.5重量％至3重量％的活化剂。
17.根据权利要求12或13所述的烧结膏，其中所述膏包含1重量％至3重量％的活化剂。
18.根据权利要求16所述的烧结膏，其中所述活化剂包含二羧酸。
19.根据权利要求18所述的烧结膏，其中所述二羧酸包含丙二酸。
20.根据权利要求12或13所述的烧结膏，其中所述膏包含0.5重量％至2重量％的分散剂。
21.根据权利要求20所述的烧结膏，其中所述分散剂包含表面活性剂。
22.根据权利要求12或13所述的烧结膏，其中所述膏包含10重量％至15重量％的有机溶剂。
23.根据权利要求22所述的烧结膏，其中所述有机溶剂包含萜品醇。
24.根据权利要求12或13所述的烧结膏，其中所述膏包含：
70重量％至90重量％的所述烧结粉末，
1重量％至3重量％的活化剂，
0.5重量％至2重量％的分散剂，
10重量％至15重量％的有机溶剂，以及
任选地，1重量％至5重量％的粘结剂。
25.根据权利要求12或13所述的烧结膏，其中所述膏是可印刷的和/或可分配的和/或可喷射的和/或可针转印的。
26.根据权利要求12或13所述的烧结膏，其中所述膏是可分配的和/或可喷射的和/或可针转印的和/或可丝网印刷的。
27.一种烧结膜，所述烧结膜包含根据权利要求12至26中任一项所述的烧结膏。
28.根据权利要求27所述的烧结膜，其中将所述膜预施加到晶片。
29.根据权利要求27所述的烧结膜，其中所述膜位于聚合物衬底上。
30.根据权利要求27所述的烧结膜，其中所述膜是自立式的。
31.一种制造根据权利要求1至11中任一项所述的烧结粉末的方法，所述方法包括：
提供包含铜离子和包覆剂的溶液，
使所述溶液与还原剂接触以提供所述烧结粉末，并且
回收所述烧结粉末，
其中所述包覆剂包含三乙醇胺。
32.根据权利要求31所述的方法，其中所述溶液中的铜离子:包覆剂的摩尔比率为1:1至10:1。
33.根据权利要求31所述的方法，其中所述溶液中的铜离子:包覆剂的摩尔比率为2:1至7:1。
34.根据权利要求31所述的方法，其中所述溶液中的铜离子:包覆剂的摩尔比率为4:1至6:1。
35.根据权利要求31或权利要求32所述的方法，其中所述溶液中的所述铜离子以铜盐的形式提供，并且所述铜盐包含乙酸铜。
36.根据权利要求31或32所述的方法，其中所述溶液具有大于7的pH。
37.根据权利要求31或32所述的方法，其中还原剂与铜离子的摩尔比率大于1:1。
38.根据权利要求31或32所述的方法，其中所述还原剂包含肼。
39.根据权利要求31或32所述的方法，其中包含铜离子和包覆剂的所述溶液与所述还原剂接触5小时至30小时。
40.根据权利要求31或32所述的方法，其中包含铜离子和包覆剂的所述溶液与所述还原剂接触10小时至20小时。
41.根据权利要求31或32所述的方法，其中回收包括以下步骤中的一个或多个步骤：从所述烧结粉末滗析所得溶液，洗涤所述烧结粉末并且干燥所述烧结粉末。
42.根据权利要求31或32所述的方法，其中所述方法在非惰性气氛中进行。
43.根据权利要求31或32所述的方法，其中所述方法在空气中进行。
44.一种制造根据权利要求12至26中任一项所述的烧结膏的方法，所述方法包括：
提供根据权利要求1至11中任一项所述的烧结粉末，并且
将所述烧结粉末与有机溶剂及任选地活化剂、分散剂、包覆剂和粘结剂中的一者或多者混合。
45.根据权利要求44所述的方法，所述方法还包括研磨所述烧结膏。
46.根据权利要求44或权利要求45所述的方法，所述方法还包括将所述烧结膏流延成膜。
47.一种在两个或更多个工件之间形成接头的方法，所述方法包括：
提供待接合的两个或更多个工件，
在所述两个或更多个工件附近提供根据权利要求1至11中任一项所述的烧结粉末和/或根据权利要求12至26中任一项所述的烧结膏和/或根据权利要求27至30中任一项所述的烧结膜，
干燥所述烧结粉末和/或所述烧结膏和/或所述烧结膜，并且
加热所述烧结粉末和/或所述烧结膏和/或所述烧结膜以至少部分地烧结金属。
48.根据权利要求47所述的方法，其中所述两个或更多个工件包括管芯和衬底。
49.根据权利要求47或48所述的方法，其中所述干燥在30℃至100℃的温度下进行。
50.根据权利要求47或48所述的方法，其中所述干燥在40℃至80℃的温度下进行。
51.根据权利要求47或48所述的方法，其中所述干燥在50℃至70℃的温度下进行。
52.根据权利要求49所述的方法，其中所述干燥进行1分钟至60分钟。
53.根据权利要求49所述的方法，其中所述干燥进行5分钟至40分钟。
54.根据权利要求49所述的方法，其中所述干燥进行10分钟至30分钟。
55.根据权利要求47或48所述的方法，其中在所述加热步骤期间施加2MPa至18MPa的压力。
56.根据权利要求47或48所述的方法，其中在所述加热步骤期间施加3MPa至15MPa的压力。
57.根据权利要求47或48所述的方法，其中在所述加热步骤期间施加5MPa至13MPa的压力。
58.根据权利要求47或48所述的方法，其中在所述加热步骤期间施加8MPa至12MPa的压力。
59.根据权利要求47或48所述的方法，其中：
将所述烧结膏丝网印刷到待接合的所述工件中的一个或多个工件上以形成丝网印刷的图案；并且
将焊料施加到所述丝网印刷的图案，
任选地其中在施加所述焊料之前通过化学镀镍浸金(ENIG)技术来涂覆所述丝网印刷的图案。
60.根据权利要求1至11中任一项所述的烧结粉末和/或根据权利要求12至26中任一项所述的烧结膏和/或根据权利要求27至30中任一项所述的膜在选自以下的方法中的用途：管芯附接；晶片至晶片粘结；气密或近气密密封；烧结包含烧结粉末和在背衬层上的膜中形成的粘结剂的膜；分配和产生互连线。
61.一种烧结接头，所述烧结接头使用根据权利要求1至11中任一项所述的烧结粉末和/或根据权利要求12至26中任一项所述的烧结膏和/或根据权利要求27至30中任一项所述的烧结膜来形成。
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