CN106457404A - 用于制造金属粉末的方法 - Google Patents

用于制造金属粉末的方法 Download PDF

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Publication number
CN106457404A
CN106457404A CN201580020718.XA CN201580020718A CN106457404A CN 106457404 A CN106457404 A CN 106457404A CN 201580020718 A CN201580020718 A CN 201580020718A CN 106457404 A CN106457404 A CN 106457404A
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acid
silver
metal
copper
sintered
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CN201580020718.XA
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CN106457404B (zh
Inventor
R·P·赛特纳
N·K·查奇
P·S·罗伊
S·萨尔卡尔
S·慕克吉
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Alpha Assembly Solutions Inc
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Alpha Metals Inc
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    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract

一种用于制造金属粉末的方法，包括：提供碱性金属盐溶液；使该碱性金属盐溶液与还原剂接触以从其中沉淀出金属粉末；以及从溶剂中回收所沉淀的金属粉末。

Description

用于制造金属粉末的方法
技术领域
本发明涉及一种用于制造金属粉末的方法，以及根据该方法制造的金属粉末。
背景技术
烧结接头提供了焊接接头的替代品。形成烧结接头的典型方法包括将金属粉末(通常为粉末压块的形式)放置在待接合的两个工件之间，然后烧结该金属粉末。由此引起的金属原子的原子扩散形成两个工件之间的结合。
金属纳米粉末已被用于形成电子工业中的烧结接头，并且被认为是无铅焊接的有用替代品。纳米材料和相应粒状材料之间的不同行为被认为是由于纳米材料具有较高的表面积与体积之比。
含银纳米颗粒的烧结粉末是已知的。由银纳米颗粒的原子扩散形成的烧结接头可以在比粒状材料的熔融温度显著低的温度下进行处理，并且还可用于高温应用。诸如高温稳定性、高导电性和导热性以及良好的机械性能的潜在优势使这种烧结粉末成为管芯连接应用的有前途的候选者。然而，这种烧结粉末的烧结温度，对于大多数电子应用的有效利用来说仍然过高。
烧结温度可以通过在烧结过程中施加外部压力而降低。银膏的压力辅助低温烧结已被证明是回流焊接的一种可行的替代以作为管芯连接方法。高压的应用已经显示出显著降低烧结温度，而用于管芯连接的所需特性可以相对快的速率来实现，使得在几分钟内形成烧结接头。然而，大的外部压力使得方法的自动化困难。此外，大的外部压力的施加会导致对工件的损坏。
已知分配焊膏用于各种应用，但当波峰焊或丝网印刷不可能时主要是作为一种替代。焊膏可以在各种表面贴装应用中分配在印刷电路板、集成电路封装和电元件连接器上。锡膏的典型问题包括：滴漏、跳点和点胶不一致。软硬焊料通常在电子行业中用于管芯连接和点胶。软焊料在热循环条件下容易疲劳失效。另一方面，硬焊料和玻璃基质复合材料用于使设备能于更高结温运行，但是其较高的弹性模量和处理温度可在设备中产生高的机械应力，并且这些材料还具有相对低的导热性和导电性。
发明内容
本发明的目的是解决与现有技术相关的问题中的至少一些或为此至少提供一种商业上可接受的替代的解决方案。
在第一方面，本发明提供了一种用于制造金属粉末的方法，包括：
提供碱性金属盐溶液；
使该碱性金属盐溶液与还原剂接触以从其中沉淀出金属粉末；以及
从溶剂中回收所沉淀的金属粉末。
除非明确有相反的指示，如本文所定义的各个方面或实施方案可与任何其他(多个)方面或(多个)实施方案进行组合。特别是，任何指示为优选或有利的特征可与任何指示为优选或有利的其他特征相结合。
本文所用术语“烧结粉末”可包括能够形成烧结接头的粉末。烧结接头由放置在待接合的两个工件之间的金属颗粒的原子扩散形成。术语“烧结粉末”可包括粒状物。烧结粉末可包括规则形状的颗粒(如，例如球)或不规则形状的颗粒(如，例如晶须、板、棒或薄片)。
本文所用术语“封端剂”可包括这样一种物种，当其存在于金属颗粒表面上时，其减少金属颗粒的附聚，在粉末生产过程中能进行粒度控制，并减少颗粒表面氧化或其他污染。
本发明人出乎意料地发现，根据该方法制造的金属粉末可显示出大于2g/cm3，典型地大于3g/cm3，更典型地3.5～5.5g/cm3的振实密度。减小振实密度会导致增加的颗粒聚集。因此，通过本文中所描述的方法制造的粉末易于处理，并且可用于形成精细线路。减小振实密度可能会导致不利的非紧凑而多孔的烧结接头。振实密度可通过使用振实密度计以标准程序来测量。
金属粉末的粒度通常是微米级，并会表现出提供特别有利的烧结特性的粒度分布。例如，粉末通常显示出500nm至10μm的D50。D50可通过使用动态光散射法或激光散射法用粒度分析仪进行测定。有利的是，构成粉末的大多数颗粒具有100nm到50μm，优选100nm至30μm的最长尺寸。通常，基本上所有构成粉末的颗粒都具有这些范围内的最长尺寸。当颗粒是球形时，最长尺寸将是球的直径。
由金属粉末显示出的大小，粒度和形状分布以及堆积密度值的组合可以使粉末特别有效地在例如高密度、低孔隙率的烧结金属接头的制造中用作烧结粉末。这种接头可以扩展工业和汽车应用所需的现代动力模块的功率和热循环性能。
本发明人已出乎意料地发现，根据本发明的方法制造的粉末可以在相对低的温度下，只需施加非常低的压力，典型地基本上无压力进行烧结。其结果是，使用金属粉末在工件之间形成的烧结接头可减少工件的损伤发生。另外，由于不需要施加高压力，烧结接头的形成可简化，并且可更容易实现自动化。此外，相对于纳米尺度的颗粒，金属颗粒的附聚可通过仅使用少量封端剂而得以避免。因此，相对于仅包括纳米尺度颗粒的烧结粉末，包含在所得烧结接头中的残余有机物的量减少，从而改善了接头的机械性能。
碱性金属盐溶液一般是水溶液，并且通常表现出大于7，更典型地大于约7.5，甚至更优选约8的pH。高pH值可由含金属的氢氧化物例如氢氧化钠的存在提供。或者，或此外，高pH值可由有机叔碱例如三乙胺的存在提供。
特别合适的金属盐溶液是一种金属硝酸盐溶液。金属硝酸盐溶液的例子包括例如硝酸银溶液和硝酸铜溶液。金属硝酸盐溶液可以包含表面活性剂，例如DAXAD。
构成金属粉末的金属颗粒可全都包含相同的金属。或者，一些颗粒可包含不同的金属。此外，个别颗粒可包含两种或更多种不同的金属。本文所用术语“金属”可包括合金或核-壳结构。因此，颗粒可包含一种或多种金属的一种或多种合金或核-壳结构。
颗粒的形状使得所得金属粉末为球形的、多面的、不规则的、片状的或两种或更多种这些形状的组合。
所沉淀的金属粉末可通过例如过滤和/或倾析和/或离心分离从溶剂中回收。然后可使过滤的和/或倾析的和/或离心分离的金属粉末经受例如洗涤和/或干燥。
还原剂优选包含肼、甲醛和硼氢化物中的一种或多种。这样的还原剂对于提供所得金属粉末的良好粒度分布和振实密度值特别有效。在这方面，包含肼和氢氧化物的组合的还原剂是特别优选的。这是出乎意料的，因为按本领域的理解，肼的使用通常导致纳米尺度颗粒的形成。不受理论的束缚，可以认为，氢氧化物的存在与肼组合，并且在反应介质中(初始)不存在任何封端剂，会减慢反应速率，并通过奥斯特瓦尔德熟化过程增强较大颗粒的生长，从而导致具有良好粒度分布的微米尺度颗粒而不是纳米尺度颗粒的形成。进一步认为，延迟加入封端剂(见下文)将导致颗粒聚集的良好粒度分布。合适的还原剂的例子包括例如水合肼、碱性福尔马林溶液和硼氢化钠。
优选的是，该方法进一步包括在使该碱性金属盐溶液与该还原剂接触之后，使该碱性金属盐溶液与封端剂接触。换句话说，封端剂优选在还原剂已被添加到溶液中之后，但在所沉淀的金属颗粒从溶剂中回收之前添加。封端剂可至少部分地涂覆在构成金属粉末的颗粒的表面上，并因此可有助于减少颗粒的不受控制的附聚。高程度的不受控制的附聚是不利的，因为它会降低振实密度，并会导致非紧凑而多孔的烧结接头。封端剂的使用可有助于避免金属的降解，例如因金属暴露于空气而造成的损害。此外，在添加还原剂之后添加封端剂可有助于产生良好的粒度分布和振实密度值。封端剂优选在还原剂之后至少1秒，更优选在还原剂之后至少2秒，甚至更优选2～600秒，还更优选3～120秒再与溶液接触。在一个特别优选的实施方案中，封端剂在还原剂之后约5秒再与溶液接触。
封端剂可以包含例如脂肪酸，以及酯、酰胺、胺、表面活性剂和/或聚合物。封端剂优选包含脂肪酸，更优选月桂酸、棕榈酸、硬脂酸、异硬脂酸和油酸中的一种或多种。这种封端剂对于防止构成金属粉末的金属颗粒的聚集特别有效。
该方法优选还包括研磨所回收的沉淀的金属粉末。这种研磨会导致构成金属粉末的具有平的或“薄片状”形状的颗粒的比例增加。例如，该粉末可典型地包含至少10体积％，更典型地20～80体积％的具有薄片状形状的颗粒。增加的研磨时间会增加薄片状颗粒的比例和长宽比。与包含球形的粉末相比，具有这样的粒度分布并具有高比例薄片状颗粒的粉末会显示出增强的紧凑性，并会由此显示出更有利的烧结特性。此外，包含这种粉末的膏料会表现出提高的粘度，并因此会更容易处理。此外，具有这种粉末的膏料与仅由球体状颗粒制成的具有较低的振实密度的膏料相比，由于存在具有合适粒度、长宽比、分布和振实密度的薄片状颗粒而显示出增强的对衬底和工件的润湿行为。润湿性的提高对于形成两个工件之间牢固的结合是非常重要的，所述牢固的结合因烧结过程中金属原子的原子扩散而致。薄片形状与本文所述的振实密度、粒度和长宽比的分布的组合导致金属粉末表现出特别有利的烧结特性。
研磨优选使用球磨机进行。球磨机的使用对于增加薄片状颗粒的比例的同时保持有利的粒度分布和振实密度值是特别有效的。使用氧化锆珠粒的立式搅拌(attritor)球磨机是合适的球磨机的例子。优选的珠粒直径包括例如0.05mm～2mm，优选约0.1mm。
研磨优选在脂肪酸，优选月桂酸、棕榈酸、硬脂酸、异硬脂酸和油酸中的一种或多种的存在下；和/或在聚合物，优选PEG 400的存在下；和/或在多胺，优选三亚乙基四胺的存在下进行。这些物质可以在研磨期间用作封端剂，从而用于在研磨期间并在使用之前减少粉末的聚集和/或氧化。
研磨优选进行至少30分钟，优选至少90分钟。增加的研磨时间可以增加具有薄片状形状的颗粒的比例。
金属优选包含银、铜和它们的一种或多种的合金中的一种或多种。这种金属表现出高的导电性和导热性，因此当粉末用于电子应用如管芯连接和微电子封装时是特别有利的。合适的银合金包括例如AgSn、AgPd、AuAg、AgCu和AgNi。金属颗粒可包括涂银颗粒的核-壳结构，例如涂银的铜、涂银的镍、涂银的CuNi、涂银的CuNiZn和涂银的BN。
当颗粒包含银时，粉末可以有利地表现出如下的粒度分布：3～6μm，优选4～5.5μm的D90；和/或0.9～2μm，优选1～1.8μm的D50；和/或0.3～0.8μm，优选0.5～0.75μm的D10。当颗粒包含铜时，粉末可有利地表现出如下的粒度分布：4～15μm，优选10～13μm的D90；和/或2～10μm，优选4～6μm的D50；和/或0.5～3μm，优选1.5～2.5μm的D10。结合有利的振实密度值，这可使粉末能用于制造高密度和低孔隙率的烧结接头。铜颗粒可以是多面的。
在一个特别优选的实施方案中，
该金属包含银；并且
该还原剂包含肼，
该方法还包括：
在使该碱性金属盐溶液与该还原剂接触之后，使该碱性金属盐溶液与油酸封端剂接触；以及
在油酸封端剂的存在下，使用球磨机研磨所回收的沉淀的金属粉末至少30分钟。
通过这种方法制造的金属粉末显示出特别有利的颗粒粒度分布和振实密度值，并且可显示出以上所讨论的有利的粒度分布。
当金属包含铜时，该方法优选还包括在构成粉末的颗粒上施加银涂层。这种涂银的铜颗粒以铜颗粒的相对较低成本表现出银颗粒的高导电性和导热性。涂银的铜颗粒优选显示出如下的粒度分布：4～13μm，优选9～12μm的D90；和/或1～10μm，优选4～5.5μm的D50；和/或0.5～3μm，优选2～2.8μm的D10。
施加银涂层优选包括：
从铜颗粒上蚀刻氧化物层；以及
使用电镀在铜颗粒上施加银涂层。
这种方法在涂覆铜颗粒时特别有效。在一个实施方案中，蚀刻使用多胺例如三亚乙基四胺来进行，并且电镀是在溶解于去离子水和柠檬酸中的水溶性银盐的存在下进行。在一个替代实施方案中，使用硫酸铵和氢氧化铵的组合，接着用多胺例如三亚乙基四胺处理而进行两步蚀刻。
该方法优选还包括在涂银颗粒上施加脂肪酸涂层。脂肪酸涂层用作封端剂，从而可用于减少构成金属粉末的金属颗粒的附聚和/或氧化。
另一方面，本发明提供了一种制造铜粉末的方法，包括：
提供铜粉末；以及
在聚合物和/或多胺的存在下，使用球磨机研磨该铜粉末。
所得铜粉可主要包含显示出“薄片状”形状的颗粒。所得粉末可具有500nm至10μm的d50值和/或大于2g/cm3的振实密度。聚合物可包含例如PEG 400和/或多胺，例如三亚乙基三胺。
另一方面，本发明提供了根据本文所述的方法制造的金属粉末。
另一方面，本发明提供了一种金属粉末，其具有：
500nm至10μm的d50；以及
大于2g/cm3的振实密度，
其中该金属粉末包含银、铜和它们的一种或多种的合金中的一种或多种。
由金属粉末表现出的粒度分布和振实密度值的组合可以使得粉末特别有效地例如在制造高密度、低孔隙率的烧结金属接头中用作烧结粉末。
金属粉末可有利地具有低水平的有机物，例如小于5重量％有机物，优选小于3重量％有机物，更优选小于1重量％有机物，更优选小于0.5重量％有机物。(本文中使用的术语重量％有机物是指通过热或化学分析测量的碳的重量％)
金属粉末可以有利地显示出低的比表面积(BET)，例如小于1.5m2/g，优选小于1m2/g，更优选小于0.8m2/g。
另一方面，本发明提供了一种使用如本文所述的金属粉末形成的烧结接头。这种烧结接头可以显示出特别高的强度和/或特别高的电导率和热导率。此外，烧结接头可在热冲击后表现出非常小的剪切强度变化，通常基本上没有剪切强度的变化。
另一方面，本发明提供了LED(发光二极管)、MEMS(微机电系统)、OLED(有机发光二极管)、PV电池(光伏电池)、电力电子或聚合物上的印刷电子或其他包括本文所述的烧结接头的柔性或可成形衬底。
另一方面，本发明提供一种烧结膏，其包含：
如本文所述的金属粉末；
粘合剂；
溶剂；和
任选的流变改性剂和/或有机银化合物和/或活化剂和/或表面活性剂和/或润湿剂和/或过氧化氢或有机过氧化物。
膏料可以是可印刷的和/或可分配的和/或可喷射的和/或可引脚(pin)转移的。膏料可具有特别有利于分配的粘度和流动特性，这意味着膏料可用作焊料的一对一替代品。
与本领域已知的烧结膏相比，本发明的烧结膏在室温下表现出高的稳定性。这意味着不需要烧结膏的低温存储。这是本发明的烧结膏的特别重要的优点。
通常选择粘合剂和/或溶剂使得它们能够在低于烧结粉末的目标烧结温度的温度下从膏料中除去(例如通过蒸发和/或烧尽)。这可有助于促进金属颗粒的几乎完全烧结。当在烧结期间有机材料保留在接头中时，会发生金属颗粒的不充分烧结。这会导致弱的烧结接头。
粘合剂可以用于将膏料粘合在一起，使得其更容易处理并在所需烧结接头的位置精确定位。合适的粘合剂的例子包括但不限于热塑性聚合物，例如聚(甲基丙烯酸甲酯)、聚酰胺、聚乙烯、聚丙烯、聚苯乙烯；或热固性聚合物，例如聚氨酯、聚氰脲酸酯、环氧树脂、聚酰亚胺、三聚氰胺树脂和双马来酰亚胺树脂。特别优选的例子包括羟丙基甲基纤维素、三醋精和聚乙酸乙烯酯。优选地，粘合剂包含环氧基树脂。环氧基树脂可特别有效地将膏料粘合在一起，使得膏料更易于处理并且可更容易在所需烧结接头的位置精确定位。此外，环氧树脂的使用可导致在烧结之前形成更牢固的接头，这意味着在烧结之前不需要将待接合的工件保持在一起。当封端剂包含胺官能团时，环氧树脂的使用是特别有利的。在这种情况下，胺用作形成交联结构的硬化剂。这可以在烧结之前产生特别牢固的接头。
溶剂优选包含单萜醇和/或二醇和/或二醇醚，优选萜品醇和/或二甘醇单正丁基醚。单萜醇和/或二醇醚可特别有效地将金属颗粒分散在膏料中，导致金属颗粒在有机组分的基质中均匀分布，具有减少的簇聚集和/或附聚。单萜醇和/或二醇醚的使用可以用于提高烧结膏料的流动性和印刷能力。
可以加入流变改性剂以控制膏料的粘度。合适的流变改性剂的例子包括但不限于短链或长链(C＝2～30)羧酸或二羧酸或羟基羧酸，例如月桂酸、硬脂酸、新癸酸、硬脂酸、油酸、草酸、丙二酸、琥珀酸、己二酸、马来酸、柠檬酸、乳酸，或短链或长链(C＝2～30)胺，例如丁胺、己胺、辛胺、十二烷基胺、十六烷基胺、Thixcin R和Crayvallac Super，或它们的两种或更多种的组合。
在烧结期间，有机银化合物会分解成金属银，这会增加烧结接头的导热性。此外，有机银化合物的存在增加了膏料对接合界面的润湿性。有机银化合物可包含一种或多种短链或长链羧酸(C＝1～30)，例如硬脂酸银、棕榈酸银、油酸银、月桂酸银、新癸酸银、癸酸银、辛酸银、己酸银、乳酸银、草酸银、柠檬酸银、乙酸银和琥珀酸银。在一些实施方案中，可以省略有机银化合物。
可以加入活化剂以除去可能存在于被印刷的表面上的任何金属氧化物和/或除去可能存在于烧结粉末中的任何氧化物。芳基或烷基羧酸可以用作活化剂，例如己二酸、琥珀酸和戊二酸中的一种或多种。
可以将表面活性剂加入到烧结膏中以帮助将烧结粉末分散在烧结膏中。合适的表面活性剂的例子包括但不限于Disperbyk 163、IGEPAL CA-630、月桂基葡糖苷和TritonX100。
烧结膏优选进一步包含过氧化物。合适的过氧化物的例子包括但不限于过氧化氢或有机过氧化物，例如叔丁基氢过氧化物和叔丁基过氧-2-乙基己酸酯。过氧化物将氧引入到膏料中，这可有助于在管芯连接方法中在管芯区域之下膏料的烧结。氧气还可以使得金属颗粒在惰性气氛(例如氮气气氛)下烧结。烧结膏料优选包含至多3重量％的过氧化氢或有机过氧化物，优选0.5～2重量％的过氧化氢或有机过氧化物，更优选0.7～1.8重量％的过氧化氢或有机过氧化物。优选液体过氧化物以控制流变性和银的沉降。
烧结膏优选包含：
1～15重量％的粘合剂；和/或
1～30重量％的溶剂；和/或
至多5重量％的流变改性剂；和/或
至多10重量％的有机银化合物；和/或
至多2重量％的活化剂；和/或
至多6重量％的表面活性剂；和/或
至多2重量％的过氧化氢或有机过氧化物。
在这些范围内的粘合剂和/或溶剂含量可有助于提供具有特别理想的流动性和印刷能力的烧结膏。优选地，烧结膏包含2～8重量％的粘合剂。在一个实施方案中，烧结膏包含约4.5重量％的粘合剂。优选地，烧结膏包含5～30重量％的溶剂。在一个实施方案中，烧结膏包含约26重量％的溶剂。烧结膏可包含0～5重量％的流变改性剂和/或0～2重量％的活化剂和/或0～6重量％的表面活性剂和/或0～2个过氧化氢或有机过氧化物。烧结膏可包含62～90重量％的烧结粉末。烧结粉末可形成烧结膏的余量。
另一方面，本发明提供一种烧结膏，其包含：
如本文所述的金属粉末；
有机银化合物；
溶剂；和
任选的活化剂和/或流变改性剂和/或表面活性剂和/或过氧化氢或有机过氧化物。
在烧结期间，有机银化合物会分解成金属银，这会增加烧结接头的导热性。此外，有机银化合物的存在增加了膏料对接合界面的润湿性。有机银化合物可包含一种或多种短链或长链羧酸(C＝1～30)，例如硬脂酸银、棕榈酸银、油酸银、月桂酸银、新癸酸银、癸酸银、辛酸银、己酸银、乳酸银、草酸银、柠檬酸银、乙酸银和琥珀酸银。在一些实施方案中，可以省略有机银化合物。
烧结膏优选进一步包含脂肪酸和/或润湿剂，优选一种或多种短链或长链(C＝2～30)羧酸或二羧酸或羟基羧酸，更优选月桂酸、硬脂酸、新癸酸、硬脂酸、油酸、草酸、丙二酸、琥珀酸、己二酸、马来酸、柠檬酸或乳酸；或短链或长链(C＝2～30)胺，更优选丁胺、己胺、辛胺、十二烷基胺或十六烷基胺；或表面活性剂，更优选triton X100、IGEPAL CA-630或月桂基葡糖苷。脂肪酸的存在有助于将膏料粘合在一起。换句话说，脂肪酸的存在避免需要单独的粘合剂，例如以上所讨论的环氧基树脂粘合剂。因此，膏料中有机物的总量较少，导致更强的最终接头。
烧结膏优选进一步包含过氧化物。合适的过氧化物的例子包括但不限于过氧化氢或有机过氧化物，例如叔丁基氢过氧化物和叔丁基过氧-2-乙基己酸酯。过氧化物将氧引入到膏料中，这可有助于在管芯连接方法中在管芯区域之下膏料的烧结。氧气还可以使得金属颗粒在惰性气氛(例如氮气气氛)下烧结。烧结膏料优选包含至多3重量％的过氧化氢或有机过氧化物，优选0.5～2重量％的过氧化氢或有机过氧化物，更优选0.7～1.8重量％的过氧化氢或有机过氧化物。优选液体过氧化物以控制流变性和银的沉降。
烧结膏可包含成膜剂，例如聚酰胺、聚异丁烯、聚酰胺蜡流变改性剂和蓖麻油基触变剂。
优选地，烧结膏基本上不含树脂，更优选完全不含树脂。树脂的存在会降低银的导热性和导电性。溶剂优选包含单萜醇和/或二醇和/或二醇醚，更优选萜品醇和/或二甘醇单正丁基醚。
烧结膏优选包含：
1～30重量％的溶剂；和/或
至多50重量％的有机银化合物，优选0.1～25重量％，更优选0.1～10重量％，甚至更优选0.1～9重量％；和/或
至多5重量％的流变改性剂；和/或
至多2重量％的活化剂；和/或
至多6重量％的表面活性剂；和/或
至多2重量％的过氧化氢或有机过氧化物。
烧结膏可包含0～5重量％的流变改性剂和/或0～2重量％的活化剂和/或0～6重量％的表面活性剂和/或0～2个过氧化氢或有机过氧化物。烧结粉末可形成烧结膏的余量。
另一方面，本发明提供了包含本文所述的金属粉末和粘合剂的烧结膜。该膜可以在晶圆级、管芯级、封装/衬底级和/或模块级应用。这样的膜可以例如通过将本文所述的烧结膏印刷到聚酯片材上，加热该膏料以至少部分地除去溶剂并形成膜，然后从聚酯片材上除去膜而获得。如本文所述的膜是特别有利的，因为其可以通过在稍微升高的温度下简单地将管芯压到膜上而转移到管芯上。转印的膜是一种替代施用方法，在某些情况下有利地提供。该膜可以形成在聚合物、玻璃、金属或陶瓷衬底上或直接形成在晶圆上。该膜可以形成在包含聚酯的聚合物衬底上。该膜可以形成在聚合物衬底上，其中该聚合物衬底包含防粘涂层。所述膜可以通过材料的印刷或浇铸施加所述膏料组合物来制备。该膜可以通过在连续层中印刷来产生。或者，可以通过印刷来形成该膜以形成离散形状的阵列。
另一方面，本发明提供一种管芯连接方法，包括：
(i)将本文所述的烧结膜放置在管芯和待接合的衬底之间；以及
(ii)烧结该烧结膜，
其中该烧结在不施加压力的情况下进行。
这种“低压”或“无压”烧结是特别有利的，因为其可使工艺的自动化更简单。此外，可以减少对工件的损坏。与使用加压烧结的方法相比，更多的优点包括：更短的管芯放置所需的时间(高UPH)，对于放置的低压要求(对于处理薄晶圆非常有利)，与商业管芯接合器的兼容性和在外部加热设备中的烧结(间歇工艺以改善UPH)。
烧结优选在150～400℃的温度下进行最多120分钟。这种条件可以导致烧结膜的特别有效的烧结，同时避免对工件的损坏。
步骤(i)优选包括：
(a)将该烧结膜施加到管芯上以形成具有管芯侧和烧结膜侧的组件；以及
(b)使该组件的膜侧与衬底接触。
这样的步骤可以使过程的自动化更简单，并且可以通过例如使用印模来执行。
步骤(a)优选在15～400℃的温度和0.1～5MPa的压力下进行0.1～60秒。这种条件可导致烧结膜的特别有效的应用，同时避免对管芯的损坏。
步骤(b)优选在15～400℃的温度和0.1～40MPa的压力下进行0.1～60分钟。这种条件可导致管芯对衬底特别有效的接触，同时避免对管芯或衬底的损坏。
另一方面，本发明提供一种管芯连接方法，包括：
(i)将本文所述的烧结膜放置在管芯和待接合的衬底之间；以及
(ii)烧结该烧结膜，
其中，该烧结在施加0.1～40MPa的压力的同时进行。
另一方面，本发明提供一种晶圆接合的方法，包括：
(i)将本文所述的烧结膜放置在待接合的两个或更多个晶圆之间；以及
(ii)烧结该烧结膜，
其中该烧结在不施加压力的情况下进行。
另一方面，本发明提供了一种将烧结膜转移到部件的方法，包括：
将本文所述的烧结膜施加到衬底上，以形成具有烧结膜侧和衬底侧的组件；
使该组件的烧结膜侧与部件接触；
将该组件加热至50～200℃的温度；
向所述组件施加1～5MPa的压力0.1秒～至60分钟；以及
从该烧结膜分离该衬底。
衬底可以是聚合物。烧结膜可以具有与部件基本相同的尺寸。该部件可以是LED。
另一方面，本发明提供了一种用于管芯连接的连接方法，包括：将本文所述的烧结膜施加到衬底；将管芯放置在该膜上以形成组件；向该组件施加小于5MPa的压力；以及在100～400℃的温度下烧结该组件0.1秒～60分钟，施加小于40MPa的压力。可以使用各种提供适当程度的热以引发和完成烧结的方法和设备，在175～400℃的温度下以无压方式进一步烧结同一组件。
另一方面，本发明提供了一种用于管芯连接的连接方法，包括：在晶圆的背面上施加本文所述的烧结膜；切割该晶圆以形成多个管芯；将至少一个管芯放置在衬底上以形成组件；向该组件施加大于1MPa的压力；以及在100～400℃的温度下烧结该组件0.1秒～60分钟，施加小于40MPa的压力。可以使用各种提供适当程度的热以引发和完成烧结的方法和设备，在175～400℃的温度下以无压方式进一步烧结同一组件。
另一方面，本发明提供了一种用于晶圆接合的方法，包括：在晶圆的背面上施加本文所述的烧结膜；在可烧结的含Ag膜的晶圆上放置一个或多个相同或不同类型的晶圆以形成组件；向该组件施加大于0.1MPa的压力；以及在100～400℃的温度下烧结该组件0.25秒～120分钟。可以使用各种提供适当程度的热以引发和完成烧结的方法和设备，在175～400℃的温度下以无压方式进一步烧结同一组件。
另一方面，本发明提供了一种用于晶圆接合的方法，包括：在晶圆的背面上施加烧结膜；在含有该烧结膜的晶圆上放置一个或多个相同或不同类型的晶圆以形成组件；向该组件施加小于40MPa的压力；并在100～400℃的温度下烧结该组件0.25秒～120分钟。可以使用各种提供适当程度的热以引发和完成烧结的方法和设备，在175～400℃的温度下以无压方式进一步烧结同一组件。
另一方面，本发明提供了如本文所述的金属粉末或如本文所述的烧结膏或膜在选自以下的方法中的用途：管芯连接(例如，晶片到板，晶片到衬底，晶片到散热片，晶片到固定件)，晶圆对晶圆连接(例如，晶片到散热片)，反射层印刷，气密和接近气密密封(例如用于封装和周边密封)，生产互连线(例如电路，焊盘)，半导体器件和衬底中的通路填充，以及覆晶技术和晶圆凸块。
另一方面，本发明提供一种制造烧结接头的方法，包括以下步骤：
在待接合的两个或更多个工件的附近提供如本文所述的金属粉末或如本文所述的烧结膏或膜；以及
加热该金属粉末或烧结膏或膜以至少部分地烧结该金属。
有利的是，加热步骤可在大气压下进行。金属粉末或烧结膏或膜可以在低压下(通常在1～5MPa下在约175～250℃的温度下0.1～60秒)放置在工件附近。
加热步骤优选在至少140℃，更优选150～350℃，甚至更优选160～300℃的温度下进行。低于140℃的温度可能不会导致烧结粉末中颗粒的充分烧结和/或可能不会导致通过蒸发和/或烧尽而充分地除去有机物。高于350℃的温度可能会导致工件损坏。
另一方面，本发明提供一种制造烧结膏的方法，包括：
根据本文所述的方法制备金属粉末；以及
将该金属粉末与粘合剂、溶剂和任选的流变改性剂和/或有机银化合物和/或活化剂和/或过氧化物结合。
如将理解的，本文公开的方法、粉末、膏料和膜相对于现有技术具有许多益处。特别地，当用膏料印刷时，没有坍落现象，没有桥接，印刷沉积物中没有气泡，没有渗出和孔隙堵塞。此外，可以提供80～90μm的膏料高度，具有平坦的沉积物，没有卷边且没有起伏。因此，包括粘合剂(例如树脂)的膏料的好处包括：
无压烧结
标准SMT线的加工能力
平坦和均匀的表面拓扑
管芯剪切强度平均值>15MPa
无界面失效模式
室温稳定性＝最少1个月
热循环：可接受的接头强度高达1000循环(-40℃至+125℃，10分钟停留)。
针和喷射可分配
成膜因素
除了上述益处之外，含有有机银化合物的膏料还具有以下列出的一些其它优点：
高管芯剪切强度(15～45MPa)
高导热性(>100W/mK)
引脚可转换
良好的高热性能
附图说明
现在将参考以下非限制性附图描述本发明，其中：
图1显示Ag1～3型Ag颗粒的粒度分布(PSD)图。
图2显示Ag1～3型Ag颗粒的扫描电子显微照片(SEM)。
图3显示Ag1～3型Ag颗粒的热重分析(TGA)图。
图4显示Ag1～3型Ag颗粒的差示扫描量热(DSC)图。
图5显示Cu1～5型Cu颗粒的粒度分布(PSD)图。
图6显示Cu1～5型Cu颗粒的扫描电子显微照片(SEM)。
图7显示涂Ag的AgCu1～5型Cu颗粒的粒度分布(PSD)图。
图8显示涂Ag的AgCu1～5型银颗粒的扫描电子显微照片(SEM)。
具体实施方式
现在将参考以下非限制性实施例描述本发明。
实施例1-Ag微米颗粒类型-1
在化学过程中，通过搅拌将420g硝酸银溶解在2100g去离子水中。向其中加入420gDMF并连续搅拌。向该溶液中同时加入两种单独的溶液，(1)325g三乙胺与460g甲醛的混合物，和(2)30g氢氧化钠在200g去离子水中的溶液。然后立即加入新鲜制备的油酸钠溶液(将6.3g油酸加入到1.3g氢氧化钠在200g水中的溶液中)。将混合物搅拌1小时，然后过滤粉末，用水和丙酮洗涤，直至滤液的pH为中性。然后将粉末在烘箱中在70℃下干燥8小时。
随后是机械过程，其中将200g干燥的粉末在250g甲苯和4g油酸的溶液中搅拌30分钟，然后使用立式搅拌球磨机，使用尺寸为0.1mm的氧化锆珠粒机械处理4.5小时。然后将其用丙酮洗涤以将珠粒与粉末分离并使其沉降。通过倾析溶剂收集粉末。将其用丙酮洗涤以除去额外的有机物。然后将粉末在烘箱中在70℃下干燥8小时。
实施例2和3-Ag微米颗粒类型-2和3
在化学过程中，通过搅拌将420g硝酸银溶解在1500g去离子水中。向其中加入89g氢氧化钠在400g去离子水中的溶液，得到棕色非均质溶液。向反应混合物中加入126g水合肼在1890g去离子水中的溶液，然后加入新鲜制备的油酸钠溶液(将6.3g油酸加入到1.3g氢氧化钠在210g水中的溶液中)。将混合物搅拌1小时，之后过滤粉末，用水和丙酮洗涤，直到滤液的pH为中性。然后将粉末在烘箱中在70℃下干燥8小时。
随后是机械过程，其中将200g干燥的粉末在200g甲苯和4g油酸的溶液中搅拌30分钟，然后使用立式搅拌球磨机，使用尺寸为0.1mm的氧化锆珠粒机械处理(a)4.5小时，以产生Ag-微米颗粒类型-2或(b)9小时，以产生Ag-微米颗粒类型-3。然后将其用丙酮洗涤以将珠粒与粉末分离并使其沉降。通过倾析溶剂收集粉末。将其用丙酮洗涤以除去额外的有机物。然后将粉末在烘箱中在70℃下干燥8小时。
实施例4-多面铜微米颗粒类型Cu 2的制备
通过搅拌30分钟，将1140g硝酸铜(II)三水合物溶解在1550g含有6.9g表面活性剂(DAXAD)的去离子水中。将反应混合物保持在具有电子温度计的热板上。将1380mL 30％的氨溶液加入到上述溶液中直至pH变为8。将溶液搅拌10分钟。温度设定为70℃。达到所需温度后，以每分钟30mL的速率加入1970mL 60％的水合肼，并连续搅拌30分钟。为了减少泡腾，每隔一段时间加入最少量的乙醇。温度设定在85℃。达到温度后，将溶液搅拌2.5小时。使粉末沉降并通过倾析上清液收集粉末。将其用水和丙酮洗涤并在50℃的形成气体(90～95％的氮气:5～10％的氢气)环境中烘干8小时。
实施例5～7-薄片状铜微米颗粒类型Cu 3～5的制备
将500g细碎的铜粉(Cu 1)加入到300g蒸馏水、25g PEG 400、2.25g三亚乙基四胺的溶液中。将其充分混合以获得均匀的混合物，并完全转移到具有2.2Kg尺寸为1.6mm的氧化锆珠粒的立式搅拌球磨机中。继续研磨(a)45分钟，以获得Cu 3，(b)1小时，以获得Cu 4，(c)2小时，以获得Cu 5。在机械加工之后，将混合物与珠粒一起取出到烧杯中，用水将铜薄片与珠粒分离。用水和丙酮混合物洗涤，直到蓝色上清液消失，然后用丙酮洗涤。在50℃下在形成气体(90～95％的氮气:5～10％的氢气)环境中干燥铜薄片，以避免其氧化。
实施例8-球形AgCu：AgCu 1型
Ag涂覆方法：将1Kg细碎的商业铜粉(Cu 1)加入到2Kg去离子水中。向其中加入50gPEG-400，将混合物充分搅拌10分钟，得到均匀的形式。在不断搅拌下将上述浆液加入到3L三亚乙基四胺中。将该混合物搅拌1.5小时。将10Kg冰冷的水加入到反应器中。然后将其再搅拌15分钟。将220g硝酸银和660g柠檬酸溶解在5Kg蒸馏水中，并在不断搅拌下缓慢加入到上述反应混合物中(在约20分钟内)。完全加入后，将反应混合物再搅拌1小时。反应完成后，使混合物沉降，将上清液蓝色溶液倾析并沉淀，用水洗涤AgCu直至上清液完全无色，然后用丙酮洗涤。将粉末在50～60℃的烘箱中干燥。
有机涂层工艺：涂层溶液由2600g甲苯中的140g异硬脂酸组成。将干燥的AgCu粉末加入到该溶液中并搅拌1小时。使混合物沉降；倒出上清液海绿色溶液。用丙酮洗涤AgCu粉末，直到获得无色溶液。将粉末在50～60℃的烘箱中干燥。
实施例9-多面AgCu：AgCu 2型
Ag涂覆工艺：将100g多面铜粉(Cu 2)放入到350g水中并充分搅拌以进行适当分散。向其中加入350g水、22.75g硫酸铵和20mL氢氧化铵的混合物，并搅拌15分钟。倾析上清液，立即向其中加入5g PEG、350g水和350g三乙基四胺的混合物，并搅拌1.5小时。向其中加入1Kg水，然后滴加26.4g AgNO3和22g柠檬酸在250g水中的溶液，并搅拌1小时。用丙酮洗涤粉末，直到获得无色溶液。将粉末在50～60℃的烘箱中干燥。
有机涂层方法：将粉末放入500mL烧杯中，向其中加入300g5％的异硬脂酸溶液(285g甲苯和15g异硬脂酸)并搅拌1小时。将涂覆的粉末用丙酮洗涤并在50～60℃的烘箱中干燥。
实施例10～12-薄片状AgCu：AgCu类型3～5
Ag和有机涂层工艺：将薄片状铜颗粒Cu 3～5用于制备薄片状AgCu颗粒。Ag涂层和有机涂层工艺与球形AgCu 1所述相同。
使用SEM、PSD、元素分析、BET、振实密度和热分析(TGA和DSC)表征实施例1～12的银、铜和涂银的铜微米颗粒，并总结在表1(Ag微米颗粒)、表2(铜微米颗粒)和表3(涂Ag的铜微米颗粒)中。
表1：银微米颗粒Ag类型1～3的表征数据。
表2：铜微米颗粒Cu类型1～5的表征数据。
表3：涂银的铜微米颗粒AuCu类型1～5的表征数据。
本发明的金属粉末、烧结膜和烧结膏的其他应用如下：
1.用于垂直LED设计的晶圆对晶圆接合层、薄膜覆晶设计和红色LED设计，基于可印刷的膏料和薄膜。非常需要低温下(在250℃下并且也在200℃下)的晶圆对晶圆接合，其中接合层在接合后表现出非常高的温度性质。在LED晶圆接合的情况下，这可以例如在薄膜覆晶或垂直薄膜或截顶倒金字塔LED的情况下实现，其中CTE失配，因此应变和缺陷产生可以最小化，同时允许各种先进材料进行高温后处理，用于增强装置的光输出和电效率。此外，接合层的高温和高的热导率和电导率允许优异的热转移、器件的高温操作以及优良的电流扩展等优点。这种晶圆接合可以通过在晶圆的背面上层压所述材料的膜，然后在标准晶圆接合器或压机中进行温度和压力处理来实现。进行处理的另一种方法包括在晶圆背面上印刷保形的膏料层，随后在温度和压力条件下在标准晶圆接合器或压机中干燥和接合。这种晶圆接合的其他应用包括功率半导体晶圆、硅通孔(TSV)应用、层叠管芯应用、MEMS、集中光伏和其他应用。低温烧结使得能够组装高CTE不匹配堆叠以及温度敏感材料堆叠、热电材料和压电材料。
2.将半导体管芯(覆晶或引线接合)连接到各种衬底上，例如DBC(直接结合铜)、DPC(直接板铜)、MCPCB(金属芯PCB)、FR4、铜引线框、柔性PCB和衬底、铜和铝散热片、固定件等。应用包括由各种化合物半导体材料制成的LED管芯(例如横向、垂直薄膜或覆晶变种的发光二极管)、由硅制成的功率管芯、集中光伏化合物半导体电池(例如多结电池)、用于动力模块的碳化硅和氮化镓，以及分立器件、所有类型的MEMS(微机电传感器)器件、半导体和堆叠管芯以及诸如热电材料和压电材料的其他应用。
(a)这种半导体或其他管芯元件的连接可以通过印刷到衬底上，然后通过管芯接合器或拾取和放置机器放置管芯，以及在回流炉带或箱式炉中烧结来完成。这种半导体和管芯元件的连接还可以通过分配膏料，随后是如上所述的管芯放置和烧结，或者在由所述材料制成的膜的管芯背面上进行膜转移和层压，然后是管芯放置并粘合到基底上，然后烧结来完成。覆晶管芯可以通过在衬底上印刷凸块、放置管芯、然后烧结来组装。低温烧结使得能够组装高CTE不匹配堆叠以及温度敏感材料堆叠。
3.各种类型的半导体封装(例如底部终端组件，例如LGA、QFP、QFP等)连接到各种衬底上，例如DBC(直接结合铜)、DPC(直接板铜)、MCPCB(金属芯PCB)、FR4、柔性PCB和衬底、铜和铝散热片、固定件等。应用包括各种类型的LED封装(例如，陶瓷底座LED、具有引线框架构造的SMD LED等)、功率模块和分立器件、所有类型的MEMS(微机电传感器)封装、半导体和堆叠管芯封装等应用。
(a)这种半导体或其他封装的连接可以通过在衬底上印刷，随后通过具有Z高度调节和/或压力能力的标准拾取和放置机器进行封装放置，并在回流炉带式烘箱或箱式炉中烧结来完成。低温烧结使得能够组装高CTE不匹配堆叠以及温度敏感材料堆叠。
4.单独地以及与覆晶互连件一起生产互连线(电路、焊盘等)。例如，互连线的应用包括LED板和灯具，其中互连线可以通过各种印刷(例如模板印刷)或分配或喷射技术来施加。在LED应用的情况下，这种互连可以用作电导体和热导体以将电子携带到器件和从器件携带电子，以及将热量从器件带走。此外，这种互连线可以以与用于连接覆晶或引线接合器件的互连件相同的步骤直接施加。这种互连件的另一个例子是太阳能电池(基于硅或基于薄膜)，其中网格图案的互连件可以用于收集所产生的电子，并且还将一个电池连接到另一个。
5.用于LED和光学应用的反射层印刷。所述材料可用于将反射层印刷到例如DBC(直接结合铜)、DPC(直接板铜)、MCPCB(金属芯PCB)、FR4、铜引线框、柔性PCB和衬底、铜和铝散热片、固定件等的衬底上，以便提供LED输出增强并因此提高LED和其他光学系统的发光效率。这种反射层可以通过所述材料的模板或丝网印刷、喷射或分配或膜层压形成。
6.用于LED、MEMS、OLED和PV应用的封装、周边密封等的密封和接近气密密封以及一般半导体封装。非常需要对LED、OLED、MEMS和薄膜PV封装进行气密密封，以保护器件免受湿气侵入。所述材料可以在适当施加和烧结时表现出密封或接近气密的密封行为。所述材料可以在用于上述器件的制造工艺的各个阶段中应用：晶圆接合的晶圆级，或者通过膜层压和接合的封装工艺，或者膏料喷射/分配之后是盖或玻璃或层压盖片连接和烧结。低温烧结能够组装高CTE不匹配堆叠以及温度敏感材料堆叠。
7.ACF替代品。所述材料的凸块阵列可以通过模版印刷、凸块转移或高速喷射分配被递送到衬底。这样的阵列可以用作电接点以在没有明确的高度对准的情况下组装器件。

Claims (18)

1.一种用于制造金属粉末的方法，包括：
提供碱性金属盐溶液；
使该碱性金属盐溶液与还原剂接触以从其中沉淀出金属粉末；以及
从溶剂中回收所沉淀的金属粉末。
2.权利要求1的方法，其中该还原剂包含肼、甲醛和硼氢化物中的一种或多种。
3.权利要求1或权利要求2的方法，还包括在使该碱性金属盐溶液与该还原剂接触之后，使该碱性金属盐溶液与封端剂接触。
4.权利要求3的方法，其中该封端剂包含脂肪酸，优选月桂酸、棕榈酸、硬脂酸、异硬脂酸和油酸中的一种或多种。
5.前述任一权利要求的方法，还包括研磨所回收的沉淀的金属粉末。
6.权利要求5的方法，其中使用球磨机进行研磨。
7.权利要求5或权利要求6的方法，其中研磨是在脂肪酸，优选月桂酸、棕榈酸、硬脂酸、异硬脂酸和油酸中的一种或多种的存在下；和/或在聚合物，优选PEG 400的存在下；和/或在多胺，优选三亚乙基四胺的存在下进行。
8.权利要求5至7中任一项的方法，其中研磨进行至少30分钟，优选至少90分钟。
9.前述任一权利要求的方法，其中该金属包含银、铜和它们的一种或多种的合金中的一种或多种。
10.前述任一项权利要求的方法，其中：
该金属包含银；并且
该还原剂包含肼，
该方法还包括：
在使该碱性金属盐溶液与该还原剂接触之后，使该碱性金属盐溶液与油酸封端剂接触；以及
在油酸封端剂的存在下，使用球磨机研磨所回收的沉淀的金属粉末至少30分钟。
11.权利要求1至9中任一项的方法，其中该金属包含铜，并且该方法进一步包括在构成粉末的颗粒上施加银涂层。
12.权利要求11的方法，其中施加银涂层包括：
从铜颗粒上蚀刻氧化物层；以及
使用电镀在铜颗粒上施加银涂层。
13.权利要求11或权利要求12的方法，还包括在涂银颗粒上施加脂肪酸涂层。
14.一种制造铜粉末的方法，包括：
提供铜粉末；以及
在聚合物，优选PEG 400的存在下；和/或在多胺，优选三亚乙基四胺的存在下，使用球磨机研磨该铜粉末。
15.根据前述任一权利要求的方法制造的金属粉末。
16.一种金属粉末，具有：
500nm至10μm的d50；以及
大于2g/cm3的振实密度，
其中该金属粉末包含银、铜和它们的一种或多种的合金中的一种或多种。
17.一种烧结膏，包含：
权利要求15或权利要求16的金属粉末；
粘合剂；
溶剂；和
任选的流变改性剂和/或有机银化合物和/或活化剂和/或表面活性剂和/或润湿剂和/或过氧化氢或有机过氧化物。
18.一种制造烧结膏的方法，包括：
根据权利要求1至14中任一项的方法制备金属粉末；以及
将该金属粉末与粘合剂、溶剂和任选的流变改性剂和/或有机银化合物和/或活化剂和/或过氧化物组合。
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