CN114391169A - 银烧结制备物及其用于连接电子部件的用途 - Google Patents

银烧结制备物及其用于连接电子部件的用途 Download PDF

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CN114391169A
CN114391169A CN202080064364.XA CN202080064364A CN114391169A CN 114391169 A CN114391169 A CN 114391169A CN 202080064364 A CN202080064364 A CN 202080064364A CN 114391169 A CN114391169 A CN 114391169A
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silver
sintering
metal contact
organic polymer
electronic component
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L·M·周
S·苏
S·沙巴兹
W·施米特
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Heraeus Deutschland GmbH and Co KG
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Abstract

本发明公开了一种银烧结制备物，该银烧结制备物包含：(A)30重量％至88重量％的平均粒径(d50)在>1μm至20μm范围内的银薄片颗粒，(B)5重量％至30重量％的至少一种银前体，(C)1重量％至10重量％的有机聚合物体系，以及(D)6重量％至30重量％的有机溶剂，其中该有机聚合物体系(C)在温度<300℃下在化学上基本稳定并且与该有机溶剂(D)一起形成连续相。

Description

银烧结制备物及其用于连接电子部件的用途
本发明涉及一种银烧结制备物以及一种用于连接(接合)电子部件的方法，在该方法中使用所述银烧结制备物。
银烧结技术作为连接(接合)电子部件的方法已成为当前最先进的技术，参见例如WO2011/026623 A1、WO2011/0266243 A1和WO2016/028221 A1、US 2017/0243849 A1和US2018/0056449 A1。
本文所用的术语“电子部件”是指用于电子器件中的有源部件和无源部件；示例包括二极管、LED(发光二极管)、管芯、IGBT(绝缘栅双极型晶体管)、MOSFET(金属氧化物半导体场效应晶体管)、IC(集成电路)、传感器、散热器、电阻器、电容器、感应器、天线、连接元件(例如，芯片)、引线框、PCB(印刷电路板)、柔性电子器件、陶瓷衬底、金属陶瓷衬底例如DCB(直接敷铜衬底)、IMS(绝缘金属衬底)等。
已经公开了可在烧结工艺期间在不施加机械压力的情况下使用基于银纳米颗粒或基于银微粒(通常粒度在1至10μm的范围内)与银纳米颗粒(通常粒度在1至100纳米的范围内)的混合物的烧结浆料来在裸铜表面上形成银烧结接头。此类公开内容的示例包括：H.Miyoshi、K.Endoh、S.Kurita，“施加银纳米颗粒以无压粘结到铜表面上–考虑铅焊料的代用材料(Application of Silver Nano Particles to Pressureless Bonding onto aCopper Surface–Consideration of Substitute Material for Lead Solder)”，2014年CIPS会议；H.Zheng、D.Berry、K.D.T.Ngo、G.Lu，“通过纳米银浆料在受控气氛下的无压烧结来实现铜上的芯片粘结(Chip-Bonding on Copper by Pressureless Sintering ofNanosilver Paste Under Controlled Atmosphere)”，《IEEE电子部件、封装与制造技术汇刊》(IEEE Transactions on Electronic components,Packaging and ManufacturingTechnology)，第4卷，第3期，2014年3月；H.Zheng、J.Calata、K.Nog、S.Luo、G.Lu，“使用纳米银浆料在铜上低压(<5MPa)低温接合大面积芯片(Low-pressure(<5MPa)Low-temperatureJoining of Large-area Chips on Copper Using Nanosilver paste)”，2012年CIPS会议；以及T.Watanabe、N.Nakajima、M.Takesue，“达到200/40℃热循环可靠性的无压烧结银的材料设计和工艺条件(Material Design and Process Conditions of PressurelessSintered Silver for 200/40℃Thermal Cycling Reliability)”，2017年欧洲PCIM。
本发明的一个目标是提供以可靠方式连接电子部件的银烧结方法；通常此类连接经由电子部件的金属接触表面发生。具体地讲，有待发现的银烧结方法应非常适合以高可靠性连接电子部件，其中至少一个电子部件具有非贵金属接触表面如铜表面。本发明的另一个目标是提供不含纳米级银颗粒并且非常适合实施此类烧结方法的银烧结制备物。即使在电子部件的未经预处理的非贵金属接触表面上并且即使在低烧结温度下，在烧结期间施加或不施加机械压力的情况下，也应实现可靠连接的形成。
本发明涉及一种用于连接电子部件的方法，在该方法中(a)提供夹层布置，该夹层布置至少包括(a1)电子部件1、(a2)电子部件2和(a3)位于这些电子部件的金属接触表面之间的银烧结制备物，并且在该方法中(b)烧结该夹层布置，由此银烧结制备物包含：
(A)30重量％至88重量％(按重量计的％)的平均粒径(d50)在>1μm至20μm范围内的银薄片颗粒，
(B)5重量％至30重量％的至少一种银前体，
(C)1重量％至10重量％的有机聚合物体系，以及
(D)6重量％至30重量％的有机溶剂，
其中该有机聚合物体系(C)在温度<300℃下在化学上基本稳定并且与该有机溶剂(D)一起形成连续相。
此外，本发明涉及一种银烧结制备物，该银烧结制备物包含：
(A)30重量％至88重量％的平均粒径(d50)在>1μm至20μm范围内的银薄片颗粒，
(B)5重量％至30重量％的至少一种银前体，
(C)1重量％至10重量％的有机聚合物体系，以及
(D)6重量％至30重量％的有机溶剂，
其中该有机聚合物体系(C)在温度<300℃下在化学上基本稳定并且与该有机溶剂(D)一起形成连续相。
本发明的银烧结制备物包含(A)30重量％至88重量％、优选地40重量％至70重量％、最优选地50重量％至70重量％的平均粒径(d50)在>1μm至20μm范围内的银薄片颗粒。
本文所用的术语“银薄片颗粒”是指纯银(具有至少99.90重量％、优选地至少99.95重量％的纯度的银)或具有55重量％至<95重量％范围内的银含量的银合金的薄片(小片)，或是指在除银之外的金属芯例如铜芯或铜银合金的芯上具有银涂层的薄片。薄片是表现出大于10:1的纵横比的扁平颗粒，其与球体(纵横比为1:1)或细粒(纵横比通常在1和5之间)完全不同。
本文所用的术语“平均粒度”(“均值粒度”)意指通过激光衍射确定的平均粒径(d50)。可利用粒度分析仪(例如得自马尔文仪器公司(Malvern Instruments)的Mastersizer 3000)进行激光衍射测量。
通常，银薄片颗粒(A)包括表面涂层。银薄片颗粒(A)的此类涂层包含至少一种类型的有机化合物。用作涂料化合物的有机化合物防止银薄片颗粒(A)附聚。
此类涂料化合物的优选示例包括游离脂肪酸、脂肪酸盐和脂肪酸酯。游离脂肪酸、脂肪酸盐和脂肪酸酯优选地是非支链的。此外，游离脂肪酸、脂肪酸盐和脂肪酸酯优选地是饱和的。优选的脂肪酸盐包括铵盐、单烷基铵盐、二烷基铵盐、三烷基铵盐、铝盐、铜盐、锂盐、钠盐和钾盐。烷基酯，特别是甲酯、乙酯、丙酯和丁酯，是优选的酯。根据一个优选的实施方案，游离脂肪酸、脂肪酸盐或脂肪酸酯是具有8至24个、更优选地8至18个碳原子的化合物。所述脂肪酸的示例包括羊脂酸(辛酸)、羊蜡酸(癸酸)、月桂酸(十二烷酸)、肉豆蔻酸(十四烷酸)、棕榈酸(十六烷酸)、珠光脂酸(十七烷酸)、硬脂酸(十八烷酸)、花生酸(二十烷酸/二十酸)、山萮酸(二十二烷酸)和木蜡酸(二十四烷酸)。
脂肪酸或脂肪酸盐类型的特别优选的涂料化合物包括十二烷酸、十八烷酸、硬脂酸铝、硬脂酸铜、硬脂酸钠、硬酯酸钾、棕榈酸钠和棕榈酸钾。
优选地，有机化合物，特别是选自游离脂肪酸、脂肪酸盐和脂肪酸酯的化合物相对于整个涂层的分数为至少60重量％、更优选地至少90重量％、特别是至少95重量％、至少99重量％或100重量％。
涂料化合物，优选地选自游离脂肪酸、脂肪酸盐和脂肪酸酯的涂料化合物相对于带涂层的银薄片颗粒(A)的重量的分数为<5重量％，例如0.01重量％至2重量％、优选地0.3重量％至1.5重量％。
涂覆程度(被定义为涂料化合物的质量与银薄片颗粒(A)的表面积的比率)优选地为每平方米(m2)银薄片颗粒(A)的表面积0.00005g至0.03g、更优选地0.0001g至0.02g的涂料化合物。
本发明的银烧结制备物包含5重量％至30重量％的至少一种银前体(B)。
银前体是在低于200℃的温度下分解同时释放单质银的银化合物。因此，银前体在烧结工艺中的使用优选地与银的原位产生相关联。银前体的示例包括碳酸银、乳酸银(I)、甲酸银(II)、柠檬酸银、氧化银(例如AgO或Ag2O)。碳酸银、氧化银(I)和氧化银(II)是优选的银前体。
银前体优选地以颗粒的形式存在。此类银前体颗粒可采取薄片的形状或球形(球状)形状。优选地，银前体颗粒以薄片的形式存在。
本发明的银烧结制备物包含1重量％至10重量％、优选地2重量％至7重量％的有机聚合物体系(C)，其在温度<300℃下在化学上基本稳定并且与有机溶剂(D)一起形成连续相。
有机聚合物体系(C)(呈游离形式或与本发明的银烧结制备物的其他成分共存)在至多<300℃的温度下在化学上基本稳定并且因此也在本发明的方法的所有步骤期间、特别是也在烧结步骤(b)期间普遍的温度范围内。还换句话讲，有机聚合物体系(C)既基本上不分解，也不经历基本的化学变化，如例如所述条件下的非期望的交联反应。
本文所用的术语“可交联、交联”与通过形成共价键实现的“可硬化、硬化”或“可固化、固化”同义。形成共价键的交联反应具体地包括自由基聚合反应、缩合反应和/或加成反应。
可通过银烧结制备物内的有机聚合物体系(C)与已在温度<300℃下或在烧结步骤(b)期间普遍的实际温度范围内烧结的银烧结制备物的样品的有机聚合物体系(C)的定性与定量分析比较来确定有机聚合物体系(C)的化学稳定性。在至多<300℃的温度下在化学上基本稳定的有机聚合物体系(C)在烧结步骤(b)的条件下对其进行处理时将不显示出重量损失或仅显示出例如0重量％至不超过5重量％范围内的小重量损失。可例如通过热重分析以例如每分钟5K的加热速率确定或监测重量损失。
在所述条件下，此类在化学上基本稳定的有机聚合物体系(C)不但将不显示出重量损失或仅显示出小重量损失；而且将不显示出分子量的变化或增加。可例如通过凝胶渗透色谱法(GPC；二乙烯基苯交联的聚苯乙烯作为固定相，四氢呋喃作为液相，聚苯乙烯标准品)来确定或监测分子量变化。
有机聚合物体系(C)由至少一种有机聚合物组成，即除了一种或多种有机聚合物以外没有其他成分，每种有机聚合物在上述意义上都在化学上基本稳定。从而，该至少一种有机聚合物在上述条件下不分解并且不可自交联，即其没有能够在所述条件下进行自交联反应的官能团。例如，该至少一种有机聚合物可具有在所述条件下彼此不反应的相同或不同官能团；从而，可防止自交联。为了避免误解，在所述条件下，一个独立有机聚合物分子内和单独有机聚合物分子之间都没有交联反应，而不论有机聚合物体系(C)是否由一种、两种或更多种有机聚合物组成。
在一个实施方案中，该至少一种不可自交联有机聚合物可包括仅仅由于缺少反应性官能团或甚至由于缺少任何官能团而不可自交联的一种或多种有机聚合物。
在另一个实施方案中，该至少一种不可自交联有机聚合物可包括具有在上述条件下彼此间不反应的官能团的一种或多种有机聚合物。
然而，在又一个实施方案中，该至少一种不可自交联有机聚合物可包括外部可交联类型的一种或多种有机聚合物；此处，有机聚合物包含原则上能够在上述条件下进行交联反应，但仅在与单独(外部)交联剂联合的情况下才能反应的官能团。至少在该实施方案中，本发明的银烧结制备物不含任何此类单独交联剂或任何能够充当单独交联剂的物质。不确定某种物质或材料是否能够这样无意充当单独交联剂的技术人员可对此简单地进行检查。为此，技术人员可将有机聚合物体系(C)与所考虑的物质混合并且将该混合物加热到例如至多<300℃，然后检查是否发生交联反应，这与分子量增加相符。
通常，本发明的银烧结制备物不包含能够在温度<300℃下或在本发明的方法的步骤期间、特别是在其烧结步骤(b)期间普遍存在的温度范围内生成自由基的物质。如果本发明的银烧结制备物或更确切地说其有机聚合物体系(C)包含具有可自由基聚合的基团的一种或多种有机聚合物，则尤其如此。于是本发明的银烧结制备物绝对不含此类物质。此类物质的示例包括可热裂解的自由基引发剂如过氧化物或偶氮化合物。
通常，本发明的银烧结制备物不包含能够在温度<300℃下或在本发明的方法的步骤期间、特别是在其烧结步骤(b)期间普遍存在的温度范围内表现得像或释放阳离子引发剂的物质。如果本发明的银烧结制备物或更确切地说其有机聚合物体系(C)包含具有可阳离子聚合的基团的一种或多种有机聚合物，则尤其如此。于是本发明的银烧结制备物绝对不含此类物质。
有机聚合物体系(C)的该至少一种有机聚合物的示例包括苯氧基醚树脂(双酚A与表氯醇的热塑性共聚物)、酚醛树脂、聚酰亚胺、聚酰胺、聚砜、苯并噁嗪树脂、三聚氰胺甲醛树脂、丙烯腈丁二烯苯乙烯共聚物、(甲基)丙烯酰共聚物、聚酯、聚氨酯、聚硅氧烷以及它们的任何杂化物。苯氧基醚树脂、酚醛树脂、聚酰亚胺和聚砜是优选的示例。
纤维素或纤维素衍生物如醚化和/或酯化的纤维素(纤维素醚、纤维素酯和纤维素醚酯)在上述意义上不是化学上基本稳定的。相反，它们将在步骤(b)的烧结条件下分解。因此，有机聚合物体系(C)不包含纤维素或纤维素衍生物诸如醚化和/或酯化的纤维素(纤维素醚、纤维素酯和纤维素醚酯)。
该至少一种有机聚合物的重均分子量Mw可在例如>1000至100000的范围内，如凝胶渗透色谱法(GPC；二乙烯基苯交联的聚苯乙烯作为固定相，四氢呋喃作为液相，聚苯乙烯标准品)所确定的。
该至少一种有机聚合物可表现出可在例如>60℃至190℃范围内的玻璃化转变温度Tg，如通过DSC以例如每分钟5K的加热速率所确定的。
有机聚合物体系(C)与有机溶剂(D)一起在本发明的银烧结制备物内形成连续相。这意味着有机聚合物体系(C)或其任何有机聚合物成分不以微粒或分散形式存在于本发明的银烧结制备物内。相反，有机聚合物体系(C)与有机溶剂(D)一起形成连续均匀相，例如呈有机物的溶液或有点粘性的组合物的形式。
本发明的银烧结制备物包含6重量％至30重量％、优选地8重量％至25重量％以及最优选地10重量％至25重量％的有机溶剂(D)，即一种有机溶剂或者至少两种有机溶剂的混合物。
该一种或多种有机溶剂是通常用于银烧结制备物的有机溶剂。示例包括醇，例如萜品醇、十三醇；二醇醚，例如三丙二醇单甲醚、二丙二醇单丁醚、二乙二醇单己醚；酯，例如二丙二醇甲醚乙酸酯、己二酸二乙酯、二元酯。
根据上述公开内容，本发明的银烧结制备物可包含总共0重量％至10重量％的与成分(A)至(D)不同的一种或多种另外的成分(E)(除成分(A)至(D)之外的成分)。所述另外的成分可优选地为通常用于银烧结制备物中的成分。示例包括添加剂如分散剂、表面活性剂、消泡剂、粘度控制(流变)剂和烧结剂。
为成分(A)至(E)指定的重量％分数可合计为例如相对于本发明的银烧结制备物(即，在施加该银烧结制备物之前)计100重量％。因此，可通过混合成分(A)至(E)来制备本发明的银烧结制备物。可在该上下文中使用本领域技术人员所知的设备，诸如搅拌器和三辊研磨机。有利的是，可将本发明的银烧结制备物储存在例如2℃至25℃的温度下，即在其储存或运输期间不需要巨大的冷却工作。
本发明的银烧结制备物可用于烧结工艺中。烧结应被理解为意指通过加热来连接两个或更多个电子部件而不使银薄片颗粒(A)达到液相。在本公开的上下文中，烧结工艺中的所述用途可被定义为用于连接电子部件的方法，在该方法中(a)提供夹层布置，该夹层布置至少包括(a1)电子部件1、(a2)电子部件2和(a3)位于电子部件1和2的金属接触表面之间的根据其上文公开的任何实施方案的银烧结制备物，并且在该方法中(b)烧结该夹层布置。
如同常规的电子部件一样，电子部件1和2中的每一者均具有金属接触表面。至于电子部件1和2不由金属组成而言，它们的接触表面被金属化层覆盖。在一个实施方案中，金属接触表面可由非贵金属诸如铜、镍或铝制成。在另一个实施方案中，金属接触表面可由贵金属诸如银制成。还有可能金属接触表面之一由非贵金属制成，而另一个金属接触表面由贵金属制成。
连接至少两个电子部件应被理解为意指将第一电子部件附接在第二电子部件上。在该上下文中，“在...上”仅仅意指第一电子部件的金属接触表面连接到第二电子部件的金属接触表面，而不论这两种电子部件或包括该至少两种电子部件的夹层布置的相对布置如何。
待连接的电子部件1和2可为相同或不同的电子部件。本发明不仅有利于连接电子部件的贵金属接触表面，而且特别有利于以在室温和高温下产生可靠连接的方式将电子部件的非贵金属接触表面连接到贵金属接触表面或甚至连接两个非贵金属接触表面。例如，可形成铝-镍连接、铝-铜连接、铝-银连接、铝-铝连接、铜-银连接、铜-镍连接、铜-铜连接、银-镍连接或银-银连接。术语“铝、铜、镍和银金属接触表面”包括由所述金属的合金制成的金属接触表面。正如银或其他贵金属接触表面的情况一样，即使在非贵金属接触表面如铜、镍或铝表面的情况下，也不需要在进行烧结步骤(b)之前对其进行预处理。
因此，如果两个电子部件(即，电子部件1和电子部件2)要彼此连接，则在进行步骤(b)的烧结工艺之前本发明的银烧结制备物位于电子部件1和电子部件2的金属接触表面之间。另一方面，可以想到使超过两个电子部件彼此连接。例如，三个电子部件(即，电子部件1、电子部件2和电子部件3)可彼此以适当方式连接，使得电子部件2位于电子部件1和电子部件3之间。在这种情况下，本发明的银烧结制备物既位于电子部件1和电子部件2之间，又位于电子部件2和电子部件3之间，或更确切地说，位于它们的金属接触表面之间。
优选地，首先，为电子部件之一的金属接触表面提供本发明的银烧结制备物。然后，将另一电子部件通过其金属接触表面放置在已向第一电子部件的金属接触表面施加的银烧结制备物上。
可通过常规方法将本发明的银烧结制备物施加到电子部件的金属接触表面上。示例包括分配、丝网印刷、镂空版印刷、针板转移和浸涂。优选地，待连接的电子部件之间的银烧结制备物的湿层的厚度在20μm至100μm的范围内。在该上下文中，湿层的厚度应被理解为意指干燥(如果有的话)之前和烧结步骤(b)之前的层厚度。优选的湿层厚度取决于被选择用于施加银烧结制备物的方法。如果例如通过丝网印刷或分配来施加银烧结制备物，则湿层厚度可优选地在20μm至50μm的范围内。如果通过镂空版印刷来施加银烧结制备物，则优选的湿层厚度可在20μm至100μm的范围内。
作为一个选项，在烧结步骤(b)之前引入干燥步骤，即随后从施加的银烧结制备物去除有机溶剂。可在形成夹层布置之前，即在将烧结制备物施加到电子部件1的金属接触表面之后并且在与电子部件2的金属接触表面连接之前，或在组装夹层布置之后，进行干燥步骤。根据一个优选的实施方案，干燥后的银烧结制备物中的有机溶剂的分数为例如相对于本发明的银烧结制备物中(即准备施加的银烧结制备物中)的有机溶剂的初始分数计0重量％至5重量％。换句话讲，根据所述优选的实施方案，在干燥期间去除初始存在于本发明的银烧结制备物中的例如95重量％至100重量％的有机溶剂。干燥温度可在例如100℃至150℃的范围内。通常的干燥时间在例如5分钟至45分钟的范围内。
最后对该至少两个电子部件1和2及位于它们的金属接触表面之间的银烧结制备物的夹层布置进行步骤(b)中的烧结工艺。
不论待连接的电子部件的金属接触表面类型如何，都可在<300℃例如在200℃至280℃或200℃至250℃的范围内的温度下并在施加或不施加机械压力的情况下和/或在预处理或不预处理贵金属或非贵金属接触表面的情况下进行实际烧结。
烧结时间例如在2分钟至60分钟的范围内，例如在加压烧结中在2分钟至5分钟的范围内以及例如在无机械压力的烧结中在30分钟至60分钟的范围内。
加压烧结中的机械压力优选地小于30MPa并且更优选地小于5MPa。例如，机械压力在1MPa至30MPa的范围内，并且更优选地，其在1MPa至5MPa的范围内。
在不施加机械压力的情况下进行烧结步骤(b)允许使用压敏(例如易碎)电子部件或具有机械敏感微结构的电子部件。具有机械敏感微结构的电子部件在暴露于不容许的机械压力时会遭遇电气故障。
烧结步骤(b)可在不受限于任何具体限制的气氛中进行。不必使用还原性气氛如氢气/氮气或甲酸/氮气混合物或真空，尽管这是可能的。因此，一方面，只要电子部件的非贵金属接触表面没有涉及到烧结，烧结就可在包含氧气的气氛中进行。另一方面，烧结在惰性或无氧气氛例如氮气氛或氩气氛中进行也是可行的。在电子部件的非贵金属接触表面涉及到步骤(b)的烧结的情况下，要求在惰性或无氧气氛中工作；然而，即使在此类情况下也不要求在还原性气氛中工作。在本发明的范围内，无氧气氛应被理解为意指氧含量不超过100ppm、优选地不超过80ppm以及甚至更优选地不超过50ppm的气氛。
烧结步骤(b)可在用于烧结的常规合适装置中进行，可在该装置中设定上述工艺参数。
为了在这些电子部件之间获得满足或甚至超过要求(稳定连接)的连接强度，本发明的方法既不需要预处理待连接的电子部件的金属接触表面，也不需要特别高的烧结温度，还不需要在烧结期间施加机械压力；不论所涉及的金属接触表面的金属类型如何，这点都成立。如已经在上文公开的，在涉及到非贵金属接触表面的情况下，需要满足在惰性或无氧气氛中或在真空中执行烧结步骤(b)的要求；然而，不要求在还原性气氛中工作。
因此，在一个实施方案中，甚至有可能本发明的方法是用于连接电子部件的方法，在该方法中(a)提供夹层布置，该夹层布置至少包括(a1)电子部件1、(a2)电子部件2和(a3)位于这些电子部件的未经预处理的金属接触表面之间的根据其上文公开的任何实施方案的银烧结制备物，并且在该方法中(b)烧结该夹层布置，
其中这些电子部件的未经预处理的金属接触表面中的至少一者的金属是非贵金属，并且
其中烧结步骤(b)在不施加机械压力的情况下在200℃至300℃范围内的烧结温度下在惰性气氛中进行。
实施例：
1.银烧结制备物的制备：
通过根据表1以类似的流变行为混合单独成分来制备银烧结制备物2至5(根据本发明)和参考浆料1。所有给出的量都以重量％为单位。
表1
参考浆料1 浆料2 浆料3 浆料4 浆料5
银颗粒<sup>1</sup>) 66.80 66.80 66.80 62.00 58.00
碳酸银 19.95 19.95 19.95 18.00 17.00
萜品醇 3.00 3.31
乙基纤维素 0.25
2-乙基-1,3-己二醇 8.00
异十八醇 2.00
邻苯二甲酸二甲酯 5.80 5.00
DBE<sup>2)</sup> 2.48
二乙二醇单乙酸乙酯 4.00 8.00
γ-丁内酯 1.00 6.00 15.00
己二酸二乙酯 4.25
苯氧基醚树脂<sup>3)</sup> 1.66 4.00 4.50
酚醛树脂<sup>4)</sup> 1.50
聚酰亚胺<sup>5)</sup> 5.00
合计 100 100 100 100 100
1)带有0.7重量％月桂酸/硬脂酸(重量比1:3)涂层的平均粒度(d50)为4μm的银薄片
2)得自西格玛奥德里奇公司(Sigma-Aldrich)的二元酯422053
3)重均分子量Mw为52000Da的苯氧基醚树脂(双酚A/表氯醇树脂)
4)得自乔治亚太平洋化学公司(Georgia-Pacific Chemicals LLC)的GP酚醛树脂BKRmolecular-2620
5)得自亨斯迈公司(Huntsman)的MATRIMID 5218 US
2.组合物1至5的施加和无压烧结：
通过分配将相应组合物施加到由富铜的铜/铁合金(96重量％铜、4重量％Fe)制成的引线框的铜表面上以产生30μm厚的湿层。然后，在不预先干燥的情况下使所施加的组合物经由其2×2mm银金属接触表面与硅芯片接触。在包含最多50ppm氧气的氮气氛中根据以下加热分布进行后续无压烧结：将接触点在60分钟的过程中稳步加热到200℃，然后在200℃下保持60分钟。之后，将由此形成的布置在60分钟的过程中稳步冷却到30℃。
烧结后，通过剪切测试来确定粘结强度。在该上下文中，使用剪切凿在室温下以0.3mm/s的速率剪断电子部件。通过测力传感器(德国DAGE公司制造的DAGE 4000plus设备)来测量该力。表2示出了使用组合物1至5获得的结果。
表2
Figure BDA0003544577170000121

Claims (15)

1.一种银烧结制备物，所述银烧结制备物包含：
(A)30重量％至88重量％的平均粒径(d50)在>1μm至20μm范围内的银薄片颗粒，
(B)5重量％至30重量％的至少一种银前体，
(C)1重量％至10重量％的有机聚合物体系，以及
(D)6重量％至30重量％的有机溶剂，
其中所述有机聚合物体系(C)在温度<300℃下在化学上基本稳定并且与所述有机溶剂(D)一起形成连续相。
2.根据权利要求1所述的银烧结制备物，其中所述银薄片颗粒(A)包括包含至少一种类型的有机化合物的表面涂层。
3.根据权利要求2所述的银烧结制备物，其中所述至少一种类型的有机化合物选自游离脂肪酸、脂肪酸盐和脂肪酸酯。
4.根据前述权利要求中任一项所述的银烧结制备物，其中所述至少一种银前体选自碳酸银、乳酸银(I)、甲酸银(II)、柠檬酸银、氧化银(I)和氧化银(II)。
5.根据前述权利要求中任一项所述的银烧结制备物，其中所述有机聚合物体系(C)由至少一种有机聚合物组成。
6.根据权利要求5所述的银烧结制备物，其中所述至少一种有机聚合物选自苯氧基醚树脂、酚醛树脂、聚酰亚胺、聚酰胺、聚砜、苯并
Figure FDA0003544577160000011
嗪树脂、三聚氰胺甲醛树脂、丙烯腈丁二烯苯乙烯共聚物、(甲基)丙烯酰共聚物、聚酯、聚氨酯、聚硅氧烷以及它们的任何杂化物。
7.根据权利要求5或6所述的银烧结制备物，其中所述至少一种有机聚合物具有>1000至100000的重均分子量Mw，如通过凝胶渗透色谱法所确定的。
8.根据权利要求5、6或7所述的银烧结制备物，其中所述至少一种有机聚合物表现出>60℃至190℃范围内的玻璃化转变温度Tg，如通过DSC以每分钟5K的加热速率所确定的。
9.根据前述权利要求中任一项所述的银烧结制备物，所述银烧结制备物包含总共0重量％至10重量％的与成分(A)至(D)不同的一种或多种另外的成分(E)。
10.一种用于连接电子部件的方法，在所述方法中(a)提供夹层布置，所述夹层布置至少包括(a1)电子部件1、(a2)电子部件2和(a3)位于所述电子部件的金属接触表面之间的根据前述权利要求中任一项所述的银烧结制备物，并且在所述方法中(b)烧结所述夹层布置。
11.根据权利要求10所述的方法，其中所述电子部件1和电子部件2中的每一者具有金属接触表面。
12.根据权利要求11所述的方法，其中所述金属接触表面由(i)选自铜、镍和铝的非贵金属制成，或者由(ii)贵金属制成，或者(iii)所述金属接触表面之一由选自铜、镍和铝的非贵金属制成并且另一金属接触表面由贵金属制成。
13.根据权利要求12所述的方法，其中在进行所述烧结步骤(b)之前不对非贵金属接触表面进行预处理。
14.根据权利要求10至12中任一项所述的方法，其中在200℃至280℃的温度下并在施加或不施加机械压力的情况下且在预处理或不预处理所述贵金属接触表面或非贵金属接触表面的情况下进行所述烧结。
15.根据权利要求10至14中任一项所述的方法，其中在电子部件的非贵金属接触表面涉及到步骤(b)的所述烧结的情况下，其在惰性或无氧气氛中工作。
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