CN112437706A - 接合用组合物以及导电体的接合结构及其制造方法 - Google Patents
接合用组合物以及导电体的接合结构及其制造方法 Download PDFInfo
- Publication number
- CN112437706A CN112437706A CN201980048168.0A CN201980048168A CN112437706A CN 112437706 A CN112437706 A CN 112437706A CN 201980048168 A CN201980048168 A CN 201980048168A CN 112437706 A CN112437706 A CN 112437706A
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- Prior art keywords
- reducing agent
- coating film
- bonding
- liquid medium
- mass
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Classifications
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- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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Abstract
本发明的接合用组合物包含铜粉、液介质及还原剂,上述还原剂具有至少1个氨基及多个羟基,上述还原剂的沸点比上述液介质的沸点高,上述还原剂的熔点为上述铜粉的烧结温度以下。上述还原剂优选为双(2‑羟基乙基)亚氨基三(羟基甲基)甲烷。接合用组合物优选剪切速度10s‑1及25℃下的粘度为10Pa·s以上且200Pa·s以下。接合用组合物还优选相对于上述铜粉100质量份包含0.1质量份以上且10质量份以下的上述还原剂,并且包含10质量份以上且40质量份以下的上述液介质。
Description
技术领域
本发明涉及为了将两个部位接合而使用的接合用组合物。另外,本发明涉及使用了该接合用组合物的导电体的接合结构的制造方法及通过该方法而制造的导电体的接合结构。
背景技术
伴随着近年来的世界上的节能化的潮流,作为变换器等电力转换、控制装置,在广泛地使用被称为功率器件的半导体器件。功率器件与存储器或微处理器这样的集成电路不同,由于是用于控制高电流的器件,因此驱动时的发热量变得非常大。因此,为了不让半导体元件因该热而受到损伤,对半导体封装要求冷却***等散热对策。
顺便提一下,为了大幅地改善仪器的能量利用效率,提出了各种代替以往的Si而使用了以SiC及GaN为代表的宽带隙半导体(WBG)等新材料的半导体元件。SiC或GaN与Si相比带隙较宽。起因于此,SiC或GaN与Si相比能够提高驱动温度。因此,可以谋求半导体封装的冷却***的简化,进而可以谋求装置整体的小型化。
但是,以往作为接合材料而使用的焊锡耐热性低,无法应用于超过175℃的WBG的驱动。于是,代替使用焊锡而使用了金属粒子的烧结型接合材料的研究一直在进行。例如本申请人之前提出了一种方法,其通过由包含粒径相对大的大径铜粒子、与该大径铜粒子相比粒径相对小的小径铜粒子、胺化合物和具有与该胺化合物的反应性基团的硅烷偶联剂的组合物的烧结体构成的接合部位将两个导电体进行接合(参照专利文献1)。
通过利用由上述的组合物的烧结体构成的接合部位将两个导电体进行接合,起因于由热引起的膨张/收缩所导致的尺寸变化而产生的应力有效地得以缓和。另外,上述接合部位是耐热性及接合强度高、并且低电阻的部位。
不同于上述的技术,在专利文献2中记载了一种技术,其中,将包含金属微粒的接合材料进行压制而制造片材体,在使该片材体夹在两个导电体之间并加压的状态下进行加热、烧成,从而将两个导电体进行接合。在上述的接合材料中包含在25℃下为固体形状的多元醇。
现有技术文献
专利文献
专利文献1:US2017/0140847A1
专利文献2:日本特开2013-39580号公报
发明内容
在使用专利文献1中记载的组合物将两个导电体进行接合的情况下,一般而言,使该组合物夹在两个导电体之间而在不加压的情况下进行烧结。但是,根据该组合物的使用方法或应用该组合物的对象,有时优选使该组合物夹在两个导电体之间并在加压的状态下进行烧结。其理由是由于,通过在烧结时以压力进行协助从而粒子的烧结驱动力提高,烧结被进一步促进,因此与接合对象基材的接合强度更进一步提高。在那样的情况下,若使用该文献中记载的组合物,则虽然可充分获得接合强度,但是由于该组合物在两个导电体之间进行流动,因此根据涂布图案形状有时该组合物从两个导电体间流出。若该组合物从两个导体间流出,则两个导电体间的该组合物的厚度的控制变得困难,有时由该组合物的烧结体构成的接合部位的厚度变得不均匀。另外,流出自身有时也会成为使半导体封装的可靠性降低的要因。
因此,本发明的课题在于提供可消除上述的现有技术所具有的各种缺点的接合用组合物及接合结构。
本发明通过提供一种接合用组合物来解决上述的课题,该接合用组合物包含铜粉、液介质及还原剂,
上述还原剂具有至少1个氨基及多个羟基,
上述还原剂的沸点比上述液介质的沸点高,
上述还原剂的熔点为上述铜粉的烧结温度以下。
另外,本发明提供一种导电体的接合结构的制造方法,其包含:
将上述的接合用组合物涂布于第一导电体的表面上而形成涂膜,
使上述涂膜干燥,将上述液介质的至少一部分除去而得到干燥涂膜,
将第二导电体层叠于上述干燥涂膜上,使上述干燥涂膜夹在上述第一导电体与上述第二导电体之间,
通过对上述干燥涂膜进行加热而使该干燥涂膜中的上述铜粉烧结,从而将上述第一导电体与上述第二导电体进行接合。
进而,本发明提供一种导电体的接合结构,其是两个导电体通过接合部位被电连接而成的导电体的接合结构,其中,
上述连接部位由以铜为主的材料形成,
在上述接合部位形成有以下的结构(3)。
[化学式1]
式中,R3~R5分别独立地表示氢原子、羟基、碳原子数为1以上且10以下的烃基、或具有羟基的碳原子数为1以上且10以下的烃基,
*表示与铜的键合部位。
具体实施方式
以下对本发明基于其优选的实施方式进行说明。本发明涉及一种包含铜粉、液介质及还原剂的接合用组合物。本发明的接合用组合物适宜用于将两个导电体进行接合。接合用组合物通过将其夹在两个导电体间并在该状态下进行烧成而成为导电膜,从而使两个导电体接合并且导通。
接合用组合物包含以下的成分作为其构成成分。以下,对这些成分分别进行说明。
(a)铜粉
(b)液介质
(c)还原剂
接合用组合物中所含的(a)的铜粉由铜粒子的集合体构成。在以下的说明中所谓“铜粉”根据上下文是指铜粒子、或是指铜粒子的集合体。铜粒子是以铜作为主要构成成分的粒子,例如是实质上仅由铜形成且在剩余部分中包含不可避免的杂质的粒子、或以铜作为主体(例如超过50质量%为铜。)且除了铜以外还包含其他成分的粒子。从提高导电性的观点出发,铜粒子优选包含80质量%以上的铜。
铜粒子的形状例如可以为球状。或者也可以为球状以外的形状、例如薄片状、板状、树枝状、棒状等。铜粒子的形状依赖于其制造方法。例如在使用湿式还原法或雾化法的情况下容易得到球状粒子。在使用电解还原法的情况下容易获得树枝状或棒状的粒子。薄片状或板状的粒子例如通过对球状的粒子施加机械外力并塑性变形为扁平状而得到。所述铜粒子例如可以仅由球状构成,或者也可以将球状与薄片状等混合而使用。
铜粒子为球状时的粒径以通过扫描型电子显微镜观察的图像解析而测定的累积体积50容量%时的体积累积粒径DSEM50表示,优选为0.03μm以上,更优选为0.05μm以上。另外,优选为20μm以下,更优选为10μm以下。
关于DSEM50,从铜粒子的扫描型电子显微镜图像中随机地选择50个以上而测定粒径(Heywood直径),接着,由所得到的粒径算出假定粒子为圆球时的体积,将该体积的累积体积50容量%时的体积累积粒径设定为DSEM50。
具体而言,使用Mountech公司制Mac-View,读入铜粒子的图像数据后,随机地选择50个以上的数据上的铜粒子,分别测定该粒子的粒径(Heywood直径)、该粒子的二维投影图像的面积S及该粒子的二维投影图像的周围长L。接着,由所得到的Heywood直径算出假定粒子为圆球时的体积,将该体积的累积体积50容量%时的体积累积粒径设定为DSEM50。
铜粒子是否为球形通过下述的方法进行判断。由通过上述的方法而随机地选择的各粒子的面积S和周围长L算出圆形度系数4πS/L2,进一步算出其算术平均值。在圆形度系数的算术平均值优选为0.85以上、进一步优选为0.90以上的情况下,铜粒子定义为球状。
另外,铜粒子为薄片状时的粒径通过激光衍射散射式粒度分布测定法而得到的累积体积50容量%时的体积累积粒径D50优选为0.3μm以上,更优选为0.5μm以上,进一步优选为0.7μm以上。另外,薄片状的铜粒子的粒径以D50表示,优选为100μm以下,更优选为70μm以下,进一步优选为50μm以下。通过包含这种粒径的粒子,能够形成致密地烧结的涂膜,能够实现导电体彼此的高接合强度和导电可靠性的提高。所谓薄片状是指具有形成粒子的主表面的一对板面和与这些板面正交的侧面的形状,板面及侧面可分别独立地为平面、曲面或凹凸面。
D50的测定例如可以通过以下的方法来进行。即,将0.1g的测定试样与分散剂水溶液混合,用超声波均化器(日本精机制作所制、US-300T)进行1分钟分散。之后,作为激光衍射散射式粒度分布测定装置,例如使用MicrotracBEL公司制MT3300 EXII来测定粒度分布。需要说明的是,本测定方法也可以应用于球状以外的铜粒子。
在铜粒子包含薄片状的粒子的情况下,薄片状铜粒子的长轴a的长度相对于短轴b的长度之比(以下,也将其称为长宽比(a/b)。)优选为2以上,优选为5以上。另外,长宽比优选为80以下,更优选为40以下。通过进一步包含这种形状的粒子,能够形成致密地烧结的涂膜,能够实现导电体彼此的高接合强度和导电可靠性的提高。
薄片状铜粒子中的长轴a及短轴b的长度如以下那样操作而求出。即,对于测定对象的粒子,确定其横截长最长的线段,考虑以该线段作为旋转轴并围绕该旋转轴旋转360度而得到的立体。对于该立体,求出与旋转轴正交的方向上的二维投影图像,确定该二维投影图像所外接的长方形。将该长方形的长边的长度设定为长轴a。另一方面,关于短轴b,对于上述的立体,求出沿着旋转轴的方向上的二维投影图像,确定该二维投影图像所外接的长方形。将该长方形的长边的长度设定为短轴b。随机地选择50个以上的粒子,通过上述的方法对各粒子分别确定长轴a及短轴b,算出它们的算术平均值。
接合用组合物中所含的(b)的液介质是为了使铜粉及还原剂分散并将接合用组合物制成糊状或油墨状的性状而使用的。液介质优选在室温(25℃)下为液体。另外,从使接合用组合物的印刷性变得良好的观点及使接合用组合物中均匀地存在还原剂的观点出发,液介质优选为可溶解(c)的还原剂的物质。另外,从抑制铜粉的氧化的观点出发,液介质优选为非水介质。例如优选为一元或多元醇。特别是从接合用组合物的印刷性、还原剂在液介质中的溶解性及液介质的挥发性的观点出发,醇优选为沸点低于300℃的多元醇。作为多元醇,例如可列举出丙二醇(沸点:188℃)、乙二醇(沸点:197℃)、己二醇(沸点:197℃)、二乙二醇(沸点:245℃)、1,3-丁二醇(沸点:207℃)、1,4-丁二醇(沸点:228℃)、二丙二醇(沸点:231℃)、三丙二醇(沸点:273℃)、甘油(沸点:290℃)、聚乙二醇200(沸点:250℃)、聚乙二醇300(沸点:250℃)等。液介质可以单独使用一种或将两种以上组合使用。
接合用组合物中所含的(c)的还原剂是为了促进由接合用组合物的烧成产生的铜粒子彼此的烧结而使用的。为了该目的,还原剂为具有至少1个氨基及多个羟基的结构的物质是有利的。通过使用具有这样的结构的还原剂,与具有多个羟基但不含氨基的还原剂相比,可促进铜粒子彼此的烧结,能够获得致密的烧结结构。因此,即使还原剂为少量,也能够获得包含具有高接合强度的接合部位的接合结构。
另外,从提高还原力的观点出发,还原剂优选具有3个以上的羟基,进一步优选具有4个以上,更进一步优选具有5个以上。
优选还原剂的沸点比液介质的沸点高、另外还原剂的熔点为铜粉的烧结温度以下。因此,还原剂在接合用组合物的干燥时(使接合用组合物的涂膜干燥而除去液介质而得到干燥涂膜时)停留在接合用组合物中,并且在干燥后的接合用组合物的烧成时(将接合用组合物的干燥涂膜进行烧成而使铜粉彼此烧结时)进行熔融。若使用这样的还原剂,则由于能够将液介质从该接合用组合物的涂膜中除去,因此能够提高该接合用组合物的干燥涂膜的形状保持性。其结果是,在烧成时,即使该接合用组合物的干燥涂膜被加压,该接合用组合物也不易从两个导电体间挤出,厚度的控制变得容易。另外,在将该接合用组合物的干燥涂膜进行烧成时,通过还原剂熔融而在干燥涂膜中均匀地扩展,从而铜粉的烧结被均匀地促进,能够获得更致密的烧结结构。
从提高干燥涂膜的形状保持性的观点出发,还原剂优选在室温(25℃)下为固体。从上述的观点出发,还原剂的熔点优选为30℃以上且200℃以下,进一步优选为50℃以上且200℃以下,更进一步优选为70℃以上且200℃以下。
从上述的观点出发,还原剂的沸点优选为300℃以上,进一步优选为330℃以上,更进一步优选为350℃以上。
从使接合用组合物的印刷性变得良好的观点及使还原剂在接合用组合物中均匀地存在的观点出发,还原剂优选为在室温(25℃)下可溶解于液介质中的物质、或将液介质加温而溶解后在冷却至室温(25℃)时不会析出而溶解的物质。还原剂是否可溶解于液介质中通过相对于4g液介质添加6g的还原剂并在上述的条件下使其溶解时还原剂的全部量是否溶解来进行判断。
从上述的观点出发,作为还原剂,优选使用下述的式(1)或(2)所表示的氨基醇化合物。
[化学式2]
式(1)或(2)中,R1~R6分别独立地表示氢原子、羟基、碳原子数为1以上且10以下的烃基、或具有羟基的碳原子数为1以上且10以下、优选碳原子数为1以上且4以下的烃基。作为烃基,可列举出饱和或不饱和的脂肪族基。该脂肪族基可以是直链状的,或者也可以是支链状的。作为烃基的例子,可列举出甲基、乙基、丙基等。
式(2)中,R7表示碳原子数为1以上且10以下、优选碳原子数为1以上且4以下的二价的烃基、或具有羟基的碳原子数为1以上且10以下、优选碳原子数为1以上且4以下的二价的烃基。作为烃基,可列举出饱和或不饱和的脂肪族基。该脂肪族基可以是直链状的,或者也可以是支链状的。作为烃基的例子,可列举出亚甲基、亚乙基、亚丙基、亚丁基等。
在式(1)中,R1~R5中的至少两个包含羟基。即,R1~R5中的至少两个为羟基或具有羟基的碳原子数为1以上且10以下的烃基。另外在式(2)中,R1~R6中的至少两个包含羟基。即,R1~R6中的至少两个为羟基或具有羟基的碳原子数为1以上且10以下的烃基。特别是在式(1)中,R1~R5中的至少两个优选为碳原子数为1以上且4以下的低级的羟基烷基。另外在式(2)中,R1~R6中的至少两个优选为碳原子数为1以上且4以下的低级的羟基烷基。这种情况下,羟基烷基中的羟基优选与烷基的末端键合。
从提高还原力的观点出发,式(1)所表示的还原剂优选R1~R5中的三个以上包含羟基,进一步优选四个以上包含羟基,更进一步优选包含五个羟基。通过同样的理由,式(2)所表示的还原剂优选R1~R6中的三个以上包含羟基,进一步优选四个以上包含羟基,更进一步优选包含五个羟基。
作为式(1)或(2)所表示的氨基醇化合物的具体例子,可列举出双(2-羟基乙基)亚氨基三(羟基甲基)甲烷(BIS-TRIS、熔点:104℃、沸点:超过300℃、相当于式(1))、2-氨基-2-(羟基甲基)-1,3-丙二醇(TRIS、熔点:169~173℃、沸点:超过300℃、相当于式(1))、1,3-双(三(羟基甲基)甲基氨基)丙烷(BIS-TRIS propane、熔点:164~165℃、沸点:超过300℃、相当于式(2))等。这些化合物均由于熔点高、在干燥工序中可维持液状,因此从涂膜的平滑性优异的观点出发优选。
上述的还原剂可以单独使用一种,或者可以将两种以上组合使用。在任一情况下,关于接合用组合物中的还原剂的比例,从提高铜粒子的烧结性的观点出发,相对于铜粉100质量份均优选为0.1质量份以上,进一步优选为1质量份以上。另外,关于还原剂的比例,从使铜的烧结结构变得致密的观点出发,相对于铜粉100质量份均优选为10质量份以下,进一步优选为8质量份以下。
另一方面,关于接合用组合物中的液介质的比例,从对接合用组合物赋予适度的粘性、提高将该接合用组合物涂布于导电体上时的涂膜的形状保持性的观点出发,相对于铜粉100质量份优选为10质量份以上且40质量份以下,进一步优选为10质量份以上且35质量份以下。
从提高涂布性或印刷性的观点出发,接合用组合物在烧成前的状态下的粘度(25℃)优选为10Pa·s以上且200Pa·s以下,更优选为15Pa·s以上且200Pa·s以下,进一步优选为20Pa·s以上且180Pa·s以下,进一步优选为20Pa·s以上且100Pa·s以下,更进一步优选为20Pa·s以上且60Pa·s以下。接合用组合物的粘度利用流变仪(粘弹性测定装置)进行测定。测定值是将传感器设定为并联型时的剪切速度10s-1下的值。
接合用组合物除了包含上述的(a)~(c)的成分以外,还可以包含其他的成分。作为这样的成分,例如可列举出粘合剂成分、表面张力调整剂、消泡剂、粘度调整剂等。关于接合用组合物中的这些成分的比例,其全部量相对于铜粉100质量份优选为0.1质量份以上且10质量份以下。
接着,对使用了上述的接合用组合物的导电体的接合结构的制造方法进行说明。该接合结构是两个导电体通过铜的接合部位被电连接而成的结构。为了制造该接合结构,首先,第一导电体被交付于涂布工序。在涂布工序中,在第一导电体的表面上涂布接合用组合物而形成涂膜。对接合用组合物的涂布的手段没有特别限制,可以使用公知的涂布手段。例如可以使用丝网印刷、分配印刷、凹版印刷、胶版印刷等。
从形成充分厚的接合结构的观点出发,涂膜的厚度优选设定为1μm以上且200μm以下,进一步优选设定为5μm以上且150μm以下。
一旦形成接合用组合物的涂膜,该涂膜就被交付于干燥工序。在干燥工序中,通过干燥从该涂膜中除去液介质的至少一部分,得到该液介质的量减少的干燥涂膜。通过从涂膜中除去液介质,能够进一步提高干燥涂膜的形状保持性,在后述的烧成工序中对干燥涂膜施加压力时,能够抑制该干燥涂膜的变形,可有效地防止干燥涂膜从两个导电体之间挤出。所谓干燥涂膜是被干燥至液介质相对于涂膜的总质量成为9质量%以下为止的涂膜。
对于液介质的除去,可以使用利用了该液介质的挥发性的自然干燥、热风干燥、红外线的照射、热板干燥等。液介质被除去之后的干燥涂膜中的该液介质的比例相对于涂膜的总质量100质量份,如上所述优选为9质量份以下,更优选为7质量份以下,进一步优选为5质量份以下。
一旦获得干燥涂膜,接着将第二导电体层叠于该干燥涂膜上。第一导电体与第二导电体可以由同种的材料构成,或者也可以由异种的材料构成。若考虑与涂膜中包含的铜粉的接合性,则导电体优选由铜、银、金等金属构成。
被两个导电体夹持的干燥涂膜接下来被交付于烧成工序。在烧成工序中将涂膜进行加热而使涂膜中所含的铜粒子彼此烧结。烧成的气氛优选为不活泼气体气氛。作为不活泼气体,例如可以适宜使用氮或氩等。烧成温度优选为150℃以上且350℃以下,进一步优选为200℃以上且350℃以下,更进一步优选为230℃以上且300℃以下。以烧成温度为上述的范围作为条件,烧成时间优选为0.5分钟以上且60分钟以下、特别是1分钟以上且30分钟以下。
烧成可以在无加压下或加压下进行。所谓无加压下是指除了由两个导电体的自重产生的力(重力)以外未对干燥涂膜施加压力。通过在无加压下进行烧成,具有能够将高度不同的半导体芯片同时接合的优点和不需要加压装置的优点。另一方面,在加压下进行烧成的情况下,出于协助铜粒子彼此的烧结的目的,施加优选为0.001MPa以上且20MPa以下、进一步优选为0.01MPa以上且15MPa以下的压力。
若使用以往已知的接合用组合物例如专利文献1中记载的接合用组合物在加压下进行烧成,则涂膜没有干燥,其结果是涂膜的流动性高,因此涂膜发生变形而涂膜从两个导电体间挤出。若出于防止涂膜的挤出的目的而使由专利文献1中记载的接合用组合物形成的涂膜干燥,则助烧结成分也与液介质一起挥发。因此,若使用这样的涂膜在加压下进行烧成,则铜的烧结性不足,不能得到充分的接合强度。
与此相对,根据本发明,起因于使用特定的化合物作为接合用组合物中所含的还原剂,从而即使是将涂膜干燥后在加压下进行烧成,也可有效地防止涂膜的挤出,并且可获得充分高的接合强度。另外,通过烧成,干燥涂膜中的铜粒子彼此充分地进行烧结而形成致密的烧结结构。其结果是,通过由接合用组合物的烧结体构成的接合部位将第1及第二导电体电连接。并且,通过形成致密的烧结结构,两个导电体的接合强度变得极为良好。而且,在接合部位中,由于铜粒子彼此的烧结高度地进行,因此成为接近块体(bulk)铜的结构体。其结果是,接合部位的导热性也变高。
像这样操作而形成的接合部位由以铜为主的材料形成。在用于形成接合部位的接合用组合物中包含上述的式(1)所表示的还原剂的情况下,在接合部位形成有以下的结构(3)。
[化学式3]
式中,R3~R5分别独立地表示氢原子、羟基、碳原子数为1以上且10以下的烃基或具有羟基的碳原子数为1以上且10以下的烃基。R3~R5的详细情况如上所述。另外,*表示与铜的键合部位。
在接合部位是否形成有上述的结构(3)可以通过以接合部位的截面作为对象,利用TOF-SIMS进行质量分析等来确认。例如在使用BIS-TRIS作为还原剂的情况下,在TOF-SIMS中的正极侧的质谱中观察到起因于C-N(Cu)2的分子量为152的片段。
接合部位优选其厚度按照将两个导电体可靠地结合、并且成为充分高的导电性及导热性的方式进行调整。例如接合部位优选将其厚度设定为1μm以上且200μm以下,进一步优选设定为3μm以上且150μm以下。接合部位的厚度例如可以通过调整上述的接合用组合物的涂膜的厚度来控制。接合部位的厚度通过将该接合部位进行树脂包埋后进行研磨并利用电子显微镜对该研磨面进行观察来测定。
具有这样的接合部位的导电体的接合结构有效利用其高的接合强度、导热性的特性,适宜用于暴露于高温下的环境例如车载用电子电路或安装有功率器件的电子电路。
实施例
以下,通过实施例对本发明更详细地进行说明。然而,本发明的范围并不限制于所述实施例。只要没有特别说明,则“%”及“份”分别是指“质量%”及“质量份”。
〔实施例1〕
(1)接合用组合物的制备
作为铜粉,使用了DSEM50为0.16μm的球状的铜粉。作为还原剂,使用了双(2-羟基乙基)亚氨基三(羟基甲基)甲烷。该还原剂在25℃下为固体,熔点为104℃,沸点超过300℃。作为液介质,使用了乙二醇。该液介质的沸点为197℃。将它们混合而得到糊状的接合用组合物。接合用组合物中的还原剂的比例相对于铜粉100份为2.5份,液介质的比例相对于铜粉100份为22.5份。另外,剪切速度10s-1下的接合用组合物的粘度在25℃下为25Pa·s。
(2)接合结构的制造
在10mm四方的正方形的铜板(厚度0.5mm)的中央,通过丝网印刷而涂布接合用组合物并形成涂膜。涂膜形成为5mm四方的正方形。涂膜的厚度为35μm。将该涂膜在热风干燥机中、以110℃、10分钟使其干燥而除去液介质,在室温下放置,得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。
接着,在干燥涂膜上载置5mm四方的正方形的铜板(厚度0.5mm)。在该状态下施加6MPa的压力,在氮气氛下在280℃下进行10分钟烧成,制作了两个接合结构。另外,通过利用TOF-SIMS的质量分析而确认在铜的接合部位形成有上述的结构(3)所表示的结构。
〔实施例2〕
将接合用组合物中的还原剂的比例相对于铜粉100份设定为5.0份,将液介质的比例相对于铜粉100份设定为20.0份,除此以外,与实施例1同样地操作而得到糊状的接合用组合物。另外,剪切速度10s-1下的接合用组合物的粘度在25℃下为42Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。而且,在与实施例1同样的条件下制作了接合结构。通过利用TOF-SIMS的质量分析而确认在铜的接合部位形成有上述的结构(3)所表示的结构。
〔比较例1〕
将还原剂设定为内消旋-赤藓醇(熔点:121℃、沸点:330℃),将接合用组合物中的还原剂的比例相对于铜粉100份设定为2.5份,将液介质的比例相对于铜粉100份设定为22.5份,除此以外,与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为59Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。而且,在与实施例1同样的条件下制作了接合结构。通过利用TOF-SIMS的质量分析而确认在铜的接合部位未形成上述的结构(3)所表示的结构。需要说明的是,所谓内消旋-赤藓醇是具有四个羟基但不具有氨基的还原剂。
〔比较例2〕
将还原剂设定为内消旋-赤藓醇(熔点:121℃、沸点:330℃),将接合用组合物中的还原剂的比例相对于铜粉100份设定为5.0份,将液介质的比例相对于铜粉100份设定为20.0份,除此以外,与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为70Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。而且,在与实施例1同样的条件下制作了接合结构。通过利用TOF-SIMS的质量分析而确认在铜的接合部位未形成上述的结构(3)所表示的结构。
〔比较例3〕
将还原剂设定为三羟甲基丙烷(熔点:58℃、沸点:296℃),将接合用组合物中的还原剂的比例相对于铜粉100份设定为2.5份,将液介质的比例相对于铜粉100份设定为22.5份,除此以外,与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为51Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。而且,在与实施例1同样的条件下制作了接合结构。通过利用TOF-SIMS的质量分析而确认在铜的接合部位未形成上述的结构(3)所表示的结构。需要说明的是,三羟甲基丙烷是具有羟基但不具有氨基的还原剂。
〔比较例4〕
将还原剂设定为三羟甲基丙烷(熔点:58℃、沸点:296℃),将接合用组合物中的还原剂的比例相对于铜粉100份设定为5.0份,将液介质的比例相对于铜粉100份设定为20.0份,除此以外,与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为66Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。另外,确认干燥涂膜中的液介质的含量,结果为4质量%以下。而且,在与实施例1同样的条件下制作了接合结构。通过利用TOF-SIMS的质量分析而确认在铜的接合部位未形成上述的结构(3)所表示的结构。
〔实施例3〕
将接合用组合物中的铜粉变更为DSEM50为0.14μm的球状铜粉与D50为4.9μm且长宽比为13的薄片状铜粉的混合物。球状铜粉和薄片状铜粉在铜粉的混合物中所占的含有比例设定为球状铜粉70质量%:薄片状铜粉30质量%。另外,将还原剂的比例相对于铜粉100份设定为2.5份。进而,将液介质变更为聚乙二醇300与己二醇的混合物。各液介质相对于铜粉100份的含有比例设定为如表2中所示的那样。此外与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为34Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。确认干燥涂膜中的液介质的含量,结果为5质量%以下。在与实施例1同样的条件下制作接合结构,结果通过利用TOF-SIMS的质量分析而确认在铜的接合部位形成有上述的结构(3)所表示的结构。
〔实施例4〕
将接合用组合物中的铜粉变更为与实施例3同样的球状铜粉与薄片状铜粉的混合物。另外,将还原剂的比例相对于铜粉100份设定为0.1份。进而,将液介质变更为聚乙二醇与己二醇的混合物。各液介质相对于铜粉100份的含有比例设定为如表2中所示的那样。此外与实施例1同样地操作而得到糊状的接合用组合物。剪切速度10s-1下的接合用组合物的粘度在25℃下为14Pa·s。而且,以与实施例1同样的条件得到干燥涂膜。确认干燥涂膜中的液介质的含量,结果为5质量%以下。在与实施例1同样的条件下制作接合结构,结果通过利用TOF-SIMS的质量分析而确认在铜的接合部位形成有上述的结构(3)所表示的结构。
〔评价〕
对于实施例及比较例中得到的接合结构,通过以下的方法来评价及测定外观及剪切强度。另外,对于干燥涂膜,也通过以下的方法进行了外观的评价。将它们的结果示于以下的表1及表2中。
〔干燥涂膜的外观〕
通过目视对干燥涂膜进行观察,确认有无开裂、表面的异物、孔,按照以下的基准进行了评价。
A:开裂、表面的异物及孔均未确认到。
B:确认到开裂、表面的异物及孔中的任一者。
〔接合部位的外观〕
对接合部位进行目视观察,按照以下的基准来评价从铜板的周围挤出的程度。
A:未观察到接合部位从铜板的周围挤出。
B:观察到接合部位从铜板的周围挤出。
〔剪切强度〕
使用XYZTEC公司制的粘合力试验仪Condor Sigma来测定接合结构的剪切强度。按照以下的基准进行了评价。剪切强度(MPa)为以断裂载荷(N)/接合面积(mm2)定义的值。
A:30MPa以上
B:低于30MPa
如由表1及表2中所示的结果表明的那样,判明各实施例中得到的接合结构尽管是在加压下将接合用组合物进行烧成而得到的结构,也未观察到该组合物从铜板挤出,得到具有均匀的厚度的接合部位。进而判明,各实施例中得到的接合结构与铜板的接合强度高。
产业上的可利用性
根据本发明,能够容易地形成接合用组合物的挤出的发生少、并且包含具有高接合强度的接合部位的接合结构。
Claims (7)
1.一种接合用组合物,其包含铜粉、液介质及还原剂,
所述还原剂具有至少1个氨基及多个羟基,
所述还原剂的沸点比所述液介质的沸点高,
所述还原剂的熔点为所述铜粉的烧结温度以下。
3.根据权利要求2所述的接合用组合物,其中,所述还原剂为双(2-羟基乙基)亚氨基三(羟基甲基)甲烷。
4.根据权利要求1~3中任一项所述的接合用组合物,其中,剪切速度10s-1及25℃下的粘度为10Pa·s以上且200Pa·s以下。
5.根据权利要求1~4中任一项所述的接合用组合物,其中,相对于所述铜粉100质量份,包含0.1质量份以上且10质量份以下的所述还原剂,并且包含10质量份以上且40质量份以下的所述液介质。
6.一种导电体的接合结构的制造方法,其包含:
将权利要求1~5中任一项所述的接合用组合物涂布于第一导电体的表面上而形成涂膜,
使所述涂膜干燥,将所述液介质的至少一部分除去而得到干燥涂膜,
将第二导电体层叠于所述干燥涂膜上,使所述干燥涂膜夹在所述第一导电体与所述第二导电体之间,
通过对所述干燥涂膜进行加热而使该干燥涂膜中所含的所述铜粉烧结,从而将所述第一导电体与所述第二导电体进行接合。
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TW202012564A (zh) | 2020-04-01 |
US11931808B2 (en) | 2024-03-19 |
CN112437706B (zh) | 2024-01-02 |
CN117696898A (zh) | 2024-03-15 |
US20240181528A1 (en) | 2024-06-06 |
EP3834965A1 (en) | 2021-06-16 |
WO2020032161A1 (ja) | 2020-02-13 |
EP3834965A4 (en) | 2021-08-18 |
JPWO2020032161A1 (ja) | 2021-03-11 |
US20210138541A1 (en) | 2021-05-13 |
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