CN116963856A - 接合结构体 - Google Patents

接合结构体 Download PDF

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Publication number
CN116963856A
CN116963856A CN202280019470.5A CN202280019470A CN116963856A CN 116963856 A CN116963856 A CN 116963856A CN 202280019470 A CN202280019470 A CN 202280019470A CN 116963856 A CN116963856 A CN 116963856A
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CN
China
Prior art keywords
joined
joint
joining
ratio
bonding
Prior art date
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Pending
Application number
CN202280019470.5A
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English (en)
Inventor
山内真一
穴井圭
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Publication date
Application filed by Mitsui Mining and Smelting Co Ltd filed Critical Mitsui Mining and Smelting Co Ltd
Publication of CN116963856A publication Critical patent/CN116963856A/zh
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    • B22F7/00—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
    • 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
    • B22F7/062—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 involving the connection or repairing of preformed parts
    • B22F7/064—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 involving the connection or repairing of preformed parts using an intermediate powder layer
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    • B22F7/00—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
    • 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
    • B22F7/08—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 with one or more parts not made from powder
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    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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    • B33Y10/00—Processes of additive manufacturing
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0425—Copper-based alloys
    • C—CHEMISTRY; METALLURGY
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Abstract

接合结构体(1)是2个被接合件(11、12)与在这些被接合件之间相邻地形成的接合部(15)接合而成的。接合部(15)由以铜为主体的材料构成。在接合结构体(1)的厚度方向(Z)剖视中，该接合结构体的端部区域(A2)处的被接合件与接合部的接合比例(Rs)相对于该接合结构体的中央区域(A1)处的被接合件与接合部的接合比例(Rc)之比(Rs/Rc)为0.6以上且0.9以下。接合比例(Rc)为0.3以上。

Description

接合结构体
技术领域
本发明涉及一种接合结构体。
背景技术
随着近年来的世界性节能化的趋势，作为逆变器等电力转换/控制装置，被称为功率器件的半导体器件被广泛使用。作为能够应用于这样的器件的技术，本申请人提出了通过包含铜且具有预定的化学结构的接合部将2个被接合件连接的接合结构(参照专利文献1)。
现有技术文献
专利文献
专利文献1：国际公开第2020/032161号小册子
发明内容
专利文献1所记载的接合结构能够显现出高接合强度，例如在将具备该接合结构的半导体器件用于汽车用途等时，即使长期置于温度变化剧烈的环境中，也能够较高地维持接合强度，即，要求高接合可靠性。
本发明的课题在于提供一种具有高接合可靠性的接合结构体。
本发明提供一种接合结构体，其是2个被接合件与在这些被接合件之间相邻地形成的接合部接合而成的，
所述接合部由以铜为主体的材料构成，
在所述接合结构体的厚度方向剖视中，该接合结构体的端部区域处的所述被接合件与所述接合部的接合比例Rs相对于该接合结构体的中央区域处的所述被接合件与所述接合部的接合比例Rc之比(Rs/Rc)为0.6以上0.9以下，
所述接合比例Rc为0.3以上。
附图说明
图1的(a)是本发明的接合结构体的一实施方式的示意性的俯视图，图1的(b)是图1的(a)中的I-I线处的示意性的剖视图。
图2的(a)是示意性地表示在图1的(a)所示的接合结构体1的厚度方向剖视中，被接合件11与接合部15的界面的中央区域A1的全景图像的放大图，图2的(b)是示意性地表示在图1的(a)所示的接合结构体1的厚度方向剖视中，被接合件11与接合部15的界面的端部区域A2的全景图像的放大图。
图3的(a)是实施例1的接合结构体1的冷热循环试验前的超声波图像，图3的(b)是实施例1的接合结构体1的冷热循环试验后的超声波图像。
图4的(a)是比较例1的接合结构体1的冷热循环试验前的超声波图像，图4的(b)是比较例1的接合结构体1的冷热循环试验后的超声波图像。
具体实施方式
以下，基于其优选的实施方式对本发明的接合结构体进行说明。
图1的(a)和(b)表示本发明的接合结构体的一实施方式。在该图所示的实施方式中，接合结构体1具有第1被接合件11(以下，也将其简称为“被接合件11”。)和第2被接合件12(以下，也将其简称为“被接合件12”。)，具有在这些被接合件11、12之间相邻地形成的接合部15。接合结构体1中的被接合件11、12经由接合部15接合，在各被接合件11、12与接合部15之间不隔着其他构件。该图所示的实施方式的接合结构体1成为在第2被接合件12的一个面上依次层叠有接合部15和第1被接合件11的状态。
图1的(a)和(b)所示的被接合件11构成为其尺寸比被接合件12小，但不限于该方式，各被接合件11、12也可以是彼此相同的尺寸，被接合件11也可以构成为比被接合件12大。而且，该图所示的各被接合件11、12以及接合部15均为平面，但也可以根据需要而成为曲面。
另外，图1的(a)和(b)所示的接合部15形成为其周缘比被接合件11的周缘向外侧延伸，但不限于该方式，也可以以接合部15的周缘与被接合件11的周缘一致的状态形成。
各被接合件11、12的种类没有特别限制，但优选在各被接合件11、12中的至少一者中，更优选在被接合件11、12这两者中，在与接合部15接触的面包含金属。在该情况下，两被接合件11、12也优选经由接合部15电连接。也就是说，各被接合件11、12分别独立，优选为导电体。作为形成各被接合件11、12的表面的金属，从提高导电性的观点出发，各自独立地优选列举金、银、铜、镍以及钛中的至少一种。
作为包含这样的金属的各被接合件11、12，可各自独立地列举出例如由上述金属构成的间隔件、散热板、半导体元件、以及在表面具有上述金属中的至少一种的基板等。作为基板，例如能够使用在陶瓷或氮化铝板的表面具有铜等金属层的绝缘基板等。在使用半导体元件作为被接合件的情况下，半导体元件包含Si、Ga、Ge、C、N、As等元素中的一种以上。存在于被接合件11、12的表面的金属既可以是金属单质，或者也可以是2种以上的金属的合金。
被接合件11优选为间隔件、散热板或半导体元件中的任一种。被接合件12优选为基板。
接合部15是包含铜作为主体的结构体，在各被接合件11、12之间相邻，优选介于俯视整个区域。接合部15优选含有50质量％以上的铜，更优选含有60质量％以上的铜。接合部中的铜的含量能够通过以接合结构体1的厚度方向截面为对象，利用能量色散型X射线光谱法(EDX)进行分析来测定。
这样的接合部15例如如后述的制造方法所示，能够将包含含有铜的金属颗粒的组合物与两被接合件一起焙烧，形成为金属颗粒彼此的烧结体。作为包含这样的颗粒而形成的烧结体的接合部15也可以在其结构中具有多个空孔。
本发明的接合结构体的特征之一在于，在沿厚度方向对其进行剖视中，被接合件与接合部的接合比例在接合结构体的中央区域与端部区域互不相同。
详细而言，如图1的(a)所示，在使接合结构体1的各被接合件11、12与接合部15接合的最大区域A0的俯视时的矩心与将最大区域A0的平面面积缩小至50％的相似形的俯视时的矩心一致时，将以该相似形的俯视形状表示的假想区域V1设为接合结构体1的中央区域A1。而且，在沿厚度方向Z对接合结构体1的中央区域A1进行剖视中，将位于上述的中央区域A1的至少一方的被接合件11、12与接合部15的界面处的接合比例设为第1接合比例Rc(以下，也将其简称为“接合比例Rc”。)。
需要说明的是，最大区域A0是在沿着厚度方向Z观察接合结构体1时，两被接合件11、12和接合部15全部存在的部位的最大的区域。因而，以图1的(a)和(b)所示的接合结构体1为例，最大区域A0与被接合件11的俯视时的配置区域一致。
另外，如图1的(a)所示，在接合结构体1的俯视时，在使最大区域A0的俯视时的矩心与将最大区域A0的平面面积缩小至90％的相似形的俯视时的矩心一致时，考虑由该相似形的俯视形状表示的假想区域V2。此时，在接合结构体1的俯视时，将位于该假想区域V2的外侧且比最大区域A0的周缘(在该图中，相当于被接合件11的周缘11e)靠内侧的区域设为接合结构体1的端部区域A2。而且，在沿厚度方向Z对接合结构体1的端部区域A2进行剖视中，将位于上述端部区域A2的至少一方的被接合件11、12与接合部15的界面处的接合比例设为第2接合比例Rs(以下，也将其简称为“接合比例Rs”。)。成为接合比例Rs的对象的界面设为与作为接合比例Rc的对象的界面相同的界面。
此时，接合比例Rs相对于接合比例Rc之比(Rs/Rc)优选为0.6以上，更优选为0.7以上。另外，Rs/Rc优选为0.9以下，更优选为0.8以下。也就是说，接合结构体1在至少一方的被接合件与接合部的界面，中央区域A1的接合比例比端部区域A2的接合比例高。
关于通过Rs/Rc为上述范围，接合结构体能够显现出高接合可靠性的理由，本发明的发明人推测如下。在以下的说明中，以图1中图示的附图标记为例进行说明。
在2个被接合件11、12之间形成有接合部15的接合结构体1典型地使用具有流动性的导电性的组合物作为接合部15的形成材料，在将该组合物配置于2个被接合件11、12之间的状态下，在一边加压一边加快升温速度的状态下进行焙烧而制作。此时，组合物在焙烧初期残留有流动性，因此通过加压，以位于被接合件11、12的周缘外侧的方式挤出组合物，或者在被接合件11、12的俯视中央区域A1以组合物的密度提高的方式移动。通过在该状态下进行烧结，在俯视中央区域A1成为比较紧密的结构，并且组合物高效地烧结，在各被接合件11、12之间，在该被接合件11、12的俯视整个区域形成充分显现出与被接合件11、12的密合性的接合部15。特别是，若Rs/Rc处于上述特定的范围，则维持作为接合结构体1整体的接合强度，并且缓和接合结构体1的端部区域A2的应力集中，因此在温度变化环境中也维持接合部的高接合功能，能够维持高接合可靠性。
与此相对，在加压不充分的条件、升温速度不适当的条件下形成接合部15的情况下，位于接合结构体1的俯视中央区域A1处的接合部15难以成为紧密的结构，Rs/Rc成为接近1的值。于是，无法缓和接合部15的端部区域A2的应力集中，难以维持接合可靠性。
接合比例Rc优选为0.3以上，更优选为0.4以上，进一步优选为0.5以上，从显现出与被接合件的充分的接合强度的方面出发，越高越优选。
接合比例Rs优选为0.35以上且0.6以下，更优选为0.35以上且0.55以下，进一步优选为0.35以上且0.5以下。通过接合比例Rs成为这样的比例，接合体的端部区域A2的弹性模量适度地降低，因此能够防止应力集中在端部区域A2而产生裂纹。
上述的比Rs/Rc、第1接合比例Rc以及第2接合比例Rs规定至少一方的被接合件11、12与接合部15的至少一方的界面处的关系，但上述的比以及各接合比例优选在被接合件11与接合部15的界面G1处至少满足，除此之外，更优选在被接合件12与接合部15的界面G2处也同样地满足上述的优选的范围。
这样的接合结构体1例如如后述的制造方法所示，能够通过在将包含含有铜的金属颗粒的导电性组合物与两被接合件11、12一起赋予预定的压力的状态下，以预定的升温速度进行焙烧而得到。
第1接合比例Rc和第2接合比例Rs能够通过以下的方法测定。
首先，将测定对象的接合结构体1进行树脂包埋后，通过光学显微镜观察，在接合结构体1的俯视时，分别划定最大区域A0、中央区域A1以及端部区域A2。之后，在通过最大区域A0的俯视下的矩心(在图1的(a)中，相当于第1被接合件11的俯视下的矩心)的位置，将树脂包埋的接合结构体在厚度方向上切断，对该剖切面进行研磨，进而通过离子铣削加工研磨面，之后，例如如图1的(b)所示，制作相当于通过矩心的厚度方向剖视观察的观察面。
接下来，在上述的观察面中的中央区域A1内的任意的位置，使用电子显微镜通过目测观察来确定成为测定对象的被接合件与接合部的界面G1或界面G2的位置。
接下来，在电子显微镜观察中，例如以测定视野的总长Lt成为30μm左右的方式拍摄对象变得清晰的倍率的多张图像并进行排列，由此获取全景图像。在该状态下，将被接合件11、12与接合部15的界面G1、G2中的一方的界面作为测定对象，测定该界面不清晰的部位的沿着面方向X的长度La的合计，将其作为中央区域A1的接合长度L1。代替于此，接合长度L1也可以通过从测定视野的总长Lt减去成为测定对象的被接合件11、12与接合部15的界面G1、G2清晰的部位的长度的合计来计算。接合长度L1能够以上述的电子显微镜图像、后述的二值化图像为对象，通过目测或根据需要使用软件来计算。
在图2的(a)中，以第1被接合件11与接合部15的界面G1为例，示出了中央区域A1的全景图像的示意图。在该示意图中，一并示出了总长Lt、长度La以及接合长度L1。
并且，将中央区域的接合长度L1相对于测定视野的总长Lt之比(L1/Lt)作为本发明中的第1接合比例Rc。
同样地，在上述的观察面中的端部区域A2内的任意的位置，使用电子显微镜通过目测观察来确定被接合件11、12与接合部15的界面G1、G2中的、与供于接合比例Rc的测定的界面相同的界面。
在端部区域A2内的测定中也同样地，在电子显微镜观察中，例如与上述的方法同样地以测定视野的总长Lt成为30μm左右的方式获取全景图像。在该状态下，测定成为测定对象的被接合件11、12与接合部15的界面不清晰的部位的沿着面方向X的长度Lb的合计，将其设为端部区域A2的接合长度L2。代替于此，接合长度L2也可以通过从测定视野的总长Lt减去各被接合件11、12与接合部15的界面清晰的部位的长度的合计来计算。接合长度L2能够以上述的电子显微镜图像、后述的二值化图像为对象，通过目测或根据需要使用软件来计算。
在图2的(b)中，以第1被接合件11与接合部15的界面G1为例，示出了端部区域A2的全景图像的示意图。在该示意图中，一并示出了总长Lt、长度Lb以及接合长度L2。
并且，将端部区域A2的接合长度L2相对于测定视野的总长Lt之比(L2/Lt)作为本发明中的接合比例Rs。
上述的“被接合件11、12与接合部15的界面G1、G2不清晰的部位”是指，在接合结构体1的制造时，金属颗粒与被接合件充分烧结的部位。另一方面，“被接合件11、12与接合部15的界面G1、G2清晰的部位”是指，在接合结构体1的制造时，金属颗粒与被接合件未烧结的部位。
关于被接合件11与接合部15的界面G1是否清晰，在电子显微图像中，在测定对象的被接合件11与接合部15的界面G1处，当沿着厚度方向观察二值化后的二值化图像时，如果观察到以相同颜色表示的区域与以不同颜色表示的区域的分界，则被接合件11与接合部15的界面G1清晰。另一方面，如果未观察到所述分界，则被接合件11与接合部15的界面G1不清晰。
对于被接合件12与接合部15的界面G2，也与上述方法同样地进行观察，能够判定为界面G2清晰或不清晰。
需要说明的是，为了便于说明，关于接合比例Rc、Rs的测定方法，以接合结构体1的厚度方向的一剖视观察进行了说明，但典型地，接合结构体1中的各被接合件11、12和接合部15在最大区域A0的俯视整个区域连续地接合。因而，对于接合结构体1而言，在考虑以最大区域A0的俯视时的矩心为中心的假想圆、以及通过该假想圆的中心且每隔30°切断该假想圆的假想放射状线时，观察将俯视时的接合结构体以该假想放射状线每隔30°在厚度方向上切断的截面而测定的各接合比例Rc、Rs均优选为上述范围。
接下来，对接合结构体的制造方法进行说明。本制造方法大致分为3个工序：在一个被接合件(例如被接合件12)的表面上涂布含有铜的接合用组合物而形成涂膜的涂布工序；使该涂膜干燥而形成干燥涂膜的干燥工序；以及在该干燥涂膜上进一步层叠另一个被接合件(例如被接合件11)，在该状态下一边加压一边加热而使其接合的接合工序。
首先，在一个被接合件的表面上涂布含有铜的接合用组合物而形成涂膜(涂布工序)。接合用组合物优选包含含有铜的金属颗粒和液体介质。接合用组合物的详细情况将在后述。
接合用组合物的涂布方法优选采用所形成的涂膜的厚度变得均匀、且能够涂布于涂布预定面的整个区域的方法。作为这样的涂布方法，例如可列举出丝网印刷、分配印刷、凹版印刷、胶版印刷等。从提高均匀的涂布性的观点出发，接合用组合物优选为包含液体介质的糊剂状或墨状。
从形成稳定地具有高接合强度的接合结构体的观点出发，所形成的涂膜的厚度在刚涂布后优选设定为1μm以上且250μm以下，更优选设定为5μm以上且150μm以下。另外，从不产生被接合件与接合体相邻而未密合的部分，容易在被接合件与接合体的接合面整个区域形成接合部，在接合面整个区域提高与接合对象的接合强度的观点出发，涂膜的俯视时的涂布面积优选以成为接合对象的被接合件中平面面积最小的被接合件的底面积以上的面积进行涂布。
接下来，使形成的涂膜干燥而得到干燥涂膜(干燥工序)。在本工序中，通过干燥从该涂膜中去除液体介质的至少一部分，得到涂膜中的液体介质的量减少的干燥涂膜。通过从涂膜中去除液体介质，能够提高干燥涂膜的保形性，另外，由于在该状态下将被接合件彼此接合，因此能够提高接合强度。干燥涂膜是指液体介质相对于膜的总质量的比例为9质量％以下的涂膜。在涂膜和使该涂膜干燥而成的干燥涂膜中，除了液体介质以外的各构成材料的含量实质上相同，因此干燥涂膜中的液体介质的比例例如能够通过测定干燥前后的涂膜的质量变化而计算。
为了干燥而去除液体介质，能够采用利用该液体介质的挥发性使液体介质挥发的方法，例如能够使用自然干燥、热风干燥、红外线的照射、热板干燥等干燥方法。
去除液体介质后的干燥涂膜中的该液体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。
本工序能够根据所使用的接合用组合物的组成而适当变更，在大气气氛下、在40℃以上且150℃以下、大气压、1分钟以上且60分钟以下进行时，不易发生接合用组合物和与其一起供于干燥的被接合件的变质，在维持被接合件的所期望的物性的同时提高被接合件彼此的接合强度的方面是优选的。
接下来，在干燥涂膜上层叠另一个被接合件并进行接合(接合工序)。详细而言，经过上述工序得到干燥涂膜后，将另一个被接合件层叠在该干燥涂膜上，得到第1被接合件和第2被接合件、以及在它们之间隔着干燥涂膜而配置的层叠体。该层叠体例如在第2被接合件的一个面上依次层叠有涂膜和第1被接合件。
然后，一边对层叠体进行加压一边以预定的升温速度进行加热，使干燥涂膜中所含的金属粉烧结，由此形成将2个被接合件彼此接合的接合部。
烧结时的气氛优选为氢、甲酸等还原气体气氛、或氮、氩等非活性气体气氛。
烧结温度优选为150℃以上且350℃以下，更优选为200℃以上且350℃以下，进一步优选为230℃以上且300℃以下。
烧结时的升温速度在从40℃至达到上述烧结温度的过程中，优选为120℃/分钟以上且2000℃/分钟以下，更优选为240℃/分钟以上且1500℃/分钟以下，进一步优选为360℃/分钟以上且1000℃/分钟以下。该升温速度比以往的接合结构体的制造所采用的升温速度快。通过以这样的速度进行，能够在短时间内制造满足上述Rs/Rc的关系的接合结构体。
烧结时施加的压力从加热开始至烧结结束为止，优选维持超过6MPa且为40MPa以下，更优选维持8MPa以上且30MPa以下，进一步优选维持10MPa以上且20MPa以下。
烧结时间以烧结温度处于上述范围的状态为条件，优选为0.5分钟以上且120分钟以下，更优选为1分钟以上且60分钟以下，优选为1分钟以上且30分钟以下。
经过以上的工序，成为在2个被接合件11、12之间形成有作为构成接合用组合物的含有铜的金属颗粒的烧结体的接合部15的接合结构体1。根据上述的优选的制造方法，能够适当地得到在第1被接合件11与接合部15之间、以及第2被接合件12与接合部15之间分别满足上述Rs/Rc的关系的接合结构体1。接合部15含有铜，另外，在接合用组合物含有后述的固体还原剂的情况下，在接合层形成以下的结构(1)。
式(1)中，R3至R5分别独立地表示氢原子、羟基、碳原子数1以上且10以下的烃基、或具有羟基的碳原子数1以上且10以下的烃基。R3至R5的详细情况可适当应用后述的化学式(2)和(3)的说明。另外，*表示与铜的键合部位。
在接合层是否形成有所述结构(1)，能够以接合部的截面为对象，通过进行基于TOF-SIMS的质谱分析等来确认。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由“C-N(Cu)2”引起的m/z152的片段。
接合用组合物包含由含有铜的金属颗粒构成的金属粉，优选还包含还原剂和液体介质。
在本发明中使用的金属粉优选由含有铜的金属颗粒的集合体构成。金属粉根据需要也可以还含有金、银、钯、铝、镍以及锡中的至少一种金属。
构成在本发明中使用的金属粉的金属颗粒的形状例如为球状、薄片状、枝晶状(树枝状)、棒状等。它们能够单独使用或组合多种使用。
金属颗粒为球状的情况下的粒径以通过扫描型电子显微镜观察的图像分析测定的累积体积50容量％下的体积累积粒径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。通过为这样的粒径，能够生产率高地形成薄型且具有均匀的厚度的涂膜，能够进一步提高被接合件彼此的接合强度。
另外，关于铜颗粒为薄片状的情况下的粒径，基于激光衍射散射式粒度分布测定法的累积体积50容量％下的体积累积粒径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，薄片状的铜颗粒的粒径以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。通过包含这样的粒径的颗粒，能够形成颗粒彼此无间隙地配置的涂膜，能够形成具有致密的结构的接合部，能够显现被接合件彼此的高接合强度。薄片状是指，具有形成颗粒的主面的一对板面和与这些板面正交的侧面的形状，板面和侧面能够分别独立地为平面、曲面或凹凸面。
接合用组合物中所含的还原剂优选在1个大气压、室温(25℃)下为固体。这样的还原剂用于促进由该组合物的焙烧引起的金属颗粒彼此的烧结，显现出高的接合强度。为了该目的，还原剂是具有至少1个氨基和多个羟基的化学结构是有利的。“在室温(25℃)下为固体”是指，还原剂的熔点超过25℃。以下，也将固体状的还原剂称为“固体还原剂”。
固体还原剂的熔点优选为金属粉的烧结温度以下。另外，固体还原剂的沸点也优选比后述的液体介质的沸点高。通过使用具有这样的物性的固体还原剂，在使接合用组合物的涂膜干燥而得到干燥涂膜时，能够使固体还原剂作为固体残留在接合用组合物中，其结果，能够提高该接合用组合物的干燥涂膜的保形性。
从高效地显现出进行加压接合时的高接合强度的观点、以及在使用导电体作为被接合件时显现出加压接合后的高导电可靠性的观点出发，作为固体还原剂，优选使用以下的化学式(2)或(3)所示的氨基醇化合物。
化学式(2)或(3)中，R1至R6分别独立地表示氢原子、羟基、碳原子数1以上且10以下的烃基、或具有羟基的碳原子数1以上且10以下的烃基。另外，式(2)中，R7表示碳原子数1以上且10以下的烃基，或具有羟基的碳原子数1以上且10以下的烃基。作为烃基，可列举出饱和或不饱和的脂肪族基团。该脂肪族基团既可以为直链状，或者也可以为支链状。
作为化学式(2)或(3)所示的氨基醇化合物的具体例，可列举出双(2-羟乙基)亚氨基三(羟基甲基)甲烷(BIS-TRIS，熔点：104℃，沸点：超过300℃，相当于化学式(2))、2-氨基-2-(羟基甲基)-1,3-丙二醇(TRIS，熔点：169℃～173℃，沸点：超过300℃，相当于化学式(2))、1,3-双(三(羟基甲基)甲基氨基)丙烷(BIS-TRIS丙烷，熔点：164℃～165℃，沸点：超过300℃，相当于化学式(3))等。其中，从得到在提高金属颗粒彼此的烧结性的同时显现出高接合强度的接合体的观点出发，优选使用双(2-羟基乙基)亚氨基三(羟基甲基)甲烷作为固体还原剂。
上述固体还原剂能够单独使用一种，或者能够组合使用两种以上。在任一情况下，从提高金属颗粒彼此的烧结性的观点出发，接合用组合物中的固体还原剂的比例相对于金属粉100质量份优选为0.1质量份以上，更优选为1质量份以上。另外，从维持金属粉在接合用组合物中所占的比例、并且发挥对被接合件的适当的涂布性能的观点出发，现实的是设为10质量份以下，优选设为8质量份以下，进一步优选设为5质量份以下。
从提高涂膜的涂布性的观点出发，接合用组合物优选还包含液体介质。从兼具接合用组合物的涂布性、固体还原剂的溶解性、以及伴随液体介质的适度的挥发性的干燥涂膜的形成效率的提高的观点出发，液体介质优选为非水溶剂，更优选为一元醇或多元醇，进一步优选为多元醇。
作为多元醇，例如可列举出丙二醇、乙二醇、己二醇、二甘醇、1,3-丁二醇、1,4-丁二醇、双丙甘醇、三丙二醇、丙三醇、聚乙二醇200、聚乙二醇300等。液体介质能够单独使用一种或组合使用两种以上。
在接合用组合物中包含液体介质的情况下，从提高将接合用组合物涂布于被接合件上时的涂膜的保形性和所形成的涂膜的厚度的均匀性的观点出发，液体介质的含量相对于金属粉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。
接合用组合物只要可发挥本发明的效果，则也可以包含例如粘合剂成分、表面张力调节剂、消泡剂、粘度调节剂等其他成分。其他成分的比例优选其总量相对于金属粉100质量份为0.1质量份以上且10质量份以下。
具有这样的接合部的接合体有效利用其高接合强度、导热性的特性，适合用于暴露于高温的环境、例如安装有车载用电子电路、功率器件的电子电路。
实施例
以下，通过实施例对本发明进行更详细的说明。然而，本发明的范围并不限定于该实施例。除非另有说明，“％”和“份”分别是指“质量％”和“质量份”。
〔实施例1〕
(1)接合用组合物的制备
作为铜粉，使用DSEM50为0.14μm的球状铜粉与D50为4.9μm且径厚比(主面的长度相对于颗粒的厚度之比)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为球状铜粉70质量％：薄片状铜粉30质量％。
作为还原剂，以相对于铜粉100份为2.5份的比例使用双(2-羟基乙基)亚氨基三(羟基甲基)甲烷。
作为液体介质，使用聚乙二醇300(相对于铜粉100份为1份)与己二醇(相对于铜粉100份为31.6份)的混合物。
将上述铜粉、还原剂以及液体介质混合，得到糊剂状的接合用组合物。
剪切速度10s-1下的接合用组合物的粘度在25℃下为34Pa·s。
(2)接合结构体的制造
作为第2被接合件，在20mm见方的俯视正方形的铜板(厚度1mm)的中央，通过丝网印刷涂布接合用组合物而形成涂膜。涂膜使用厚度100μm的金属掩模，在包含铜板的中央部的区域形成为6mm见方的正方形。将该涂膜在热风干燥机中，在110℃下干燥10分钟，去除一部分液体介质，放置在室温下，得到干燥涂膜。另外，确认干燥涂膜中的液体介质的含量，结果为5质量％以下。
接下来，作为第1被接合件，将在表面整个区域具有通过Ag金属化而形成的银层的4.9mm见方的俯视正方形的半导体元件(SiC芯片，厚度0.38mm，Wolfspeed公司制，CPW5-1200-Z050B)载置于干燥涂膜上，制成层叠体。在该状态下沿厚度方向施加20MPa的压力，在氮气氛下，以升温速度960℃/分钟从40℃升温至280℃，之后，在280℃下进行5分钟焙烧，制作具有图1的(a)和(b)所示的结构的接合结构体。该接合结构体的各被接合件和接合部在俯视整个区域中相邻地形成。另外，作为干燥涂膜的烧结体的接合部通过基于TOF-SIMS的质谱分析确认到形成了由所述结构(1)表示的化学结构。
〔实施例2〕
在接合结构体的制造中，将烧结时的压力赋予变更为10MPa，除此以外，通过与实施例1同样的方法，得到具有图1的(a)和(b)所示的结构的接合结构体。接合部通过基于TOF-SIMS的质谱分析确认到形成了由所述结构(1)表示的化学结构。
〔比较例1〕
在接合结构体的制造中，将烧结时的压力赋予变更为6MPa，除此以外，通过与实施例1同样的方法得到接合结构体。接合部通过基于TOF-SIMS的质谱分析确认到形成了由所述结构(1)表示的化学结构。
〔接合比例的测定〕
对于实施例和比较例的接合结构体，使用株式会社Systemin Frontier制的软件Measurement Adviser，通过上述方法分别测定和计算被接合件与接合部的界面处的各接合比例Rc、Rs以及它们的比Rs/Rc。将其结果与测定视野的总长Lt一起示于以下的表1。
需要说明的是，为了便于说明，在以下的表中，仅示出了SiC芯片(第1被接合件11)与接合部15之间的接合比例。
〔接合可靠性的评价〕
对于接合结构体，进行10个循环的冷热循环试验(TCT)，使用超声波探伤装置(日立Power Solutions公司制，型号：FineSAT III)，利用75MHz的探头通过反射法，从铜板的背面侧观察此时从烧结体剥离的状态。在TCT中，将(1)-40℃·15分钟、(2)+125℃·15分钟作为1个循环。
在观察接合层的剥离状态时，将增益的值设为25dB～35dB的值后，调节S栅极的延迟和宽度以使S栅极的峰值位置成为铜板的表面。为了指定接合层的观察范围，调整F栅极的延迟，将宽度设定为1.5波长量的峰值宽度。调整探头的Z轴坐标以使观察峰的振幅最大，进行观察。观察像的对比度使用自动功能进行调节。
在上述装置中，接合状态良好的被观察到颜色深(黑色)，产生裂纹、剥离而接合状态差的区域被观察到颜色浅(白色)。其中，将实施例1和比较例1的TCT前后的图像数据示于图3和图4。
另外，使用图像处理软件Image-J对得到的图像数据进行二值化，计算所观察的面积中的黑色的面积比例(TCT10个循环后的接合率；％)。即，启动Image-J后，选择Analyze-Set measurement，检查Area、Area fraction、Limit to Threshold。之后，选择File-Open，打开计算接合率的图像数据后，指定图像中的SiC芯片搭载部的范围(A)。接下来，选择Edit-Copy to system，复制指定的范围(A)后，选择File-New-System clipboard，粘贴指定的范围(A)的图像。之后，为了明确接合部，选择Image-Type-8bit，对图像进行变换后，选择Image-Adjust-Threshold，将图像的阈值调整为110。然后，指定存在于调整后的图像中的SiC芯片搭载部的范围(A)内的红色范围(B)。所述红色范围(B)为SiC芯片接合部，其接合率由(B)/(A)×100计算。接合率越高，表示即使在发生了过度的温度变化的情况下接合可靠性也越高。将结果示于表1。
[表1]
产业上的可利用性
根据本发明，提供一种具有高接合可靠性的接合结构体。

Claims (3)

1.一种接合结构体，其是2个被接合件与在这些被接合件之间相邻地形成的接合部接合而成的，
所述接合部由以铜为主体的材料构成，
在所述接合结构体的厚度方向剖视中，该接合结构体的端部区域处的所述被接合件与所述接合部的接合比例Rs相对于该接合结构体的中央区域处的所述被接合件与所述接合部的接合比例Rc之比(Rs/Rc)为0.6以上0.9以下，
所述接合比例Rc为0.3以上。
2.根据权利要求1所述的接合结构体，其中，所述被接合件中的至少一者在其表面具有金、银、铜、镍以及钛中的至少一种金属。
3.根据权利要求1或2所述的接合结构体，其中，在所述接合部形成有由以下的式(1)所示的结构：
式(1)中，R3至R5分别独立地表示氢原子、羟基、碳原子数1以上且10以下的烃基、或者具有羟基的碳原子数1以上且10以下的烃基，
*表示与铜的键合部位。
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