CN113166945B - 接合体及半导体装置的制造方法 - Google Patents

接合体及半导体装置的制造方法 Download PDF

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Publication number
CN113166945B
CN113166945B CN201880099778.9A CN201880099778A CN113166945B CN 113166945 B CN113166945 B CN 113166945B CN 201880099778 A CN201880099778 A CN 201880099778A CN 113166945 B CN113166945 B CN 113166945B
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particles
copper
bonding
mass
copper paste
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CN113166945A (zh
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川名祐贵
中子伟夫
根岸征央
须镰千绘
江尻芳则
谷中勇一
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Lishennoco Co ltd
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Lishennoco Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/492—Bases or plates or solder therefor
    • H01L23/4924—Bases or plates or solder therefor characterised by the materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
    • B23K20/023—Thermo-compression bonding
    • B23K20/026—Thermo-compression bonding with diffusion of soldering material
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    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/16—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating with interposition of special material to facilitate connection of the parts, e.g. material for absorbing or producing gas
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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
    • B23K20/233—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded without ferrous layer
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    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries
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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/302—Cu as the principal constituent
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C20/00—Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
    • C23C20/02—Coating with metallic material
    • C23C20/04—Coating with metallic material with metals
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    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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Abstract

本发明涉及一种接合体及半导体装置的制造方法以及接合用铜糊。本发明的一形态提供一种接合体的制造方法，包括：准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及将接合用铜糊在受到0.1MPa～1MPa的压力的状态下予以烧结的步骤，其中，接合用铜糊含有金属粒子及分散介质，金属粒子的含量以接合用铜糊的总质量为基准，为50质量％以上，金属粒子含有以所述金属粒子的总质量为基准，为95质量％以上的次微米铜粒子。

Description

接合体及半导体装置的制造方法
技术领域
本发明涉及一种接合体及半导体装置的制造方法以及接合用铜糊。
背景技术
在制造半导体装置时，为了使半导体元件与引线框架等(支撑构件)接合而使用了各种各样的接合材。半导体装置中，在以150℃以上的高温进行运行的功率半导体、大规模集成电路(Large Scale Integration，LSI)等的接合中，一直使用高熔点铅焊料作为接合材。近年来，因半导体元件的高容量化及省空间化，运行温度上升至高熔点铅焊料的熔点附近，而变得难以确保连接可靠性。另一方面，伴随着危害性物质限制指令(Restriction ofHazardous Substances，RoHS)管制强化，正在寻求一种不含铅的接合材。
迄今为止仍在研究使用铅焊料以外的材料的半导体元件的接合。例如，下述专利文献1中提出有使银纳米粒子低温烧结而形成烧结银层的技术。已知此种烧结银对于功率循环的连接可靠性高。(非专利文献1)
进而，作为其他材料，也提出有使铜粒子烧结而形成烧结铜层的技术。例如，下述专利文献2中，作为用以将半导体元件与电极接合的接合材而公开有包含氧化铜粒子及还原剂的接合用糊。另外，下述专利文献3中公开有包含铜纳米粒子、以及铜微米粒子或铜次微米粒子、或者这些两者的接合材。
[现有技术文献]
[专利文献]
专利文献1：日本专利第4928639号
专利文献2：日本专利第5006081号
专利文献3：日本专利特开2014-167145号公报
[非专利文献]
非专利文献1：R.卡贺扎卡(Khazaka),L.蒙迪扎巴尔(Mendizabal),D.亨利(Henry)：电子材料期刊(J.ElecTron.Mater),43(7),2014,2459-2466
发明内容
[发明所要解决的问题]
所述专利文献1中记载的方法为了获得高的连接可靠性而必须使烧结银层致密化，因此需要进行伴随加压的热压接工艺。在所述专利文献1中，是以5MPa进行加压，所以需要通过热加压装置进行加压，而在进行此种热压接工艺的情况下，存在生产效率下降、良率下降等课题。进而，在使用银纳米粒子的情况下，银所造成的材料成本的显著增加等成为问题。
所述专利文献2中记载的方法通过热压接工艺而避免了自氧化铜还原为铜时的体积收缩。通过热压接工艺，能够避免自氧化铜还原为铜时的厚度方向的体积收缩，但由于氧化铜粒子本身会在向铜还原时进行体积收缩，因此难以抑制面方向的体积收缩，而包含烧结铜层的接合层内部的龟裂可能成为问题。
所述专利文献3中记载的方法是在不加压的状态下进行烧结，但就以下方面而言对于供至实际应用尚不充分。即，对于铜纳米粒子，为了抑制氧化及提高分散性而需要利用保护剂对表面进行修饰，但由于铜纳米粒子的比表面积大，因此存在如下倾向：在以铜纳米粒子为主成分的接合材中表面保护剂的调配量增加。另外，为了确保分散性而存在分散介质的调配量增加的倾向。因此，为了保管或涂敷等的供给稳定性，所述专利文献3中记载的接合材加大了表面保护剂或分散介质的比例。由此，烧结时的体积收缩容易变大，而且存在烧结后的致密度容易下降的倾向，而难以确保烧结体强度。
本发明以提供一种不需要在高压下的接合，却可获得接合强度优异的接合体的接合体的制造方法及半导体装置的制造方法为目的。本发明进而也以提供一种适合于所述制造方法且涂布性优异的接合用铜糊为目的。
[解决问题的技术手段]
本发明提供一种接合体的制造方法，包括：准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及将接合用铜糊在受到0.1MPa～1MPa的压力的状态下予以烧结的步骤，其中，接合用铜糊含有金属粒子及分散介质，金属粒子的含量以接合用铜糊的总质量为基准，为50质量％以上，金属粒子含有以金属粒子的总质量为基准，为95质量％以上的次微米铜粒子。
本发明也提供一种半导体装置的制造方法，包括：准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及将接合用铜糊在受到0.1MPa～1MPa的压力的状态下予以烧结的步骤，其中，第一构件及第二构件中的至少一者为半导体元件，接合用铜糊含有金属粒子及分散介质，金属粒子的含量以接合用铜糊的总质量为基准，为50质量％以上，金属粒子含有以金属粒子的总质量为基准，为95质量％以上的次微米铜粒子。
根据本发明的接合体的制造方法及半导体装置的制造方法，尽管不需要通过使用特别的热加压装置等进行的高压下的接合，仍可获得接合强度优异的接合体及半导体装置。作为可获得此种效果的原因，可列举：通过在接合用铜糊中使用次微米铜粒子，可充分抑制由次微米铜粒子的表面保护剂和/或接合用铜糊的分散介质引起的烧结时的体积收缩。认为：由于烧结时的体积收缩被抑制，因此能够将接合用铜糊在高温下烧结，结果达成烧结体强度的确保及与被接着面的接合力提升。另外，根据此制造方法，与使用以高价的铜纳米粒子为主成分的接合材的情况相比，可更廉价且稳定地制造接合体及半导体装置。由此，能够进一步提高生产稳定性。
另外，通过本发明的制造方法制造的接合体通过具备导热系数优异的铜的烧结体而可成为构件的散热性也优异的接合体。
进而，通过本发明的制造方法而获得的半导体装置通过具备具有充分的接合力、导热系数及熔点高的铜的烧结体，可成为具有充分的裸片剪切强度、连接可靠性优异、并且功率循环耐性也优异的半导体装置。
本发明也提供一种接合用铜糊，其含有金属粒子及分散介质，金属粒子的含量以接合用铜糊的总质量为基准，为50质量％以上，金属粒子含有以金属粒子的总量为基准，为95质量％以上的次微米铜粒子。
所述接合用铜糊不易发生烧结时的体积收缩，因此即便不进行高压下的加压，也可制造接合强度优异的接合体。
金属粒子也可含有以金属粒子的总质量为基准，为5质量％以下的微米铜粒子。
接合用铜糊中，接合用铜糊的25℃下的粘度可为0.8Pa·s～40000Pa·s。由此，能够获得容易通过涂布进行制造，且强度优异的接合体或半导体装置。
接合用铜糊中，分散介质可为选自由醇类及醚类所组成的群组中的至少一种。由此，可使接合用铜糊的涂布性更优异。
接合用铜糊中，次微米铜粒子的纵横尺寸比可为5以下。由此，抑制在加压步骤时次微米粒子沿不均匀的方向排列，从而可抑制在接合体中出现孔隙(void)。
[发明的效果]
根据本发明，可提供一种不需要在高压下的接合，却可获得接合强度优异的接合体的接合体的制造方法及半导体装置的制造方法。根据本发明，进而可提供一种适合于所述制造方法且涂布性优异的接合用铜糊。
附图说明
图1是表示一实施形态的接合体的制造方法的示意剖面图。
图2是表示一实施形态的半导体装置的制造方法的示意剖面图。
图3是实施例1的接合体的剖面的扫描式电子显微镜(scanning electronmicroscope，SEM)图像。
图4是实施例2的接合体的剖面的SEM图像。
图5是比较例3的接合体的剖面的SEM图像。
[符号的说明]
1：接合用铜糊
2：第一构件
3：第二构件
4：层叠体
23：半导体元件
100：接合体
200：半导体装置
具体实施方式
以下，适当参照图式对用以实施本发明的形态(以下，称为“本实施形态”)进行详细说明。本发明并不限定于以下的实施形态。
＜接合体的制造方法＞
图1是表示一实施形态的接合体的制造方法的示意剖面图。一实施形态的接合体的制造方法包括：准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤(准备步骤)；以及将接合用铜糊在受到0.1MPa～1MPa的压力的状态下予以烧结的步骤(烧结步骤)。
[准备步骤]
在一实施形态中，准备步骤也可为制作层叠体的步骤。在准备步骤中，首先，如图1的(a)中所示，准备第一构件2、及第二构件3。
(第一构件及第二构件)
作为第一构件2及第二构件3，例如可列举：绝缘闸双极晶体管(Insulated GateBipolar Transistor，IGBT)、二极管、肖特基能障二极管(Schottky-barrier diode)、金属-氧化物半导体场效晶体管(Metal-Oxide-Semiconductor Field-Effect Transistor，MOS-FET)、晶闸管、逻辑电路、传感器、模拟集成电路、发光二极管(Light-Emitting Diode，LED)、半导体激光器、发信器等半导体元件；引线框架、贴附有金属板的陶瓷基板(例如直接覆铜板(direct bonded copper，DBC))、LED封装体等半导体元件搭载用基材；铜带、金属块、端子等供电用构件；散热板；水冷板等。
第一构件2及第二构件3也可在后述与接合用铜糊相接的面2a、3a中包含金属。作为金属，例如可列举：铜、镍、银、金、钯、铂、铅、锡、钴等。金属可单独使用一种，也可将两种以上组合使用。另外，与接合用铜糊相接的面2a、3a也可为包含所述金属的合金。作为合金中所使用的金属，除了所述金属以外，也可列举：锌、锰、铝、铍、钛、铬、铁、钼等。作为在与烧结体相接的面包含金属的构件，例如可列举：具有各种金属镀层的构件、导线(wire)、具有金属镀层的芯片、散热片(heat spreader)、贴附有金属板的陶瓷基板、具有各种金属镀层的引线框架或包含各种金属的引线框架、铜板、铜箔。
其次，如图1的(b)中所示，在第一构件2与第二构件3之间配置接合用铜糊1，制作如图1的(c)中所示那样的依次层叠有第一构件2、接合用铜糊1及第二构件3的层叠体4。关于接合用铜糊1的详细情况将后述。
为了制作层叠体4，例如如图1的(b)中所示，在第二构件3的必要部分设置接合用铜糊1，继而在接合用铜糊1上配置第一构件2。制作层叠体4的方法并不限于图1的(b)中所示的方法，也可在第一构件2的必要部分设置接合用铜糊1，并将设置有接合用铜糊1的第一构件2配置于第二构件3上。
作为将接合用铜糊1设置于第二构件3或第一构件2的必要部分的方法，只要是可堆积接合用铜糊的方法即可。作为此种方法，例如可使用：丝网印刷、转印印刷、胶版印刷、喷射印刷法、分配器、喷射分配器、针形分配器(needledispenser)、缺角轮涂布机、狭缝涂布机、模涂机、凹版涂布机(gravure coater)、狭缝涂布、凸版印刷、凹版印刷、凹版印刷(gravure printing)、模版印刷(stencil printing)、软光刻(soft lithograph)、棒涂、敷料器(applicator)、粒子堆积法、喷雾涂布机、旋转涂布机、浸渍涂布机、电着涂装等。
接合用铜糊1的厚度可为1μm以上且1000μm以下，可为10μm以上且500μm以下，可为50μm以上且200μm以下，可为10μm以上且3000μm以下，可为15μm以上且500μm以下，可为20μm以上且300μm以下，可为5μm以上且500μm以下，可为10μm以上且250μm以下，也可为15μm以上且150μm以下。
将第一构件2配置于接合用铜糊1上的方法、或将设置有接合用铜糊1的第一构件2配置于第二构件3上的方法例如可使用芯片安装器(chip mounter)、倒装芯片结合器(flipchip bonder)、碳制或陶瓷制的定位夹具等。
(接合用铜糊)
接合用铜糊1含有金属粒子及分散介质。
金属粒子含有以金属粒子的总质量为基准，为95质量％以上的次微米铜粒子。次微米铜粒子具有良好的烧结性，因此可减低在主要使用铜纳米粒子的接合材中出现的高昂的合成成本、并不良好的分散性、烧结后的体积收缩的下降等课题。
在本说明书中，次微米铜粒子是体积平均粒径为0.12μm以上且0.8μm以下的铜粒子。
再者，本说明书中，所谓体积平均粒径是指50％体积平均粒径。在求铜粒子的体积平均粒径的情况下，可通过如下方法等来求出：利用光散射法粒度分布测定装置(例如，纳米粒子径分布测定装置(SALD-7500纳米(nano)，岛津制作所股份有限公司制造))，对使用分散剂将成为原料的铜粒子、或自接合用铜糊中去除了挥发成分而成的干燥铜粒子分散于分散介质中而成者进行测定。在使用光散射法粒度分布测定装置的情况下，作为分散介质，可使用己烷、甲苯、α-萜品醇、纯水等。
关于次微米铜粒子的体积平均粒径，就获得次微米铜粒子的合成成本的抑制、良好的分散性、表面处理剂的使用量的抑制等效果的观点而言，优选为0.15μm以上，更优选为0.2μm以上，特别优选为0.3μm以上，就提高次微米铜粒子的烧结性的观点而言，优选为0.6μm以下，更优选为0.5μm以下，进而优选为0.45μm以下。
次微米铜粒子的平均二次粒径可为0.12μm以上或0.15μm以上，也可为0.8μm以下。本说明书中的次微米铜粒子的平均二次粒径是最大粒径，例如可通过利用扫描式电子显微镜(SEM)对次微米铜粒子、或者自接合用铜糊1中去除了挥发成分而成的干燥铜粒子进行观察的方法求出。
在次微米铜粒子的形状不是球状的情况下，可通过以下的方法求出平均二次粒径(最大粒径)。即，利用刮勺(spatula)将铜粒子的粉末载置于SEM用的碳胶带上，制成SEM用样品。利用SEM装置以10000倍来观察此SEM用样品。利用图像处理软件对外接于此SEM图像的铜粒子的长方形进行绘图，将长方形的长边设为所述粒子的长径。将此长径设为最大粒径。
次微米铜粒子的形状并无特别限定。作为次微米铜粒子的形状，例如可列举：球状、块状、针状、薄片状、大致球状及这些的凝聚体。就分散性及填充性的观点而言，次微米铜粒子的形状可为球状、大致球状、薄片状。就抑制烧结接合用铜糊时发生孔隙的观点而言，次微米铜粒子优选为球状或大致球状。在本说明书中，所谓“薄片状”，包含板状、鳞片状等平板状的形状。
就分散性、填充性的观点及抑制烧结后的孔隙的观点而言，次微米铜粒子的纵横尺寸比优选为5以下。就同样的观点而言，次微米铜粒子的纵横尺寸比更优选为3以下，进而优选为1.5以下。本说明书中，所谓“纵横尺寸比”表示粒子的长边/厚度。粒子的长边及厚度的测定例如可根据次微米铜粒子的SEM图像求出。
次微米铜粒子可经特定的表面处理剂处理。作为表面处理剂，例如可列举碳数8～16的有机酸。作为碳数8～16的有机酸，例如可列举：辛酸、甲基庚酸、乙基己酸、丙基戊酸、壬酸、甲基辛酸、乙基庚酸、丙基己酸、癸酸、甲基壬酸、乙基辛酸、丙基庚酸、丁基己酸、十一酸、甲基癸酸、乙基壬酸、丙基辛酸、丁基庚酸、月桂酸、甲基十一酸、乙基癸酸、丙基壬酸、丁基辛酸、戊基庚酸、十三酸、甲基十二酸、乙基十一酸、丙基癸酸、丁基壬酸、戊基辛酸、肉豆蔻酸、甲基十三酸、乙基十二酸、丙基十一酸、丁基癸酸、戊基壬酸、己基辛酸、十五酸、甲基十四酸、乙基十三酸、丙基十二酸、丁基十一酸、戊基癸酸、己基壬酸、棕榈酸、甲基十五酸、乙基十四酸、丙基十三酸、丁基十二酸、戊基十一酸、己基癸酸、庚基壬酸、甲基环己烷羧酸、乙基环己烷羧酸、丙基环己烷羧酸、丁基环己烷羧酸、戊基环己烷羧酸、己基环己烷羧酸、庚基环己烷羧酸、辛基环己烷羧酸、壬基环己烷羧酸等饱和脂肪酸；辛烯酸、壬烯酸、甲基壬烯酸、癸烯酸、十一碳烯酸、十二碳烯酸、十三碳烯酸、十四碳烯酸、肉豆蔻油酸、十五碳烯酸、十六碳烯酸、棕榈油酸、十六碳-6-烯酸(sapienic acid)等不饱和脂肪酸；对苯二甲酸、均苯四甲酸、邻苯氧基苯甲酸、甲基苯甲酸、乙基苯甲酸、丙基苯甲酸、丁基苯甲酸、戊基苯甲酸、己基苯甲酸、庚基苯甲酸、辛基苯甲酸、壬基苯甲酸等芳香族羧酸。有机酸可单独使用一种，也可将两种以上组合使用。通过将此种有机酸与所述次微米铜粒子加以组合，而存在可兼具次微米铜粒子的分散性与烧结时的有机酸的脱离性的倾向。
表面处理剂的处理量可为在次微米铜粒子的表面附着一分子层～三分子层的量。此量可根据附着于次微米铜粒子的表面的分子层数(n)、次微米铜粒子的比表面积(Ap)(单位m2/g)、表面处理剂的分子量(Ms)(单位g/mol)、表面处理剂的最小被覆面积(SS)(单位m2/个)、以及亚佛加厥数(NA)(6.02×1023个)而算出。具体而言，表面处理剂的处理量可依据表面处理剂的处理量(质量％)＝{(n·Ap·Ms)/(SS·NA+n·Ap·Ms)}×100％的式子而算出。
次微米铜粒子的比表面积可通过利用布厄特(Brunauer,Emmett and Teller，BET)比表面积测定法对经干燥的次微米铜粒子进行测定来算出。在表面处理剂为直链饱和脂肪酸的情况下，表面处理剂的最小被覆面积为2.05×10-19m2/1分子。在为除此以外的表面处理剂的情况下，例如可通过根据分子模型的计算、或《化学与教育》(上江田捷博、稻福纯夫、森严，40(2)，1992，p114-117)中记载的方法来测定。示出表面处理剂的定量方法的一例。表面处理剂可通过自接合用铜糊中去除了分散介质的干燥粉的热脱附气体·气相层析质量分析计来鉴定，由此可决定表面处理剂的碳数及分子量。表面处理剂的碳量比例可通过碳量分析来进行分析。作为碳量分析法，例如可列举高频感应加热炉燃烧/红外线吸收法。可根据经鉴定的表面处理剂的碳数、分子量及碳量比例并通过所述式来算出表面处理剂量。
表面处理剂的所述处理量可为0.07质量％以上且2.1质量％以下，也可为0.10质量％以上且1.6质量％以下，也可为0.2质量％以上且1.1质量％以下。
在次微米铜粒子由表面处理剂进行了处理的情况下，与使用未经表面处理的铜粒子(例如氧化铜(CuO)、氧化亚铜(Cu2O))相比，烧结时的体积收缩得到抑制，从而能够进一步提高接合强度。这是由于由分散介质、及氧化铜的还原引起的烧结时的体积收缩被抑制。次微米铜粒子中所含的碳量为0.5质量％～1质量％左右，烧结时的体积收缩变少，因此即便出现了由表面处理剂引起的烧结时的体积收缩，也容易确保接合体的接合强度。
作为本实施形态的次微米铜粒子，可使用市售品。作为市售的次微米粒子，例如可列举：CH-0200(三井金属矿业股份有限公司制造，体积平均粒径0.36μm)、HT-14(三井金属矿业股份有限公司制造，体积平均粒径0.41μm)、CT-500(三井金属矿业股份有限公司制造，体积平均粒径0.72μm)、Tn-Cu100(太阳日产股份有限公司制造，体积平均粒径0.12μm)。
就即便不进行高压下的接合，也容易获得接合强度优异的接合体的观点、及接合用铜糊的涂布性更优异的观点而言，次微米铜粒子的含量以金属粒子的总质量为基准，为95质量％以上。就同样的观点而言，次微米铜粒子的含量以金属粒子的总质量为基准，可为96质量％以上、98质量％以上、或99质量％以上，也可为100质量％。特别是，在将接合用铜糊用于半导体元件的接合的情况下，若次微米铜粒子的含量为所述范围内，则存在半导体装置显示出良好的裸片剪切强度及连接可靠性的倾向。
就即便不进行高压下的接合，也容易获得接合强度优异的接合体的观点、及接合用铜糊的涂布性更优异的观点而言，次微米铜粒子的含量以接合用铜糊总量为基准，优选为40质量％以上，更优选为50质量％以上，进而优选为70质量％以上，而且，优选为95质量％以下，更优选为92质量％以下，进而优选为80质量％以下。
金属粒子除了次微米铜粒子以外，也可进而含有微米铜粒子。在本说明书中，微米铜粒子是体积平均粒径为2μm以上且50μm以下的铜粒子。体积平均粒径的测定方法与所述次微米铜粒子的测定方法相同。
就即便不进行高压下的接合，也容易获得接合强度优异的接合体的观点、及接合用铜糊的涂布性更优异的观点而言，微米铜粒子的含量以金属粒子的总质量为基准，优选为5质量％以下，更优选为3质量％以下，进而优选为1质量％以下。金属粒子也可不含有微米铜粒子。
金属粒子也可包含所述铜粒子以外的其他金属粒子，例如也可包含锌、镍、银、金、钯、铂等的粒子。其他金属粒子的体积平均粒径可为0.01μm以上且10μm以下，也可为0.01μm以上且5μm以下，也可为0.05μm以上且3μm以下。在包含其他金属粒子的情况下，就获得充分的接合性的观点而言，其他金属粒子的含量以金属粒子的总质量为基准，可为5质量％以下、3质量％以下、或1质量％以下。也可不含其他金属粒子。其他金属粒子的形状并无特别限定。
通过包含铜粒子以外的金属粒子，可获得固溶或分散有多种金属的烧结体，因此烧结体的降伏应力、疲劳强度等机械特性得到改善，从而容易提高连接可靠性。另外，通过添加多种金属粒子，可使接合用铜糊1的烧结体对于特定的被接着体具有充分的接合强度。在将接合用铜糊1用于半导体元件的接合的情况下，容易提高半导体装置的裸片剪切强度及连接可靠性。
就即便不进行高压下的接合，也容易获得接合强度优异的接合体的观点、及接合用铜糊的涂布性更优异的观点而言，金属粒子的含量以接合用铜糊的总质量为基准，为50质量％以上。关于金属粒子的含量，就同样的观点而言，以接合用铜糊的总质量为基准，优选为60质量％以上，更优选为65质量％以上，进而优选为70质量％以上，就接合用铜糊的涂布性更优异的观点而言，优选为95质量％以下，更优选为90质量％以下，进而优选为85质量％以下，特别优选为80质量％以下。
分散介质并无特别限定，可为挥发性的分散介质。作为挥发性的分散介质，例如可列举：戊醇、己醇、庚醇、辛醇、癸醇、乙二醇、二乙二醇、丙二醇、丁二醇、α-萜品醇、异冰片基环己醇(MTPH)等醇类(一元及多元醇类)；乙二醇丁醚、乙二醇苯醚、二乙二醇甲醚、二乙二醇***、二乙二醇单丁醚、二乙二醇单异丁醚、二乙二醇己醚、三乙二醇甲醚、二乙二醇二甲醚、二乙二醇二***、二乙二醇二丁醚、二乙二醇丁基甲基醚、二乙二醇异丙基甲基醚、三乙二醇二甲醚、三乙二醇丁基甲基醚、丙二醇丙醚、二丙二醇甲醚、二丙二醇***、二丙二醇丙醚、二丙二醇丁醚、二丙二醇二甲醚、三丙二醇甲醚、三丙二醇二甲醚等醚类；乙二醇***乙酸酯、乙二醇丁醚乙酸酯、二乙二醇***乙酸酯、二乙二醇丁醚乙酸酯、二丙二醇甲醚乙酸酯(dipropylene glycol methyl ether acetate，DPMA)、乳酸乙酯、乳酸丁酯、γ-丁内酯、碳酸亚丙酯等酯类；N-甲基-2-吡咯烷酮、N,N-二甲基乙酰胺、N,N-二甲基甲酰胺等酸酰胺；环己酮、辛烷、壬烷、癸烷、十一烷等脂肪族烃；苯、甲苯、二甲苯等芳香族烃；具有碳数1～18的烷基的硫醇类；具有碳数5～7的环烷基的硫醇类。作为具有碳数1～18的烷基的硫醇类，例如可列举：乙基硫醇、正丙基硫醇、异丙基硫醇、正丁基硫醇、异丁基硫醇、叔丁基硫醇、戊基硫醇、己基硫醇及十二烷基硫醇。作为具有碳数5～7的环烷基的硫醇类，例如可列举：环戊基硫醇、环己基硫醇及环庚基硫醇。分散介质可将这些单独使用一种或组合两种以上来使用。
就进一步提高接合用铜糊1的涂布性的观点而言，分散介质优选为选自由醇类及醚类所组成的群组中的至少一种，更优选为选自由二乙二醇单丁醚、或α-萜品醇、MTPH及环己酮所组成的群组中的至少一种。分散介质也可为二乙二醇单丁醚与α-萜品醇的混合物或α-萜品醇与MTPH的混合物。
分散介质的含量相对于金属粒子100质量份可为5质量份～50质量份。若分散介质的含量为所述范围内，则可将接合用铜糊1调整为更适当的粘度，而且可使得难以阻碍铜粒子的烧结。
就进一步提高接合用铜糊1的涂布性的观点而言，分散介质的含量以接合用铜糊的总质量为基准，优选为5质量％以上，更优选为10质量％以上，进而优选为20质量％以上，而且，优选为70质量％以下，更优选为50质量％以下，进而优选为30质量％以下。
接合用铜糊1中除了金属粒子及分散介质以外，也可视需要适当添加非离子系表面活性剂、氟系表面活性剂等湿润性提升剂；硅酮油等消泡剂；无机离子交换体等离子捕捉剂等。也可添加所述表面处理剂作为添加剂。
关于接合用铜糊1的25℃下的粘度，就接合体100的接合强度更优异的观点而言，优选为0.8Pa·s以上，更优选为10Pa·s以上，进而优选为100Pa·s以上，特别优选为200Pa·s以上，就进一步提高接合用铜糊1的涂布性的观点而言，优选为40000Pa·s以下，更优选为30000Pa·s以下，进而优选为10000Pa·s以下，特别优选为1000Pa·s以下。粘度是指卡森(Casson)粘度，可使用粘弹性测定装置进行测定。接合用铜糊的粘度可通过调整金属粒子及分散介质的含量或适当选择分散介质的种类来进行调整。
所述接合用铜糊1例如可将所述次微米铜粒子与视需要的其他材料混合至分散介质中来进行制备。在各成分混合后的分散液中，也可进行搅拌处理。在接合用铜糊1中，也可通过分级操作来调整分散液的最大粒径。此时，分散液的最大粒径可设为10μm以下，也可设为5μm以下。
在接合用铜糊1含有次微米铜粒子以外的金属粒子的情况下，也可将次微米铜粒子及分散介质预先混合，进行分散处理而制备分散液，进而混合其他金属粒子及任意的添加剂来进行制备。通过设为此种顺序，其他金属粒子与任意的添加剂的混合性变优选，从而进一步提高接合用铜糊的性能。对于次微米铜粒子的分散液，也可通过分级操作来将凝聚物去除。
作为分散处理，例如可列举使用了薄层剪切分散机、珠磨机、超声波均质机、高剪切混合机(high shear mixer)、狭缝三辊研磨机、湿式超微粒化装置、超音速式喷射磨机、超高压均质机、分散器(Disperizer)的处理。
搅拌处理可使用搅拌机来进行。作为搅拌机，例如可列举：自转公转型搅拌装置、擂溃机、双轴混炼机、三辊研磨机、行星式搅拌机(planetary mixer)、薄层剪切分散机。另外，搅拌处理也可使用研钵利用人力来进行搅拌处理。也可在其后进而使用所述搅拌机进行搅拌处理。
分级操作例如可使用过滤、自然沉降、离心分离来进行。作为过滤用的过滤器，例如可列举：金属网、金属过滤器、尼龙网。
就抑制烧结时的流动及孔隙的产生的观点而言，也可对设于第二构件3上或第一构件2上的接合用铜糊1适当地进行干燥。干燥时的气体环境可为大气中，也可为氮气、惰性气体等无氧环境中，也可为氢气、甲酸等还原环境中。干燥方法可为常温放置下的干燥，也可为加热干燥，也可为减压干燥。加热干燥或减压干燥中例如可使用：热板、温风干燥机、温风加热炉、氮气干燥机、红外线干燥机、红外线加热炉、远红外线加热炉、微波加热装置、激光加热装置、电磁加热装置、加热器加热装置、蒸汽加热炉、热板压合装置等。干燥的温度及时间可根据所使用的分散介质的种类及量来适当地调整。作为干燥的温度及时间，例如可为50℃以上且180℃以下、1分钟以上且120分钟以下。
[烧结步骤]
继而，如图1的(d)中所示，将层叠体4中的接合用铜糊1在受到0.1MPa～1MPa的压力的状态下予以烧结。
在烧结步骤中，在将层叠体4沿层叠体4的层叠方向即图1的(d)中利用箭头表示的方向进行加压的同时进行加热。层叠体4的层叠方向也可称为第一构件2的自重的作用方向，也可称为重力的作用方向。
加压时的压力为0.1MPa～1MPa。由此，无需以高压进行加压，从而可进一步提高良率。另外，可减少接合体的孔隙，也可进一步提高裸片剪切强度。关于压力，就可减少接合体的孔隙，进一步提高裸片剪切强度的观点而言，优选为0.2MPa以上，更优选为0.3MPa以上，进而优选为0.4MPa以上，就进一步提高接合用铜糊的良率的观点而言，优选为0.8MPa以下，更优选为0.7MPa以下，进而优选为0.6MPa以下。
就减少对第一构件2及第二构件3的热损伤(thermal damage)及提高良率的观点而言，加热处理时的到达最高温度可为250℃以上且450℃以下，也可为250℃以上且400℃以下，也可为250℃以上且350℃以下。若到达最高温度为200℃以上，则存在如下倾向：在到达最高温度保持时间为60分钟以下的情况下烧结充分进行。
就使分散介质全部挥发、而且提高良率的观点而言，到达最高温度保持时间可为1分钟以上且120分钟以下，也可为1分钟以上且80分钟以下，也可为1分钟以上且60分钟以下。
层叠体4的加压及加热既可组合加热处理装置及加压处理装置来使用，也可使用加热加压处理装置。加热处理装置例如可使用：热板、温风干燥机、温风加热炉、氮气干燥机、红外线干燥机、红外线加热炉、远红外线加热炉、微波加热装置、激光加热装置、电磁加热装置、加热器加热装置、蒸汽加热炉、真空焊接装置、回流炉等。加压处理装置可使用碳制、金属制的加压夹具、重物、长尾夹(double clip)等。更具体而言，例如可使用重物作为加压处理装置，并组合批次式真空焊接装置(例如，神港精机股份有限公司制造)作为加热处理装置来使用。
作为加热加压处理装置，可使用热板压合装置(例如SIN200+(品库股份有限公司热***(PINK GmbH Thermosysteme)公司制造))、加热辊压机等。
就抑制接合用铜糊1的烧结体、第一构件及第二构件的氧化的观点而言，烧结时的气体环境可为无氧环境。就去除接合用铜糊的铜粒子的表面氧化物的观点而言，烧结时的气体环境可为还原环境。作为无氧环境，例如可列举：氮气、惰性气体等无氧气体的导入或真空下。作为还原环境，例如可列举：纯氢气中、以合成气体为代表的氢气及氮气的混合气体中、包含甲酸气体的氮气中、氢气及惰性气体的混合气体中、包含甲酸气体的惰性气体中等。
通过对接合用铜糊1进行烧结，可获得如图1的(e)中所示那样依次具备第一构件2、接合用铜糊的烧结体5及第二构件3的接合体100。即，一实施形态的接合体100包括：第一构件2、第二构件3、及将第一构件与第二构件接合的接合用铜糊的烧结体5。
就将第一构件及第二构件充分接合的观点而言，接合体的裸片剪切强度可为10MPa以上、15MPa以上、20MPa以上或30MPa以上。裸片剪切强度可使用万能型结合试验机(例如达格(DAGE)公司制造的4000系列)、通用结合试验机(universal bond tester)(例如，劳斯仪器(Royce Instruments)公司制造的劳斯(Royce)650)等来测定。
就散热性及高温下的连接可靠性优异的观点而言，接合用铜糊的烧结体的导热系数可为100W/(m·K)以上，也可为120W/(m·K)以上，也可为150W/(m·K)以上。导热系数可根据接合用铜糊的烧结体5的热扩散系数、比热容量及密度来算出。
[半导体装置的制造方法]
其次，对半导体装置的制造方法进行说明。在所述接合体100的制造方法中，第一构件及第二构件的至少一者为半导体元件的情况下，通过所述接合体的制造方法，可制造半导体装置。即，一实施形态的半导体装置的制造方法是在所述接合体的制造方法中，将第一构件和/或第二构件替换为半导体元件，所述半导体装置的制造方法包括：准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及将接合用铜糊在受到0.1MPa～1MPa的压力的状态下予以烧结的步骤，其中，第一构件及第二构件中的至少一者为半导体元件，接合用铜糊含有金属粒子及分散介质，金属粒子的含量以所述接合用铜糊的总质量为基准，为50质量％以上，金属粒子含有以所述金属粒子的总质量为基准，为95质量％以上的次微米铜粒子。
第一构件和/或第二构件中所使用的半导体元件例如可为：包含二极管、整流器、晶闸管、MOS栅极驱动器、功率开关、功率MOSFET、IGBT、肖特基二极管、快速回复二极管(fast recovery diode)等的功率模块；发信机；放大器；LED模块等。
图2是表示通过本实施形态的制造方法而获得的半导体装置的一例的示意剖面图。图2所示的半导体装置200具备：具有第一电极22及第二电极24的绝缘基板21、通过所述接合用铜糊的烧结体5而接合于第一电极22上的半导体元件23以及将半导体元件23与第二电极24电性连接的金属配线25。金属配线25与半导体元件23、以及金属配线25与第二电极24分别通过接合用铜糊的烧结体5而接合。另外，半导体元件23经由线27而连接于第三电极26。半导体装置200在绝缘基板21的搭载有所述电极等的面的相反侧具备铜板28。半导体装置200的所述结构体由绝缘体29密封。半导体装置200在第一电极22上具有一个半导体元件23，但也可具有两个以上。在此情况下，存在多个的半导体元件23可分别通过接合用铜糊的烧结体5而与金属配线25接合。
[实施例]
以下，通过实施例对本发明进一步进行具体说明。但是，本发明并不限定于以下的实施例。
＜接合用铜糊的制备＞
利用玛瑙研钵对作为分散介质的二乙二醇单丁醚(和光纯药工业股份有限公司制造)0.9g、与作为次微米铜粒子的CH-0200(三井金属矿业股份有限公司制造)9.1g进行混炼直至干燥粉消失为止，将所获得的混合液转移至塑料瓶中。使用自转公转型搅拌装置(行星式真空搅拌机(Planetary Vacuum Mixer)ARV-310，新基(Thinky)股份有限公司制造)以2000min-1(2000转/分钟)对塞紧的塑料瓶进行2分钟搅拌。将此混合液设为接合用铜糊1。
进而，变更为表1～表3中所示的组成，除此以外，通过与接合用铜糊1同样的方法制备接合用铜糊2～接合用铜糊17。
＜粘度的测定＞
使用粘弹性测定装置(MCR102，安东帕(Anton Paar)公司制造)测定接合用铜糊1～接合用铜糊17的25℃下的粘度。作为测定条件，设间隙为0.2mm、应变为2％、频率为0.5Hz。将自测定开始起5分钟后的接合用铜糊的粘度示于表1～表3。
＜接合体的制造＞
使用接合用铜糊1～接合用铜糊17并依据以下的方法来制造接合体。接合体的裸片剪切强度通过后述方法测定。
在19mm×25mm的铜板(厚度：3mm)上载置具有3mm×3mm正方形开口的不锈钢制的金属掩模(厚度：200μm)，通过使用金属刮刀的模版印刷来涂布接合用铜糊。将其在设定为90℃的热板上，在大气中，加热30分钟，载置3mm×3mm的被接着面依次溅射有钛(50nm)、镍(100nm)的硅芯片(厚度：400μm)，利用镊子(tweezers)轻轻按压。将此样本组装于批次式真空焊接炉(神港精机股份有限公司制造)，在以0.5MPa进行了加压的状态下，在氢气100％环境下进行30分钟的升温。升温后，以最高到达温度300℃、最高到达温度保持时间60分钟的条件进行烧结处理，从而获得将铜板与溅射镍的硅芯片接合而成的接合体。烧结后，在50℃以下将接合体取出至空气中。
＜评价方法＞
[裸片剪切强度]
接合体的接合强度通过裸片剪切强度来评价。针对制作的接合体，使用装配有测压仪(loadcell)(SMS-200K-24200，劳斯仪器(Royce Instruments)公司制造)的通用结合试验机(universal bond tester)(劳斯(Royce)650，劳斯仪器(Royce Instruments)公司制造)，以测定速度5mm/min、测定高度50μm将铜块朝水平方向按压，测定接合体的裸片剪切强度。将测定8个接合体所得的值的平均值设为裸片剪切强度。评价指标设为如下。若评价为S或A，则可谓裸片剪切强度优异。
评价指标：
S：30MPa以上
A：20MPa以上且不足30MPa
B：10MPa以上且不足20MPa
C：不足10MPa
[涂布性的评价]
使用具有10mm×10mm正方形开口的不锈钢制的金属掩模(厚度：200μm)，涂布接合用铜糊，由此对接合用铜糊的涂布性进行评价。评价指标设为如下。若评价为S或A，则可谓涂布性优异。
评价指标：
S：可不产生飞白地进行涂布，糊不会自开口部流出
A：稍微产生飞白，但糊不会自开口部溢出。或者虽可不产生飞白地进行涂布，但糊稍微自开口部流出。
B：产生飞白，但糊不会自开口部溢出。或者虽可不产生飞白地进行涂布，但糊自开口部流出。
C：明显产生飞白，但糊不会自开口部溢出。或者虽可不产生飞白地进行涂布，但糊明显自开口部流出。
[表1]
[表2]
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[表3]
[剖面形态观察]
利用样品夹持器(样品夹(Samplklip)I，标乐(Buehler)公司制造)将接合体固定于杯内，在周围流入环氧注型树脂(爱坡曼特(epomount)，立发科技(Refine Tec)股份有限公司制造)直至掩埋样品整体为止，在真空干燥器内静置，进行一分钟减压而加以脱泡。其后，在室温(25℃)下放置10小时而使环氧注型树脂硬化。使用装有金刚石切断轮(11-304，立发科技(Refine Tec)股份有限公司制造)的立发锯·罗(Refine Saw·Lo)(RCA-005，立发科技(Refine Tec)股份有限公司制造)在经注型的接合体的欲观察的剖面附近进行切断。利用装有耐水研磨纸(碳马克纸(carbon Mac paper)，立发科技(Refine Tec)股份有限公司制造)的研磨装置(立发抛光机(Refine Polisher)HV，立发科技(Refine Tec)股份有限公司制造)对剖面进行削切而在硅芯片露出不存在龟裂的剖面，进而削切多余的注型树脂并加工成可设置于截面抛光(Cross-section Polish，CP)加工机中的尺寸。利用CP加工机(IM4000，日立制作所股份有限公司制造)以加速电压6kV、氩气流量0.07cm3/min～0.1cm3/min、处理时间2小时的条件对经切削加工的样品进行截面抛光而进行剖面加工。使用溅射装置(离子溅射机(ION SPUTTER)，日立高新技术(Hitachi High-technologies)股份有限公司制造)对剖面以10nm的厚度溅射铂，从而制成SEM观察用的样品。利用SEM装置(ESEM XL30，飞利浦(Philips)公司制造)以施加电压10kV来观察所述SEM用样品的接合体的剖面。
图3表示实施例1的接合体的剖面的SEM图像，图4表示实施例2的接合体的剖面的SEM图像，图5表示比较例3的接合体的SEM图像。根据图3～图4可知：实施例1及实施例2中的接合用铜糊的烧结体5(5A、5B)可将镀镍的铜板31A、31B与溅射钛、镍的硅芯片32A、32B良好地接合。另一方面，根据图5可知，在比较例3的接合体中，在溅射钛、镍的硅芯片32C与接合用铜糊的烧结体5C之间的接合中存在不均。可认为：由于此种结构的不同，比较例3的接合体中未获得充分的裸片剪切强度。

Claims (10)

1.一种接合体的制造方法，包括：
准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及
在受到0.1MPa～1MPa的压力的状态下将所述接合用铜糊予以烧结的步骤，
所述接合用铜糊仅含有金属粒子及分散介质，
以所述接合用铜糊的总质量为基准，所述金属粒子的含量为70质量％以上，
以所述金属粒子的总质量为基准，所述金属粒子含有95质量％以上的次微米铜粒子，
所述分散介质包含二乙二醇单丁醚，
以所述接合用铜糊的总质量为基准，所述二乙二醇单丁醚的含量为10质量％以上且30质量％以下，
所述次微米铜粒子是体积平均粒径为0.12μm以上且0.8μm以下的铜粒子，
所述次微米铜粒子经表面处理剂进行了处理，所述表面处理剂为碳数8～16的有机酸，
进行烧结时的气体环境为无氧环境。
2.根据权利要求1所述的接合体的制造方法，其中以所述金属粒子的总质量为基准，所述金属粒子含有5质量％以下的微米铜粒子。
3.根据权利要求1或2所述的接合体的制造方法，其中所述接合用铜糊的25℃下的粘度为0.8Pa·s～40000Pa·s。
4.根据权利要求1或2所述的接合体的制造方法，其中所述金属粒子更包含锌粒子、镍粒子、银粒子、金粒子、钯粒子或铂粒子。
5.根据权利要求1或2所述的接合体的制造方法，其中所述次微米铜粒子的纵横尺寸比为5以下。
6.一种半导体装置的制造方法，包括：
准备依次层叠有第一构件、接合用铜糊及第二构件的层叠体的步骤；以及
在受到0.1MPa～1MPa的压力的状态下将所述接合用铜糊予以烧结的步骤，
所述第一构件及所述第二构件中的至少一者为半导体元件，
所述接合用铜糊仅含有金属粒子及分散介质，
以所述接合用铜糊的总质量为基准，所述金属粒子的含量为70质量％以上，
以所述金属粒子的总质量为基准，所述金属粒子含有95质量％以上的次微米铜粒子，
所述分散介质包含二乙二醇单丁醚，
以所述接合用铜糊的总质量为基准，所述二乙二醇单丁醚的含量为10质量％以上且30质量％以下，
所述次微米铜粒子是体积平均粒径为0.12μm以上且0.8μm以下的铜粒子，
所述次微米铜粒子经表面处理剂进行了处理，所述表面处理剂为碳数8～16的有机酸，
进行烧结时的气体环境为无氧环境。
7.根据权利要求6所述的半导体装置的制造方法，其中以所述金属粒子的总质量为基准，所述金属粒子含有5质量％以下的微米铜粒子。
8.根据权利要求6或7所述的半导体装置的制造方法，其中所述接合用铜糊的25℃下的粘度为0.8Pa·s～40000Pa·s。
9.根据权利要求6或7所述的半导体装置的制造方法，其中所述金属粒子更包含锌粒子、镍粒子、银粒子、金粒子、钯粒子或铂粒子。
10.根据权利要求6或7所述的半导体装置的制造方法，其中所述次微米铜粒子的纵横尺寸比为5以下。
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