TWI642511B - 接合材及使用其之接合方法 - Google Patents

接合材及使用其之接合方法 Download PDF

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Publication number
TWI642511B
TWI642511B TW104128611A TW104128611A TWI642511B TW I642511 B TWI642511 B TW I642511B TW 104128611 A TW104128611 A TW 104128611A TW 104128611 A TW104128611 A TW 104128611A TW I642511 B TWI642511 B TW I642511B
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Taiwan
Prior art keywords
copper
bonding material
mass
bonding
same manner
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TW104128611A
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English (en)
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TW201613714A (en
Inventor
遠藤圭一
三好宏昌
本村公一
栗田哲
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日商同和電子科技有限公司
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Publication of TW201613714A publication Critical patent/TW201613714A/zh
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Publication of TWI642511B publication Critical patent/TWI642511B/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • 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
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F7/008—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 characterised by the composition
    • 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
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • B23K1/0016—Brazing of electronic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/008—Soldering within a furnace
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K5/00—Gas flame welding
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
    • H01L21/52—Mounting semiconductor bodies in containers
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    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L24/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K2101/00—Articles made by soldering, welding or cutting
    • B23K2101/36—Electric or electronic devices
    • B23K2101/42—Printed circuits
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/08—Non-ferrous metals or alloys
    • B23K2103/12—Copper or alloys thereof
    • H—ELECTRICITY
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    • H01L2224/293—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/29338—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
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Abstract

本發明提供一種低價的接合材及使用其之接合方法，該接合材容易印刷於被接合物上且可抑制被接合物彼此之接合部產生孔洞。
本發明係一種接合材，其係由銅糊構成，且該銅糊含有：銅粉，其平均粒徑為0.1~1μm且含0.3質量%以下的碳；及一元醇、二元醇、三元醇、萜烯系醇等之醇系溶劑；其中，銅粉含量為80~95質量%，醇系溶劑含量為5~20質量%。

Description

接合材及使用其之接合方法 技術領域
本發明係有關於接合材及使用其之接合方法，特別係有關於由含銅粉之銅糊所構成之接合材及利用其來接合被接合物彼此之方法。
背景技術
近年來，提出有使用由包含銀微粒子作為金屬粒子之銀糊所構成之接合材，並使接合材介於被接合物間，於對被接合物間施加壓力的同時在預定時間下加熱，使接合材中的銀燒結來接合被接合物彼此(例如參照專利文獻1)。
當使用所述之接合材將Si晶片等電子零件固定於金屬基板上時，可於將已使銀微粒子分散於溶媒中之銀糊塗布於基板上後，加熱以去除溶媒，藉此於基板上形成預備乾燥膜，並於該預備乾燥膜上配置電子零件後，對電子零件施加壓力的同時進行加熱，藉此透過銀接合層使電子零件與基板接合。
先前技術文獻 專利文獻
專利文獻1：日本特開2011-80147號公報(段落編號0014-0020)
發明概要
但專利文獻1的接合材係使用銀微粒子作為金屬粒子，其為昂貴的接合材，故希望有一種使用比銀微粒子更低廉之金屬粒子的接合材。
又，若利用接合材來接合被接合物彼此時接合面有孔洞的話，即便被接合物彼此係以所欲之接合力接合著，當施加反覆冷熱循環時，孔洞部分會被施加應力，而會從孔洞龜裂到接合層，導致喪失接合可靠性。因此，為了利用接合材來良好接合被接合物彼此，必須抑制接合部產生孔洞，而需要抑制會造成孔洞之要因的溶劑(分散媒)的添加量(增加金屬粒子的含量)。另一方面，為了使用金屬罩藉由網版印刷來良好地接合接合材，則必須降低接合材的黏度。但若降低接合材的黏度則接合材中的金屬含量會降低，而另一方面若增加接合材中的金屬含量則接合材的黏度會變高，故接合材的黏度與接合材中的金屬含量為互償關係。
因此，本發明係鑑於所述習知問題點，而目的在於提供一種低價的接合材及使用其之接合方法，該接合材容易印刷於被接合物上且可抑制被接合物彼此之接合部產 生孔洞。
本發明人等為了解決上述課題而努力研究後，發現一種接合材，其由銅糊構成，且該銅糊含有平均粒徑為0.1~1μm之銅粉與醇系溶劑，並令銅粉含量為80~95質量%，醇系溶劑含量為5~20質量%，藉此可提供一種容易印刷於被接合物上且可抑制被接合物彼此之接合部產生孔洞之低價的接合材及使用其之接合方法，而完成本發明。
亦即，本發明之接合材，其特徵在於由銅糊構成，且該銅糊含有平均粒徑為0.1~1μm之銅粉與醇系溶劑，其中，銅粉含量為80~95質量%，醇系溶劑含量為5~20質量%。
該接合材中，銅粉中所含碳含量宜為0.3質量%以下。又，醇系溶劑宜為一元醇、二元醇或萜烯系醇，亦可含三元醇。又，利用流變計在25℃下以5rpm測定接合材的黏度時，黏度宜為150Pa‧s以下。進而，當使接合材介於被接合物間並加熱，藉此使接合材中的銅燒結並透過銅接合層來接合被接合物彼此時，相對於銅接合層之接合面的面積，孔洞所占面積比率宜為10%以下，且剪切強度宜為6MPa以上。
又，本發明的接合方法之特徵在於使上述接合材介於被接合物間並加熱，藉此使接合材中的銅燒結以形成銅接合層，並利用該銅接合層來接合被接合物彼此。且該接合方法以一邊對被接合物間施加壓力一邊加熱為佳。
根據本發明，可提供一種低價的接合材及使用其之接合方法，該接合材容易印刷於被接合物上且可抑制被接合物彼此之接合部產生孔洞。
用以實施發明之形態
本發明接合材的實施形態係一種接合材，其由含有平均粒徑為0.1~1μm之銅粉與醇系溶劑之銅糊構成，其中，銅粉含量為80~95質量%，醇系溶劑含量為5~20質量%。
銅粉之平均粒徑為0.1~1μm，且以0.2~0.8μm為佳，0.3~0.5μm更佳。又，銅粉以略球狀的銅粉為佳，且銅粉中所含碳含量宜為0.3質量%以下，且以0.1質量%以下更佳。
醇系溶劑宜為一元醇、二元醇或萜烯系醇，亦可含三元醇。一元醇宜使用癸醇或十二醇，亦可使用2-(2-己氧乙氧基)乙醇、2-[2-(2-乙基己氧基)乙氧基]乙醇、2-(2-丁氧乙氧基)乙醇等。二元醇宜使用己二醇或辛二醇，萜烯系醇宜使用萜品醇，亦可使用2-(1-甲基-1-(4-甲基-3-環己基)乙氧基)乙醇或異基環己醇等。三元醇宜使用甲基-丁三醇及丙三醇。此外，亦可混合該等醇系溶劑來使用。
銅糊中的(較佳為碳含量在0.3質量%以下的)銅 粉含量宜為80~95質量%(較佳為80~90質量%)，醇系溶劑含量宜為5~20質量%，(較佳為碳含量在0.3質量%以下的)銅粉與醇系溶劑合計宜為100質量%。該銅糊宜製成為將銅粉與醇系溶劑混合並捏合後，醇溶劑中僅有(較佳為碳含量為在0.3質量%以下的)銅粉呈分散之狀態者。
又，利用流變計在25℃下以5rpm測定接合材的黏度時，黏度宜在150Pa‧s以下，且以100Pa‧s以下為佳。
藉由使接合材介於被接合物間，並一邊對被接合物間施加壓力一邊加熱，以使接合材中的銅燒結並透過銅接合層來接合被接合物彼此時，相對銅接合層接合面之面積，孔洞所占面積比率宜為10%以下，且以5%以下為佳，又，剪切強度(將其中一被接合物朝寬度方向(往水平方向)按住而該被接合物從另一被接合物剝離時的力)宜為6MPa以上，且以30MPa以上為佳。
本發明接合方法的實施形態係藉由使上述接合材介於被接合物間(較佳為一邊對被接合物施加壓力)並加熱，以使接合材中的銅燒結以形成銅接合層，並透過該銅接合層來接合被接合物彼此。
具體來說，將上述接合材塗佈於2個被接合物其中一者上，並配置成接合材介於被接合物間，而於氮氣環境等惰性氣體環境中，一邊對被接合物間施加較佳為1~20MPa(更佳為5~10MPa)的壓力，一邊以較佳為60~150℃(更佳為80~130℃)加熱使接合材乾燥後，以較佳為200~400℃(更佳為250~370℃)加熱，藉此使銅糊中的銅燒結以 形成銅接合層，並透過該銅接合層來接合被接合物彼此。
此外，本說明書中，「平均粒徑」係指從場致發射型掃描電子顯微鏡(FE-SEM)算出之平均一次粒徑。該「平均一次粒徑」可利用場致發射型掃描電子顯微鏡(FE-SEM)以倍率2萬倍來觀察銅粒子，並於可在任意挑選之視野內觀察到的銅粒子(一次粒子)中測量長徑之全部銅粒子總數在200~500個程度之正方形測定範囲內，使用影像解析式粒度分布測定軟體(Mountech社製之Mac-View Ver.4)，測量各銅粒子最長的長度，算出個數基準之粒徑分布的累積值顯示為50%之50%粒徑。
實施例
以下，將就本發明之接合材及使用其之接合方法的實施例進行詳細說明。
[實施例1]
首先，準備一混合了如下硝酸銅水溶液與檸檬酸水溶液而得之混合溶液，該硝酸銅水溶液係於硝酸銅三水合物濃度為50.2質量%的硝酸銅溶液1174.6g中添加純水486.9g後稀釋而得，且該檸檬酸水溶液係使檸檬酸一水合物92.3g溶解於純水687g中而得。又，於混合了苛性鈉濃度為48.7質量%的苛性鈉水溶液449.1g與純水678g後倒入5L的反應槽內，並從反應槽上部以4.0L/分之流量導入氮藉此進行以氮除氣而得苛性鈉水溶液，並於準備苛性鈉水溶液的同時準備一已使含水肼(大塚化學工業股份有限公司製之80%肼水合物)26.6g溶解於純水687g中而成之肼水合物溶液。
接著，將上述苛性鈉水溶液倒入具備攪拌機的5L燒杯內並將液溫保持在27℃，一邊以旋轉數350rpm攪拌一邊添加上述混合溶液以生成氫氧化銅，之後，添加上述肼水合物溶液並升溫至70℃後，保持2小時以生成次氧化銅，藉此而製出次氧化銅漿體溶液。
於依上述所製得之次氧化銅漿體溶液中添加含水肼(大塚化學工業股份有限公司製之80%肼水合物)113.9g後，升溫至90℃而製得銅粉漿體溶液。將該銅粉漿體溶液進行固液分離，並用純水充分洗淨固體成分後，於氮氣環境中以110℃乾燥9小時而製得銅粉。利用場致發射型掃描電子顯微鏡(FE-SEM)(股份有限公司日立製作所製之S-4700)觀察依上述所製得之銅粉，其為略球狀粒子，且算出平均粒徑為0.5μm。並且利用碳.硫分析裝置(股份有限公司堀場製作所製之EMIA-220V)求得銅粉中的碳含量，碳含量為0.057質量%。
接著，將所製得之銅粉20.666g(86.9質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)3.124g(13.1質量%)混合而得一混合物，將該混合物倒入一次性杯中，以捏合脫泡機(股份有限公司EME製之V-mini300型)在公轉速度1400rpm、自轉速度700rpm下進行捏合30秒鐘之操作2次後，再倒入另一個一次性杯中進行2次相同之捏合，藉此而製得由銅糊構成之接合材。
以目視觀察依上述所製得之接合材(銅糊)之分 散狀態，其無液分離，分散狀態良好。又，利用流變計(黏彈性測定裝置)(Thermo社製之HAAKE Rheostress 600、使用錐：C35/2°)求得該接合材(銅糊)的黏度，在25℃下以5rpm下為42(Pa‧s)，印刷性(印刷適性)良好。
又，準備3片大小為10mm×10mm×2mm之(由無氧銅C1020構成)純銅板，且該純銅板係於以工業用醇(日本醇販售股份有限公司製之SOLMIX AP7)脫脂後經以10%之硫酸進行過處理者，並準備3片經施行過Ag鍍敷且大小為3mm×3mm×0.3mm的Si晶片。
接著，於各銅板上配置厚度50μm的金屬罩，並將上述接合材(銅糊)塗布於銅板上，塗成大小成為4mm×4mm且厚度成為50μm。
將依上述經塗佈有接合材之各銅板設置於接合裝置(倒裝晶片安裝)(HiSOL股份有限公司製之M90 DON-400)內，於氮氣環境中以100℃加熱而預備乾燥後，冷卻至25℃後於接合材上搭載Si晶片，並一邊於接合材與Si晶片之間施加荷重，一邊自25℃起以升溫速度10℃/s升溫至燒成溫度為止，且在該燒成溫度下保持5分鐘進行燒成，以使銅糊中的銅燒結而形成銅接合層，並透過該銅接合層將Si晶片接合於銅板上。此外，於3片銅板上分別以下述接合條件接合Si晶片，第1接合條件：預備乾燥時間為10分鐘，荷重為5MPa，燒成溫度為350℃；第2接合條件：預備乾燥時間為5分鐘，荷重為10MPa，燒成溫度為300℃；及第3接合條件：預備乾燥時間為5分鐘，荷重為10MPa，燒成溫度為350℃。
針對依上述所製得之接合體，使用高精度超音波顯微鏡(C-SAM)(SONOS社製之D9500)以50MHz觀察接合面之直徑0.1mm以上的孔洞(空孔)，並測定接合面的孔洞率(相對於接合面面積，孔洞所佔面積之比率)，孔洞率皆低至0%，為良好。又，使用接合強度試験機(bond tester)(DAGE社製之series 4000)，以剪切高度50μm、試験速度5mm/分來測定剪切強度(將Si晶片朝寬度方向(往水平方向)按住而Si晶片從銅板剝離時的力)，剪切強度各為高達84MPa、9MPa及100MPa，為良好。
[實施例2]
首先，於硝酸銅三水合物濃度為50.1質量%的硝酸銅溶液1412.3g中加入純水249.2g後稀釋而得硝酸銅水溶液，且使檸檬酸一水合物110.8g溶解於純水684.3g中而得檸檬酸水溶液，將該硝酸銅水溶液與檸檬酸水溶液混合後倒入5L的反應槽內，並自反應槽上部以4.0L/分的流量導入氮，藉此進行以氮除氣而得一混合溶液。又，準備一混合了苛性鈉濃度為48.8質量%的苛性鈉水溶液538g與純水589g而成之苛性鈉水溶液，並同時準備一已使含水肼(大塚化學工業股份有限公司製之80%肼水合物)31.9g溶解於純水684.3g而成之肼水合物溶液。
接著，將上述硝酸銅水溶液倒入具備攪拌機之5L燒杯內並將液溫保持在27℃，一邊以旋轉數350rpm攪拌一邊添加上述苛性鈉水溶液以生成氫氧化銅，並升溫至35℃後，添加上述肼水合物溶液並升溫至50℃，之後，保持2 小時以生成次氧化銅，藉此而製出次氧化銅漿體溶液。
於依上述所製得之次氧化銅漿體溶液中添加含水肼(大塚化學工業股份有限公司製之80%肼水合物)136.9g後，升溫至90℃而製得銅粉漿體溶液。將該銅粉漿體溶液進行固液分離，並用純水充分洗淨固體成分後，於氮氣環境中以110℃乾燥9小時而製得銅粉。以與實施例1相同方法觀察依上述所製得之銅粉，其為略球狀粒子，且算出平均粒徑為0.4μm。又，以與實施例1相同方法求得銅粉中的碳含量，碳含量為0.028質量%。
接著，除了使用將所製得之銅粉19.9968g(86.4質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)3.1368g(13.6質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為37(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法製得之接合體的接合面的孔洞率與剪切強度，孔洞率皆低至0%，且剪切強度各高達87MPa、23MPa及22MPa，皆良好。
[實施例3]
首先，於5L的反應槽內倒入純水3800g，並自反應槽下 部以0.5L/分的流量吹入空氣，且旋轉反應槽內的攪拌棒。接著，作為錯化劑將檸檬酸一水合物(扶桑化學工業股份有限公司製)5.33g投入反應槽內，同時將次氧化銅(日進-chemco股份有限公司製之NC-301，平均粒徑2.5μm)43.17g投入反應槽內，並於30℃下反應2小時而進行錯化處理後，停止供給空氣並自反應槽上部以2.0L/分的流量導入氮。接著，升溫至90℃為止，作為還原劑將含水肼(大塚化學工業股份有限公司製之80%肼水合物)40.2g投入反應槽內進行還原反應並保持1小時後，停止攪拌並洗浄、乾燥而製得銅粉。以與實施例1相同方法觀察依上述所製得之銅粉，其為略球狀粒子，且算出平均粒徑為0.2μm。又，以與實施例1相同方法求得銅粉中的碳含量，碳含量為0.183質量%。
接著，除了使用將所製得之銅粉20.0471g(87.0質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)3.0047g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其雖然看似有要凝集，但分散狀態幾乎良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為18(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第1接合條件)所得之接合體的接合面的孔洞率與剪切強度，孔洞率低至3%，而剪 切強度高達38MPa，皆良好。
[比較例1]
除了於次氧化銅漿體溶液中添加含水肼時添加膠原蛋白肽(新田明膠股份有限公司製之collagen peptide 800F)35.1g作為明膠類外，以與實施例2相同方法而得經明膠類被覆之銅粉。以與實施例1相同方法觀察依上述所製得之(經明膠類被覆之)銅粉，其為略球狀粒子，且算出平均粒徑為約0.3μm。又，以與實施例1相同方法求得銅粉中的碳含量，碳含量為0.347質量%。
接著，除了使用將所製得之(經明膠類被覆之)銅粉20.2517g(86.4質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)3.1805g(13.6質量%)混合而得之一混合物外，以與實施例1相同方法(之第1接合條件)而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其有些電漿子，但分散狀態幾乎良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為59(Pa‧s)，印刷性(印刷適性)幾乎良好。
又，使用所製得之接合材，以與實施例1相同方法(之第1及第3之接合條件)試著製作接合體，然皆無法將Si晶接合於銅板上。又，除了將荷重增加至10MPa外，以與實施例1相同方法試著製作接合體，但無法將Si晶片接合於銅板上。
[實施例4]
首先，準備一使硫酸銅五水合物(CuSO4‧5H2O)2.240kg溶解於純水5.353kg中而得之硫酸銅水溶液，及一於苛性鈉濃度為48.4質量%之苛性鈉水溶液1.840kg中加純水6.800kg稀釋而得之鹼性水溶液。
接著，於已保持在溫度27.6℃之上述鹼性水溶液中添加溫度27.3℃之上述硫酸銅水溶液並強攪拌後，將液溫升溫至36.0℃並予以保持，而得液中析出有氫氧化銅的氫氧化銅懸濁液。此外，於上述硫酸銅水溶液中添加上述鹼性水溶液後，液中苛性鈉相對於銅的當量比為1.24。
接著，將已使2.419kg的葡萄糖溶解於純水3.433kg而得之葡萄糖水溶液在氮氣環境下添加至上述氫氧化銅懸濁液中，並在30分鐘內升溫至液溫70.6℃為止後保持30分鐘。
於該氫氧化銅懸濁液中以2.26L/分之流量導入空氣並打泡200分鐘後，靜置在氮氣環境下1天，之後，去除上清液並採取幾乎全部量的沉澱物，且於該沉澱物中添加純水2.32kg而得4.80kg次氧化銅懸濁液。
將依上述所製得之次氧化銅懸濁液倒入反應槽內並一邊攪拌一邊保持在45.0℃，且添加含水肼(80.5%之肼一水合物)1.25當量(將全部次氧化銅還原所需之化學量論之1.25倍的量)後，在30分鐘內升溫至50.0℃為止，並更在70分鐘內升溫至85.0℃為止並予以保持，且將含水肼(80.5%之肼一水合物)分割出0.600當量後在30分間內添加，使全部的次氧化銅還原成銅而得銅粉漿體溶液。將該銅粉漿體溶 液進行固液分離，並用純水充分洗淨固體成分後，於氮氣環境中以110℃乾燥9小時而製得銅粉。利用場致發射型掃描電子顯微鏡(FE-SEM)(股份有限公司日立製作所製之S-4700)觀察依上述所製得之銅粉，其為略球狀粒子，且算出平均粒徑為1.0μm。並且利用碳.硫分析裝置(股份有限公司堀場製作所製之EMIA-220V)求得銅粉中的碳含量，碳含量為0.019質量%。
接著，除了使用將所製得之銅粉13.1g(87.0質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為32.0(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第1接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達14.6MPa，皆良好。
[比較例2]
首先，準備一已使硫酸銅五水合物(CuSO4‧5H2O)2.240kg溶解於純水5.353kg中而得之硫酸銅水溶液，及一於苛性鈉濃度為48.4質量%之苛性鈉水溶液1.840kg中加純水6.800kg稀釋而得之鹼性水溶液。
接著，於已保持在溫度27.6℃之上述鹼性水溶液中添加溫度27.3℃的上述硫酸銅水溶液並強攪拌後，將液溫升溫至36.0℃並予以保持，而得液中析出有氫氧化銅的氫氧化銅懸濁液。此外，於上述硫酸銅水溶液中添加上述鹼性水溶液後，液中苛性鈉相對於銅的當量比為1.24。
接著，將已使2.419kg的葡萄糖溶解於純水3.433kg而得之葡萄糖水溶液在氮氣環境下添加至上述氫氧化銅懸濁液中，並在30分鐘內升溫至液溫70.6℃為止後保持30分鐘。
於該氫氧化銅懸濁液中以2.26L/分之流量導入空氣並打泡200分鐘後，靜置在氮氣環境下1天，之後，去除上清液並採取幾乎全部量的沉澱物，且於該沉澱物中添加純水2.32kg而得4.80kg次氧化銅懸濁液。
將依上述所製得之次氧化銅懸濁液倒入反應槽內並一邊攪拌一邊保持在45.0℃，且添加含水肼(80.5%之肼一水合物)0.223當量(將全部次氧化銅還原所需之化學量論之0.223倍的量)後，在30分鐘內升溫至49.1℃為止，並將含水肼(80.5%之肼一水合物)分割出0.668當量後在120分鐘內添加，之後，在140分鐘內升溫至84.1℃為止並予以保持，且將含水肼(80.5%之肼一水合物)分割出1.055當量後在150分鐘內添加，使全部的次氧化銅還原成銅而得銅粉漿體溶液。將該銅粉漿體溶液進行固液分離，並用純水充分洗淨固體成分後，於氮氣環境中以110℃乾燥9小時而製得銅粉。利用場致發射型掃描電子顯微鏡(FE-SEM)(股份有限公司 日立製作所製之S-4700)觀察依上述所製得之銅粉，其為略球狀粒子，且算出平均粒徑為3.0μm。並且利用碳.硫分析裝置(股份有限公司堀場製作所製之EMIA-220V)求得銅粉中的碳含量，碳含量為0.051質量%。
接著，除了使用將所製得之銅粉13.1g(87.0質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為5.7(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率高達20%，剪切強度低至4.2MPa，皆非良好。
[實施例5]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之1-癸醇(和光純藥工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為7.6(Pa‧s)， 印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達12.2MPa，皆良好。
[實施例6]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之1-十二醇(東京化成工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為16.8(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達14.7MPa，皆良好。
[實施例7]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)1.0g(6.5質量%)及2-甲基丁烷-1,2,4-三元醇(日本萜烯化學股份有限公司製之IPLT-B)1.0g(6.5質量%)混合而得之一混合物外，以與實施例1相同方法而得由 銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為96.4(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達11.6MPa，皆良好。
[實施例8]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之2,5己二醇(東京化成工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為16.8(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達12.2MPa，皆良好。
[實施例9]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、 與作為溶劑之2-(2-己氧基)乙氧基)乙醇(日本乳化劑股份有限公司製之己基二甘醇)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為10.1(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達19.0MPa，皆良好。
[實施例10]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之2-(1-甲基-1-(4-甲基-3-環己基)乙氧基)乙醇(日本萜烯化學股份有限公司製之Terusolve TOE-100)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為46.0(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接 合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達13.3MPa，皆良好。
[實施例11]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為溶劑之萜品醇(和光純藥工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為41.6(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達25.8MPa，皆良好。
[實施例12]
除了使用將於實施例2製得之銅粉12.0g(80.0質量%)、與作為溶劑之辛二醇(和光純藥工業股份有限公司製之2-乙基-1,3-己二醇)3.0g(20.0質量%)混合而得之一混合物外，以與實施例1相同方法而得由銅糊構成之接合材。
以與實施例1相同方法觀察依上述所製得之接合材(銅糊)的分散狀態，其分散狀態良好。又，以與實施例1相同方法求得黏度，黏度在25℃下以5rpm下為4.6(Pa‧s)，印刷性(印刷適性)良好。
又，使用所製得之接合材，以與實施例1相同方法測定經以與實施例1相同方法(之第2接合條件)製得之接合體的接合面的孔洞率與剪切強度，孔洞率低至0%，且剪切強度高達22.0MPa，皆良好。
[比較例3]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為乙二醇醚系溶劑之二丁酯二甘醇(日本乳化劑股份有限公司社製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法試著製得由銅糊構成之接合材，但無法製成糊狀。
[比較例4]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為碳氫系溶劑之十四烷(東京化成工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法試著製得由銅糊構成之接合材，但無法製成糊狀。
[比較例5]
除了使用將於實施例2製得之銅粉13.1g(87.0質量%)、與作為乙二醇醚系溶劑之乙酸丁卡必醇(和光純藥工業股份有限公司製)2.0g(13.0質量%)混合而得之一混合物外，以與實施例1相同方法試著製得由銅糊構成之接合材，但無法製成糊狀。

Claims (7)

  1. 一種接合材，特徵在於由銅糊構成，且該銅糊含有平均粒徑為0.1~1μm之銅粉與醇系溶劑，其中，銅粉含量為80~95質量%，醇系溶劑含量為5~20質量%；以及該醇系溶劑包含一元醇、二元醇或萜烯系醇且包含三元醇。
  2. 如請求項1之接合材，其中前述銅粉中所含碳含量在0.3質量%以下。
  3. 如請求項1之接合材，其利用流變計在25℃下以5rpm測定前述接合材的黏度時，黏度在150Pa‧s以下。
  4. 如請求項1之接合材，當使前述接合材介於被接合物間並予以加熱，藉此使前述接合材中的銅燒結並透過銅接合層來接合被接合物彼此時，相對於銅接合層的接合面面積，其孔洞所占面積的比率在10%以下。
  5. 如請求項1之接合材，當使前述接合材介於被接合物間並予以加熱，藉此使前述接合材中的銅燒結並透過銅接合層來接合被接合物彼此時，其剪切強度在6MPa以上。
  6. 一種接合方法，其特徵在於：使如請求項1至5中任一項之接合材介於被接合物間並予以加熱，藉此使接合材中的銅燒結以形成銅接合層，並利用該銅接合層來接合被接合物彼此。
  7. 如請求項6之接合方法，其係一邊對前述被接合物間施加壓力一邊進行前述加熱。
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