TWI657463B - 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
TWI657463B
TWI657463B TW104116052A TW104116052A TWI657463B TW I657463 B TWI657463 B TW I657463B TW 104116052 A TW104116052 A TW 104116052A TW 104116052 A TW104116052 A TW 104116052A TW I657463 B TWI657463 B TW I657463B
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Taiwan
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silver
bonding material
mass
bonding
particles
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TW104116052A
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TW201603051A (zh
Inventor
遠藤圭一
湯崎浩一
永岡實奈美
三好宏昌
栗田哲
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日商同和電子科技有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01L24/01—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
    • 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
    • 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
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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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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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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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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    • 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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    • B23K1/0016—Brazing of electronic components
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    • B23K35/24—Selection of soldering or welding materials proper
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    • B23K35/3006—Ag as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
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    • B23K35/3613—Polymers, e.g. resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
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Abstract

一種接合材，該接合材係由銀糊膏構成，該銀糊膏含有銀微粒子、銀粒子、溶劑及分散劑，該銀微粒子係被己酸等碳數8以下之有機化合物所被覆且平均一次粒徑為1~50nm，該銀粒子係被油酸等有機化合物所被覆且平均一次粒徑為0.5~4μm，該溶劑係由1級醇系溶劑與萜烯系醇溶劑構成，該分散劑係由磷酸酯系分散劑(或磷酸酯系分散劑與丙烯酸樹脂系分散劑)構成，其中，銀微粒子之含量為5~30質量%，銀粒子之含量為60~90質量%，銀微粒子與前述銀粒子之合計含量為90質量%以上，且接合材中添加有具醚鍵之單羧酸系燒結助劑。

Description

接合材及使用其之接合方法 發明領域
本發明是有關於接合材及使用其之接合方法，尤其是有關於使用由含銀微粒子之銀糊膏所構成之接合材及使用其來將被接合物彼此接合之方法。
發明背景
近年，有提案使用含銀微粒子之銀糊膏作為接合材來使用，係使接合材中介於被接合物之間，一面在被接合物間施加壓力一面加熱預定時間，使接合材中之銀燒結，而將被接合物彼此接合(例如參照日本特開2011-80147號公報)。
使用這種接合材來取代鉛軟焊料以將被接合物彼此接合時，與利用鉛軟焊料接合被接合物彼此的情況相同，以不須在被接合物間施加壓力即可接合(無加壓接合)為佳。又，為了防止被接合物間之接合部有氧化銀形成致使接合力降低，以可在氮氣體環境等惰性氣體環境中亦可將被接合物彼此接合為宜。
這種不須在被接合物間施加壓力仍可在惰性氣體 環境中將被接合物彼此接合之接合材，已提案了在含銀微粒子之銀糊膏中添加氧二乙酸(雙二元醇酸)等助溶劑成分之接合材(參照例如日本特開2011-240406號公報)。
此外，為了使用金屬掩模藉網版印刷將接合材良好地塗佈，必須降低接合材的黏度。然而，一旦降低接合材的黏度，接合材中之銀含量會降低，另一方面，若提高接合材中之銀含量，則接合材之黏度變高，接合材的黏度與接合材中之銀含量呈現彼此制衡的關係。
一般而言，已知於接合材中添加分散劑以求降低由含銀微粒子之銀糊膏所構成之接合材的黏度，銀的含量高(溶劑添加量低)且可降低適於印刷時之黏度的接合材方面，已提案有在含銀微粒子之銀糊膏中添加磷酸酯系分散劑等磷酸系分散劑之接合材(參照例如日本特開2013-4309號公報)。
但是，當利用如日本特開2011-240406號公報這種在銀糊膏添加氧二乙酸(3-氧代戊二酸；diglycol acid)等助溶劑成分之接合材、或如日本特開2013-4309號公報這種添加了磷酸酯系分散劑等磷酸系分散劑之接合材進行被接合物間之接合時，有時會有接合部(銀接合層)生成未燒結部而無法良好地接合的情況。
因此，本發明鑑於上述習知問題點，目的在於提供一種接合材及使用其之接合方法，可輕易印刷至被接合物且可抑制被接合物彼此的接合部處產生未燒結部。
本發明群為了解決上述課題而專精研究，結果發現，在由含有平均一次粒徑1~50nm之銀微粒子、平均一次粒徑0.5~4μm之銀粒子、溶劑與分散劑之銀微粒子之銀糊膏所構成之接合材中，添加具有醚鍵之單羧酸系燒結助劑，藉此，可提供一種接合材及使用其之接合方法，其可容易對被接合物印刷，且可抑制在被接合物彼此之接合部產生未燒結部，進而完成本發明。
即，依據本發明之接合材，係由銀糊膏構成，其特徵在於該銀糊膏含有平均一次粒徑1~50nm之銀微粒子、平均一次粒徑0.5~4μm之銀粒子、溶劑及分散劑，其中，銀微粒子之含量為5~30質量%，銀粒子之含量為60~90質量%，銀微粒子與前述銀粒子之合計含量為90質量%以上，且接合材中添加有具醚鍵之單羧酸系燒結助劑。
該接合材中，前述具有醚鍵之單羧酸系燒結助劑以丁氧基乙基乙酸(butoxyethoxyacetic acid)為佳，且該具有醚鍵之單羧酸系燒結助劑之量，相對於前述銀糊膏以0.2~1.5質量%為佳。又，分散劑以磷酸系分散劑為佳，且磷酸酯系分散劑之量，相對於前述銀糊膏以0.01~0.2質量%為佳。又，分散劑也可含有丙烯酸樹脂系分散劑。這種情況下，丙烯酸樹脂系分散劑之量，相對於前述銀糊膏以2質量%以下為佳。又，溶劑以由1級醇系溶劑與萜烯系醇溶劑構成為佳。進一步，銀微粒子係被己酸等碳數8以下之有機化合物所被覆為佳，銀粒子係被油酸等有機化合物所被覆為佳。又，當利用流變儀在25℃下以6.4rpm測定上述接合 材之黏度時，黏度在100Pa‧s以下為佳。
又，依據本發明之接合方法，特徵在於係使上述接合材中介於被接合物之間予以加熱，藉此使接合材中之銀燒結以形成銀接合層，並透過該銀接合層將被接合物彼此接合。
再者，本說明書中，所謂「銀微粒子之平均一次粒徑」係指依據穿透式電子顯微鏡照片(TEM像)所得之銀微粒子一次粒徑的平均值，所謂「銀粒子之平均一次粒徑」係指藉由雷射繞射測定之銀粒子50%粒徑(D50徑)(累積50質量%粒徑)。
依據本發明，可提供一種接合材及使用其之接合方法，而輕易印刷至被接合物且可抑制被接合物彼此之接合部發生未燒結部。
發明之較佳實施態樣
依據本發明之接合材的實施形態，係一種由銀糊膏構成之接合材，該銀糊膏含有平均一次粒徑1~50nm之銀微粒子、平均一次粒徑0.5~4μm之銀粒子、溶劑及分散劑；其中銀微粒子之含量為5~30質量%、銀粒子之含量為60~90質量%、銀微粒子與銀粒子之合計含量在90質量%以上，並添加有具醚鍵之單羧酸系燒結助劑。
銀微粒子(銀奈米粒子)之平均一次粒徑為 1~50nm，以5~40nm為佳，10~30nm更佳。又，銀微粒子係以被己酸或山梨酸等碳數8以下之有機化合物所被覆為佳，被己酸所被覆更佳。
銀粒子(銀微米粒子)之平均一次粒徑為0.5~4μm，以0.7~3.5μm為佳，0.8~3μm更佳。又，銀粒子係以被油酸或硬脂酸等有機化合物所被覆為佳，被油酸所被覆更佳。
具醚鍵之單羧酸系燒結助劑以丁氧基乙氧基乙酸為佳。該具醚鍵之單羧酸系燒結助劑的量，相對於銀糊膏係以0.2~1.5質量%為佳，0.25~1.2質量%更佳。
分散劑係以含磷酸酯之分散劑等磷酸酯系分散劑為佳。該磷酸酯系分散劑之量，相對於銀糊膏係以0.01~0.2質量%為佳，0.1~0.15質量%更佳。又，分散劑亦可含有丙烯酸樹脂系分散劑。這種情況下，丙烯酸樹脂系分散劑之量，相對於銀糊膏係以2質量%以下為佳，1.5質量%以下更佳。
溶劑係以由1級醇系溶劑與萜烯系醇溶劑構成為佳。1級醇系溶劑方面可使用1-辛醇或1-癸醇，萜烯系醇溶劑方面可使用市售之含萜烯醇溶劑(日本Terpene Chemicals製之Terusolve TOE-100或Terusolve MTPH等)。溶劑之量，相對於銀糊膏係以3~8質量%為佳，4~7質量%更佳。
再者，利用流變儀(黏彈性測定裝置)在25℃下以6.4rpm測定該接合材之黏度時，黏度以100Pa‧s以下為佳。
依據本發明之接合方法之實施形態中，係使上述接合材介於被接合物之間進行加熱，藉此使接合材中之銀燒結而形成銀接合層，並藉該銀接合層將被接合物彼此接合。
具體而言，將上述接合材塗佈於兩被接合物之至少一者，並以令接合材介於被接合物之間予以配置，在60~200℃下、較佳為80~170℃下進行加熱，藉此使接合材乾燥而形成預備乾燥膜之後，在210~400℃下、較佳為230~300℃下進行加熱，藉此使銀糊膏中之銀燒結而形成銀接合層，並透過該銀接合層將被接合物彼此接合。再者，加熱之際，不需在被接合物間加諸壓力，不過加諸壓力亦無妨。此外，在氮氣體環境等非活性氣體環境下加熱即可將被接合物彼此接合，不過，在大氣中加壓也可將被接合物彼此接合。
以下，針對以本發明所獲致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
準備由銀糊膏構成之接合材，該銀糊膏含有：業經己酸被覆之平均一次粒徑20nm之銀微粒子(DOWA electronics(股)製之DP-1)19.785質量%、業經油酸被覆之平均一次粒徑0.8μm之銀粒子(DOWA HITEC(股)製之AG2-1C)72.215質量%、作為具有醚鍵之單羧酸系燒結助劑之丁氧基乙氧基乙酸(BEA)(東京化成工業(股)製)1.0質量%、及磷酸酯系分散劑(Lubrizol社製之SOLPLUS D540)0.14質 量%，且含有作為溶劑之1-癸醇(醇)3.64質量%、萜烯系醇溶劑(Japan Terpene Chemical(股)之Terusolve MTPH)3.22質量%。再者，該接合材中之銀濃度為91.32質量%。
利用流變儀(黏彈性測定裝置)(Thermo公司製之HAAKE Rheostress 600、使用圓錐：C35/2°)求取該接合材(銀糊膏)之黏度時，在25℃下，0.6rpm(2.1s-1)為211.8(Pa‧s)、6.4rpm(20.1s-1)為18.09(Pa‧s)，2s-1黏度相對於已在25℃下測定之20s-1黏度之比(2s-1黏度/20.1s-1黏度)(觸變比)為11.7，接合材(銀糊膏)之印刷性(印刷適性)良好。
此外，準備已利用乙醇脫脂且其後以10%硫酸處理之10mm×10mm×1mm大小之銅板、及已施予Ag鍍之3mm×3mm×0.3mm大小之Si晶片。
接下來，於銅板上配置厚度50μm之金屬掩模，並在銅板上塗佈上述接合材(銀糊膏)成3.5mm×3.5mm大小且厚度50μm。
接下來，將Si晶片配置於已塗佈在銅板上之接合材上，在接合材與Si晶片之間施加0.1MPa之負荷10秒之後，利用燈爐在氮氣體環境中自25℃以升溫速度0.1℃/s升溫至150℃，進行在150℃下保持30分鐘之預備燒成使銀糊膏乾燥，之後，以升溫速度0.1℃/s使之升溫至250℃，進行在250℃下保持60分鐘之正規燒成，使銀糊膏中之銀燒結而形成銀接合層，利用該銀接合層將Si晶片接合至銅板。
針對如此製得之接合體，利用掃描式電子顯微鏡(SEM)以3萬倍之倍率觀察接合部(銀接合層)之截面，結果 並未發現未燒結部，已良好接合。
實施例2
準備下述接合材：令丁氧基乙氧基乙酸(BEA)之量為0.5質量%，1-癸醇(醇)之量為4.14質量%，此外與實施例1同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為91.36質量%。
依據與實施例1相同之方法求取該接合材(銀糊膏)之黏度，在25℃下以0.6rpm(2.1s-1)測定為203.2(Pa‧s)、以6.4rpm(20.1s-1)測定為15.55(Pa‧s)，即在25℃下測定之2s-1黏度相對於20s-1黏度之比(觸變比)為13.1，接合材(銀糊膏)之印刷性(印刷適性)良好。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果未發現未燒結部，已經良好接合。
實施例3
準備下述接合材：令丁氧基乙氧基乙酸(BEA)之量為0.3質量%，1-癸醇(醇)之量為4.34質量%，此外與實施例1同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為91.36質量%。
依據與實施例1相同之方法求取該接合材(銀糊膏)之黏度，在25℃下以0.6rpm(2.1s-1)測定為125.7(Pa‧s)、以6.4rpm(20.1s-1)測定為16.69(Pa‧s)，即在25℃下測定之2s-1黏度相對於20s-1黏度之比(觸變比)為7.5，接合材(銀糊膏)之印刷性(印刷適性)良好。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果未發現未燒結部，已經良好接合。
實施例4
準備下述接合材：使用磷酸酯系分散劑，加上添加丙烯酸樹脂系分散劑(楠本化成(股)製之V0340)1.0質量%，且令1-癸醇(醇)之量為2.64質量%，此外與實施例1同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為91.32質量%。
依據與實施例1相同之方法求取該接合材(銀糊膏)之黏度，在25℃下以0.6rpm(2.1s-1)測定為497.5(Pa‧s)、以6.4rpm(20.1s-1)測定為39.46(Pa‧s)，即在25℃下測定之2s-1黏度相對於20s-1黏度之比(觸變比)為12.6，接合材(銀糊膏)之印刷性(印刷適性)良好。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果未發現未燒結部，已經良好接合。
比較例1
準備下述接合材：使用具有醚鍵之二羧酸系燒結助劑即二元醇酸(DGA)(Midori Kagaku(股)製)0.067質量%來取代丁氧基乙氧基乙酸(BEA)，且令1-癸醇(醇)之量為3.58質量%，此外與實施例4同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為91.33質量%。
依據與實施例1相同之方法求取該接合材(銀糊 膏)之黏度，在25℃下以0.6rpm(2.1s-1)測定為494.0(Pa‧s)、以6.4rpm(20.1s-1)測定為48.65(Pa‧s)，即在25℃下測定之2s-1黏度相對於20s-1黏度之比(觸變比)為10.2，接合材(銀糊膏)之印刷性(印刷適性)良好。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果很輕易即觀察到未燒結部，並未良好接合。
比較例2
準備下述接合材：令二元醇酸(DGA)(二羧酸)之量為0.201質量%，1-癸醇(醇)之量為3.44質量%，此外與比較例1同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為91.48質量%。
依據與實施例1相同之方法求取該接合材(銀糊膏)之黏度，結果黏度過高無法測定，接合材(銀糊膏)之印刷性(印刷適性)不良。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果觀察到些許未燒結部，並未良好接合。
比較例3
準備下述接合材：令丁氧基乙氧基乙酸(BEA)之量為0.1質量%，1-癸醇(醇)之量為4.54質量%，此外與實施例1同樣之銀糊膏所構成之接合材。再者，該接合材中之銀濃度為89.46質量%。
依據與實施例1相同之方法求取該接合材(銀糊膏)之黏度，在25℃下以0.6rpm(2.1s-1)測定為137.4(Pa‧s)、以6.4rpm(20.1s-1)測定為19.0(Pa‧s)，即在25℃下測定之2s-1黏度相對於20s-1黏度之比(觸變比)為7.2，接合材(銀糊膏)之印刷性(印刷適性)良好。
使用該接合材(銀糊膏)，依據與實施例1相同之方法製得接合體。針對該接合體，依據與實施例1相同之方法觀察銀接合層，結果觀察到些許未燒結部，並未良好接合。
該等實施例及比較例之接合材的製造條件及特性顯示於表1~表2。此外，表2中，接合材之黏度、印刷性及燒結性良好之情況以「○」表示，不良之情況以「×」表示。

Claims (12)

  1. 一種接合材，該接合材係由銀糊膏構成，其特徵在於該銀糊膏含有：平均一次粒徑為1~50nm之銀微粒子、平均一次粒徑為0.5~4μm之銀粒子、溶劑及分散劑，其中，銀微粒子之含量為5~30質量%，銀粒子之含量為60~90質量%，銀微粒子與前述銀粒子之合計含量為90質量%以上，溶劑由1級醇系溶劑與萜烯系醇溶劑構成，分散劑為磷酸酯系分散劑，且接合材中添加有具醚鍵之單羧酸系燒結助劑。
  2. 如請求項1之接合材，其中前述具有醚鍵之單羧酸系燒結助劑為丁氧基乙氧基乙酸。
  3. 如請求項1之接合材，其中前述具有醚鍵之單羧酸系燒結助劑之量，相對於前述銀糊膏為0.2~1.5質量%。
  4. 如請求項1之接合材，其中前述磷酸酯系分散劑之量，相對於前述銀糊膏為0.01~0.2質量%。
  5. 如請求項1之接合材，其中前述分散劑含有丙烯酸樹脂系分散劑。
  6. 如請求項5之接合材，其中前述丙烯酸樹脂系分散劑之量，相對於前述銀糊膏為2質量%以下。
  7. 如請求項1之接合材，其中前述銀微粒子係被碳數8以下之有機化合物所被覆。
  8. 如請求項7之接合材，其中前述被覆銀微粒子之有機化合物為己酸。
  9. 如請求項1之接合材，其中前述銀粒子係被有機化合物所被覆。
  10. 如請求項9之接合材，其中前述被覆銀粒子之有機化合物為油酸。
  11. 如請求項1之接合材，當利用流變儀在25℃下以6.4rpm測定前述接合材之黏度時，黏度在100Pa‧s以下。
  12. 一種接合方法，係使如請求項1至11中任一項之接合材中介於被接合物之間予以加熱，藉此使接合材中之銀燒結以形成銀接合層，並透過該銀接合層將被接合物彼此接合。
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