TWI729373B - 導電性膠及燒結體 - Google Patents

導電性膠及燒結體 Download PDF

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TWI729373B
TWI729373B TW108111518A TW108111518A TWI729373B TW I729373 B TWI729373 B TW I729373B TW 108111518 A TW108111518 A TW 108111518A TW 108111518 A TW108111518 A TW 108111518A TW I729373 B TWI729373 B TW I729373B
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Taiwan
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silver powder
mass
parts
particle size
aforementioned
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TW108111518A
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English (en)
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TW202006749A (zh
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酒金婷
竹政哲
清野順子
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日商千住金屬工業股份有限公司
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    • 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
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • 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
    • 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
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
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    • 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
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    • B22F3/10—Sintering only
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

本發明之目的在於提供一種作成燒結體時之電阻值低、導電性優異之導電性膠及其燒結體。
本發明之導電性膠係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑，相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份。

Description

導電性膠及燒結體
本發明係關於一種導電性膠及燒結體。
以往，使用μm尺寸(以下有時稱為「微米尺寸」)或nm尺寸(以下有時稱為「奈米尺寸」)之金屬粉的導電性膠係廣泛被使用為導電性材料。如此之使用微米尺寸或奈米尺寸之金屬粉的導電性膠，例如係使用於印刷配線基板中之電極、配線等電子電路的形成、或電子基板與電子零件之間的接合。
就如此使用金屬粉的導電性膠而言，於專利文獻1提出一種膠狀銀粒子組成物，其係由平均粒徑0.1至18μm且碳量為1.0重量%以下的非球狀銀粒子、及揮發性分散介質所構成的膠狀物，藉由加熱將該揮發性分散介質揮散而使該非球狀銀粒子彼此燒結。於專利文獻1中，具體揭示一種導電性膠，其係使用片狀銀粒子作為上述非球狀銀粒子，然而，如後述本發明之比較例2所述，如專利文獻1所記載之僅使用18μm以下之小平均粒徑之銀粒子(銀粉)的導電性膠，其燒結作成配線時的電阻值高，導電性並不充分。
又，於專利文獻2提出一種導電性膠，其含有具有0.1μm至15μm之平均粒徑(中位粒徑)的銀粒子、及醇類。於專利文獻2中，具體揭 示一種導電性膠，其係混合平均粒徑(中位粒徑)為0.3μm之銀粒子與平均粒徑(中位粒徑)為2.0至3.2μm之銀粒子的兩種銀粒子作為上述銀粒子。然而，如後述之本發明之比較例3及4所述，如專利文獻2之記載之僅混合15μm以下之小平均粒徑之兩種銀粒子的導電性膠，其燒結作成配線時的電阻值高，導電性並不充分。
於專利文獻3提出一種以銀粉末為主體之導電性膠的製造方法，其係包含下述步驟：準備導電性粉末之步驟，該導電性粉末係將平均粒徑互為不同之至少兩種球狀銀粉末、與平均粒徑互為不同之至少兩種片狀銀粉末混合而成者；使前述導電性粉末分散於有機介質中之步驟。於專利文獻3揭示了：作為上述至少兩種球狀銀粉末及至少兩種片狀銀粉末，係使用平均粒徑0.1至0.8μm之球狀銀粉末、平均粒徑1.0至2.0μm之球狀銀粉末、平均粒徑1至4μm之片狀銀粉末、及平均粒徑5至15μm之片狀銀粉末的組合。然而，專利文獻3所記載之4種銀粉末，皆為具有15μm以下之小平均粒徑者。如後述之本發明之比較例11至13所述，如專利文獻3所記載之不含具有25μm以上之中位粒徑之銀粉的導電性膠，於接合電子基板與電子零件時的接合強度並不充分。
於專利文獻4提出一種導電性接著劑，其特徵係，將銀箔粉碎所得之平均粒徑為45μm至1000μm、含有皺摺狀銀粉且視密度為0.01g/cm3至0.1/cm3之大型銀粉的充填量為5重量%以上、未滿25重量%，充填劑之充填量超過75重量%、95重量%以下。然而，專利文獻4所記載之導電性接著劑，係以含有高分子化合物為前提，與僅混合銀粉與溶劑的導電性膠為不同之材料。
[先前技術文獻] [專利文獻]
專利文獻1：國際公開第2007/034833號
專利文獻2：日本特開2009-170277號
專利文獻3：日本特開2004-362950號
專利文獻4：日本特開平5-81923號
以往之導電性膠的問題在於，塗布印刷配線基板上之後燒結作成配線時的電阻值高、導電性不充分，並且，接合電子基板與電子零件時之接合強度亦不充分。
因此，期盼一種作成燒結體時之電阻值低、導電性優異的導電性膠。再者，也期盼一種導電性優異且接合電子基板時之接合強度優異的導電性膠。
本發明之目的在於提供一種作成燒結體時之電阻值低、導電性優異的導電性膠及其燒結體。又，本發明之另一目的在於提供一種導電性優異且接合電子基板時之接合強度亦優異的導電性膠及其燒結體。
本發明人等為了解決上述問題而努力研究的結果發現，藉由將特定量之具有15μm以下之中位粒徑D50之片狀銀粉、特定量之具有25μm以上之中位粒徑D50之銀粉、及溶劑組合使用，可解決上述課題，而完成本發明。本發明之具體樣態係如以下所述。
又，本說明書中，使用「至」表示數值範圍時，該範圍係包含兩端的數值。
[1]一種導電性膠，係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑，其中相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份。
[2]一種導電性膠，係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、於0.1μm至0.5μm與1μm至15μm具有波峰之具有雙峰性粒度分布的銀粉、及溶劑，其中相對於前述片狀銀粉、前述具有25μm以上之中位粒徑D50之銀粉、及前述具有雙峰性粒度分布之銀粉的合計100質量份，前述片狀銀粉之含量為8至55質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為15至65質量份，前述具有雙峰性粒度分布之銀粉的含量為4至45質量份。
[3]如[1]所記載之導電性膠，其中，相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為30至42質量份、前述具有25μm以上之中位粒徑D50之銀粉的含量為58至70質量份。
[4]如[2]所記載之導電性膠，其中，相對於前述片狀銀粉、前述具有25μm以上之中位粒徑D50之銀粉、及前述具有雙峰性粒度分布之銀粉的合計100質量份，前述片狀銀粉之含量為23至35質量份，前述具有25μm 以上之中位粒徑D50之銀粉的含量為40至63質量份，前述具有雙峰性粒度分布之銀粉的含量為12至35質量份。
[5]一種燒結體，係將[1]至[4]中任一項所記載之導電性膠燒結所而成者。
[6]一種燒結體，係將含有基板、[1]至[4]中任一項所記載之導電性膠、及導電體的積層體燒結而成者。
本發明之導電性膠及其燒結體，作成燒結體時之電阻值低、導電性優異。
又，本發明之導電性膠及其燒結體，不只導電性優異，且將電子基板等接合時之接合強度亦優異。
第1圖係實施例中之電阻值之評價所使用之配線的概要圖。
第2圖係實施例中之剪切強度之評價所使用之試樣的概要圖。
第3A圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝實施例之銀粉(2-1)之表面的影像。
第3B圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝實施例之銀粉(2-2)之表面的影像。
第3C圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝實施例之銀粉(2-3)之表面的影像。
第3D圖係以掃描型電子顯微鏡(倍率：20000倍)拍攝實施例之銀粉(2-4)之表面的影像。
第4A圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝實施例3之燒結體之配線表面的影像。
第4B圖係以掃描型電子顯微鏡(倍率：700倍)拍攝實施例3之燒結體之配線剖面的影像。
第4C圖係以掃描型電子顯微鏡(倍率：5000倍)拍攝實施例3之燒結體之配線表面的影像。
第4D圖係以掃描型電子顯微鏡(倍率：10000倍)拍攝實施例3之燒結體之配線表面的影像。
第5A圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝比較例3之燒結體之配線表面的影像。
第5B圖係以掃描型電子顯微鏡(倍率：700倍)拍攝比較例3之燒結體之配線剖面的影像。
第5C圖係以掃描型電子顯微鏡(倍率：5000倍)拍攝比較例3之燒結體之配線表面的影像。
第5D圖係以掃描型電子顯微鏡(倍率：10000倍)拍攝比較例3之燒結體之配線表面的影像。
第6A圖係以掃描型電子顯微鏡(倍率：400倍)拍攝比較例7之燒結體之配線表面的影像。
第6B圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝比較例7之燒結體之配線表面的影像。
第7A圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝實施例3之燒結後之剪切強度測定用試樣之剖面的影像。
第7B圖係以掃描型電子顯微鏡(倍率：2500倍)拍攝實施例3之燒結後之剪切強度測定用試樣之剖面的影像。
第8A圖係以掃描型電子顯微鏡(倍率：1000倍)拍攝比較例3之燒結後之剪切強度測定用試樣之剖面的影像。
第8B圖係以掃描型電子顯微鏡(倍率：2500倍)拍攝比較例3之燒結後之剪切強度測定用試樣之剖面的影像。
以下，說明本發明之導電性膠及燒結體。
[第一實施形態]
本發明之導電性膠，係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑，其中，相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份。
片狀銀粉之中位粒徑D50為15μm以下，較佳為0.1μm至15μm，更佳為2μm至10μm。片狀銀粉之中位粒徑若在上述數值範圍內，會比使用球狀粉時增加表面積，故容易形成燒結體。
本發明中，各銀粉之中位粒徑D50，係指使用SALD-2300(島津製作所製)，以雷射繞射法所測定者。
本發明中，關於片狀銀粉，只要構成該銀粉之粒子的超過半數可於顯微鏡下確認為片狀(薄片狀或剝片狀)者即可。典型來說，係指構成該銀粉之粒子(初級粒子)的51質量%以上具有片(薄片或剝片)的形狀。此 處，所謂片狀(薄片狀或剝片狀)的粒子，係指長寬比(最長的長徑/最短的短徑之比)為5至300的粒子。
具有25μm以上之中位粒徑D50之銀粉的中位粒徑D50為25μm以上，較佳為25μm至100μm，更佳為30μm至80μm。
當僅使用粒徑未滿25μm者時，電流會傳遞至各粒子而流動，故粒子的接點數增多，使整體的電阻率增高。另一方面，具有25μm以上之中位粒徑D50之銀粉的中位粒徑若為上述範圍內，則由於含有每粒為大粒的粒子，故可減少粒子的接點數，使整體的電阻率降低。因此，比起僅使用粒徑未滿25μm者的情形相比，可得到作成燒結體時之電阻值低、導電性優異的導電性膠。
具有25μm以上之中位粒徑D50之銀粉的形狀，並無特別限定，可為球狀或非球狀之任一者。非球狀之例，可舉例如片狀、針狀、角狀、樹枝狀、粒狀、不規則形狀、淚滴狀、板狀、極薄板狀、六角板狀、柱狀、棒狀、多孔狀、纖維狀、塊狀、海綿狀、多角狀、丸狀等。如此之形狀之中，較佳為球狀、柱狀。
相對於片狀銀粉與具有25μm以上之中位粒徑D50之銀粉的合計100質量份，片狀銀粉之含量為15至70質量份，較佳為30至60質量份、更佳為30至50質量份。
相對於片狀銀粉與具有25μm以上之中位粒徑D50之銀粉的合計100質量份，具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份，較佳為40至70質量份，更佳為50至70質量份。
片狀銀粉之含量及具有25μm以上之中位粒徑D50之銀粉之含量，若皆在上述數值範圍內，則可得到作成燒結體時之電阻值低、導電性優異並且於接合電子基板等時之接合強度優異的導電性膠。
相對於導電性膠100質量份，片狀銀粉的含量較佳為10至50質量份，更佳為20至50質量份，最佳為30至50質量份。
相對於導電性膠100質量份，片狀銀粉的含量若未滿10質量份，則難以將含有片狀銀粉的組成物作成膠狀。又，即使可將含有片狀銀粉的組成物作成膠狀，由如此之導電性膠所得之燒結體，電阻值高、導電性差。
相對於導電性膠100質量份，具有25μm以上之中位粒徑D50之銀粉的含量較佳為15至60質量份，更佳為20至55質量份，最佳為30至55質量份。具有25μm以上之中位粒徑D50之銀粉的含量若在上述數值範圍內，則可得到作成燒結體時之電阻值低、導電性優異並且於接合電子基板等時之接合強度優異的導電性膠。
溶劑可舉例如水、醇系溶劑、二醇醚系溶劑、萜品醇類等。
醇系溶劑可舉例如異丙醇、1,2-二丁醇、異莰基環己醇、2,4-二乙基-1,5-戊二醇、2,2-二甲基-1,3-丙二醇、2,5-二甲基-2,5-己二醇、2,5-二甲基-3-己炔-2,5-二醇、2,3-二甲基-2,3-丁二醇、1,1,1-參(羥基甲基)乙烷、2-乙基-2-羥基甲基-1,3-丙二醇、2,2’-氧代雙(亞甲基)雙(2-乙基-1,3-丙二醇)、2,2-雙(羥基甲基)-1,3-丙二醇、1,2,6-三羥基己烷、雙[2,2,2-參(羥基甲基)乙基]醚、1-乙炔基-1-環己醇、1,4-環己二醇、1,4-環己烷二甲醇、赤蘚醇(erythritol)、蘇糖醇(threitol)、愈創甘油醚(Guaiacol Glycerol Ether)、3,6-二甲基-4-辛炔-3,6-二醇、2,4,7,9-四甲基-5-癸炔-4,7-二醇等。
二醇醚系溶劑可舉例如二乙二醇單-2-乙基己醚、乙二醇單苯醚、2-甲基戊烷-2,4-二醇、二乙二醇單己醚、二乙二醇二丁醚、三乙二醇單丁醚等。
相對於導電性膠100質量份，溶劑的含量較佳為2至20質量份，更佳為2至15質量份，最佳為5至10質量份。藉由使溶劑的含量在上述數值範圍內，可得到塗布性良好的膠。
[第二實施形態]
本發明之導電性膠係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、於0.1μm至0.5μm與1μm至15μm具有波峰之具有雙峰性粒度分布的銀粉、及溶劑，其中，相對於前述片狀銀粉、前述具有25μm以上之中位粒徑D50之銀粉、及前述具有雙峰性粒度分布之銀粉的合計100質量份，前述片狀銀粉之含量為8至55質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為15至65質量份，前述具有雙峰性粒度分布之銀粉的含量為4至45質量份。
有關片狀銀粉之中位粒徑D50、片狀形狀的定義、相對於導電性膠100質量份之片狀銀粉的含量、具有25μm以上之中位粒徑D50之銀粉的中位粒徑D50及形狀、相對於導電性膠100質量份之具有25μm以上之中位粒徑D50之銀粉的含量、溶劑的種類、以及相對於導電性膠100質量份之溶劑的含量，可使用第一實施形態中所示者。
具有雙峰性粒度分布之銀粉，係於0.1μm至0.5μm與1μm至15μm具有波峰，較佳為於0.1μm至0.3μm與3μm至10μm具有波峰。
本發明中，雙峰性粒度分布係指使用SALD-2300(島津製作所製)，以雷射繞射法所測定者。
具有雙峰性粒度分布之銀粉的形狀並無特別限定，可為球狀或非球狀之任一者。非球狀之例可舉例如片狀、針狀、角狀、樹枝狀、粒狀、不規則形狀、淚滴狀、板狀、極薄板狀、六角板狀、柱狀、棒狀、多孔狀、纖維狀、塊狀、海綿狀、多角狀、丸狀等。如此之形狀之中，較佳為球狀。
當具有雙峰性粒度分布之銀粉的形狀為球狀時，並不限於真球狀，只要構成該銀粉之粒子的過半數於顯微鏡下確認為球狀者即可。典 型來說，係指構成該銀粉之粒子(初級粒子)之80質量%以上具有球狀或類似於球狀之形狀。此處，所謂球狀之粒子，係指長寬比(長徑/短徑之比)為1.0至1.3的粒子。
相對於片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及具有雙峰性粒度分布之銀粉的合計100質量份，片狀銀粉的含量為8至55質量份，較佳為15至40質量份，更佳為20至35質量份。
相對於片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及具有雙峰性粒度分布之銀粉的合計100質量份，具有25μm以上之中位粒徑D50之銀粉的含量為15至65質量份，較佳為20至65質量份，更佳為30至60質量份。
相對於片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及具有雙峰性粒度分布之銀粉的合計100質量份，具有雙峰性粒度分布之銀粉的含量為4至45質量份，較佳為10至40質量份，更佳為15至30質量份。
片狀銀粉之含量、具有25μm以上之中位粒徑D50之銀粉的含量、及具有雙峰性粒度分布之銀粉的含量，若皆在上述數值範圍內，則可得到作成燒結體時之電阻值低、導電性優異並且於接合電子基板等時之接合強度優異的導電性膠。
相對於導電性膠100質量份，具有雙峰性粒度分布之銀粉的含量較佳為5至40質量份，更佳為10至35質量份，最佳為10至30質量份。
本發明之導電性膠可使用片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑、以及視情況之具有雙峰性粒度分布之銀粉，並使用ARV-310(THINKY股份有限公司製)裝置進行混練來製作。
[第三實施形態]
本發明係提供將上述導電性膠燒結而成之燒結體。
燒結體可藉由將導電性膠印刷或塗布於基板上之後進行燒結而得。如此之燒結體因具有導電性，可作為基板上之配線(電路)發揮功能。印刷或塗布導電性膠之方法，並無特別限定，可舉例如浸漬塗布、印刷塗布、噴霧塗布、刷毛塗布、注入等。
作為設置燒結體之基板，並無特別限定，可舉例如高耐熱之FR4等玻璃纖維強化環氧系印刷基板或聚醯亞胺系之基板、DBA(Direct Bonded Aluminum)或DBC(Direct Bonded Copper)等陶瓷基板、銅、銀、鋁等金屬基板、Cu導線架等。於基板可裝載電子零件。於金屬基板亦可施以金屬鍍覆。金屬鍍覆所使用之金屬，可舉例如金、銀、鎳、錫等。
燒結導電性膠時之條件，並無特別限定，燒結之溫度較佳為150至350℃，更佳為180至300℃，最佳為200至300℃。又，燒結之加熱時間較佳為10至60分鐘，更佳為15至45分鐘，最佳為20至30分鐘。於燒結時，對於導電性膠並不施加壓力。燒結可於大氣環境氛圍下、或氧濃度1%以上之環境氛圍下進行。
燒結體之形狀，並無特別限定，可舉例如片狀、薄膜狀、帶狀、線狀、圓盤狀、塊狀、點狀、不定形狀等。
本發明之燒結體可達成8.5μΩ‧cm以下之電阻值。燒結體之電阻值可藉由後述之(評價)之「(1)電阻值之評價」所記載之方法進行測定。
[第四實施形態]
本發明係提供一種將含有基板、上述導電性膠及導電體的積層體燒結而成的燒結體。
於基板上可依序積層導電性膠及導電體而製造積層體。接著，藉由燒結該積層體，可得到燒結體。於如此之燒結體中，來自導電性膠的部分由於具有導電性，並且接合基板與導電體，故具有作為導電性之接合部(接著部)的功能。所接合之基板可舉例如電路基板、玻璃纖維強化環氧系印刷基板或聚醯亞胺系之基板、陶瓷基板、金屬基板、Cu導線架等。又，所接合之導電體可舉例如電容器及電阻等晶片零件，或於晶圓形成電阻、電晶體、電容器、及積體電路等半導體元件後，由晶圓裁切出各半導體元件之區塊而得的晶片等。
燒結上述積層體時之條件，雖視要接合的對象而異，但例如對鍍Ag之Cu導線架燒結4mm×4mm矽晶片時，可舉例如在250℃、30分鐘、大氣壓、大氣環境氛圍下的條件。
燒結後之上述積層體可達成25MPa以上之剪切強度。於本發明中，剪切強度係指依據JIS Z 3198之方法所測定者，燒結後之上述積層體之接合強度(剪切強度)，可藉由後述之(評價)之「(2)剪切強度之評價」所記載之方法進行測定。
以下，依據實施例以更具體地說明本發明，但本發明並不限定於實施例所記載的內容。
[實施例]
(評價)
關於實施例1至11及比較例1至13之各導電性膠，如以下之方式進行電阻值及剪切強度的評價。
(1)電阻值的評價
將實施例1至11及比較例1至13之各導電性膠，使用金屬罩(厚度100μm)以網版印刷塗布於玻璃基板(厚度2mm)。將塗布有導電性膠之玻璃 基板，於大氣環境氛圍下，以大氣壓在200℃加熱30分鐘，以進行燒結而形成配線。如此所得之導電性膠之燒結體所成之配線的縱×寬之尺寸：3mm×30mm。所得的配線之概要圖顯示於第1圖。
對如此所得之實施例1至11及比較例1至13之各燒結體所成之配線，於室溫(25℃)及相對濕度50%的條件下，使用標準外徑測微器M110(MITUTOYO股份有限公司)測定配線的厚度。然後，對實施例1至11及比較例1至13之各配線，於室溫(25℃)及相對濕度50%的條件下，使用lozesta-GP MCP-T610(三菱化學股份有限公司)，以四端點法進行配線之電阻值(μΩ‧cm)的測定。電阻值測定時之四端點探針係使用ESP探針(三菱化學股份有限公司，MCP-TP08P、No.014052B)。對各配線進行測定三次，計算出電阻值(μΩ‧cm)的平均值。
配線之電阻值的平均值若為8.5μΩ‧cm以下，則可稱為導電性良好。
(2)剪切強度之評價
準備由銅基板側起依序藉由濺鍍而積層有Ti層(厚度40nm)及Ag層(厚度1000nm)的銅基板(縱×橫之尺寸：50mm×50mm)(以下稱為試驗片(1))。使用金屬罩(厚度100μm)將實施例1至11及比較例1至13之各導電性膠，網版印刷於試驗片(1)之Ag層上。
另一方面，準備由Si晶片側起依序藉由濺鍍而積層有Ti層(厚度40nm)及Ag層(厚度1000nm)的Si晶片(縱×橫之尺寸：3mm×3mm)(以下稱為試驗片(2))。
對於實施例1至3及5至11、及比較例1至3及5至13，使用晶片貼合機(製品名SMT-64RH，奧原電氣股份有限公司製)，將試驗片(2)之Ag層側積層於試驗片(1)所塗布之導電性膠上，而製得含有試驗片(1)、導電性膠、及試驗片(2)的試樣。將所得之試樣於大氣環境氛圍下、大氣壓下，以200℃加熱30分鐘，進行燒結。關於使用乙醇作為溶劑的實施例4及比較例4，若使用晶片貼合機，則於導電性膠上積層試驗片(2)之前，溶劑即揮發而無法接合試驗片(2)，又，若於大氣壓下進行燒結，則由於溶劑揮發快，而無法接合試驗片(2)。因此，關於實施例4及比較例4，除了於導電性膠上之試驗片(2)的積層以手動快速進行，並使燒結時之壓力為0.4MPa，除此以外之條件，與實施例1至3及5至11、以及比較例1至3及5至13同樣地進行，製得燒結後之試樣。
所得之燒結後之試樣的概要圖顯示於第2圖。
關於實施例1至11及比較例1至13之各燒結體的試樣，使用萬能型強度試驗機NordsonDAGE Series4000(Noedon Corporation製)，於室溫(25℃)條件下，依據JIS Z 3198的方法進行試驗片(1)與試驗片(2)之間的剪切強度(MPa)的測定。對各試樣進行測定5次，計算出剪切強度(MPa)的平均值。
若試樣之剪切強度的平均值為25MPa以上，則試驗片彼此的接合性可稱為良好。
(實施例1至11、比較例1至13)
使用市售之製品AgC239(福田金屬箔粉工業股份有限公司製，中位粒徑D50：2.5μm，片狀)(以下稱為「銀粉(1)」)作為片狀銀粉。
又，依以下的順序調製具有25μm以上之中位粒徑D50的兩種銀粉(以下分別稱為「銀粉(2-1)」及「銀粉(2-2)」)、具有未滿25μm之中位粒徑D50的銀粉(以下稱為「銀粉(2-3)」)、具有300至700nm之粒度分布的銀粉(以下稱為「銀粉(2-4)」)、及具有雙峰性粒度分布的銀粉(以下稱為「銀粉(3)」)。
‧銀粉(2-1)之製造
加熱銀使其為熔融狀態，藉由對該熔融之銀噴霧使其冷卻的方法(熔融噴霧法)，製作成中位粒徑D50：36.34μm之球狀的銀粉(銀粉(2-1))。
‧銀粉(2-2)之製造
加熱銀使其為熔融狀態，藉由對該熔融之銀噴霧使其冷卻的方法(熔融噴霧法)，製作成中位粒徑D50：31.13μm之球狀的銀粉(銀粉(2-2))。
‧銀粉(2-3)之製造
加熱銀使其為熔融狀態，藉由對該熔融之銀噴霧使其冷卻的方法(熔融噴霧法)，製作成中位粒徑D50：13.67μm之球狀的銀粉(銀粉(2-3))。
‧銀粉(2-4)之製造
以下述製造方法製作於300至700nm具有波峰之銀粉(銀粉(2-4))。
首先，使1.0g的硝酸銀(銀化合物)溶解於50g之乙二醇(多元醇)中。接著，於乙二醇中分散聚乙烯吡咯烷酮(分散劑)0.5g。接著，使乙二醇升溫至150℃(反應溫度)後，保持於反應溫度150℃，在以500rpm的轉速攪拌的情況下進行反應1小時。使用金屬罩將反應後之銀粉由乙二醇(多元醇)分離，並使用乙醇將分離後的銀粉洗淨，製得銀粉(2-4)。
對於所得之銀粉(2-1)至(2-4)，將以場發射掃描式電子顯微鏡(FE-SEM)(日本電子製JSM-7000F)所拍攝之影像顯示於第3A至3D圖。第3A至3C圖，係分別以1000倍拍攝銀粉(2-1)至(2-3)之表面者，第3D圖，為以20000倍拍攝銀粉(2-4)之表面者。
以下，將上述銀粉(2-1)至(2-4)統稱為銀粉(2)。
‧銀粉(3)之製造
藉由下述之製造方法製作於0.1μm至0.5μm與1μm至15μm具有波峰之具有雙峰性粒度分布的銀粉(銀粉(3))。
首先，以與銀粉(2-4)完全相同的製作方法製作銀粉A。接著，於以500rpm之轉速將50g之乙二醇攪拌之情況下，使2.0g之硝酸銀溶解於乙二醇中後，再於乙二醇中分散0.05g之銀粉A。接著，使乙二醇升溫至150 ℃(反應溫度)後，保持於反應溫度150℃，於以500rpm之轉速攪拌之情況下進行反應1小時。之後，使用金屬罩將反應後之銀粉由乙二醇分離，並使用乙醇洗淨分離後之銀粉，製得銀粉(3)。
又，本實施例及比較例所使用之銀粉(1)及(2-1)至(2-3)之中位粒徑D50、及銀粉(2-4)及銀粉(3)之粒度分布，係指使用SALD-2300(島津製作所製)以雷射折射法所測定者。
‧導電性膠之製作
依下述表1及表2所示之組成調製實施例1至11及比較例1至13之導電性膠。
又，下述表1及表2中之各成分之數值，係表示相對於導電性膠100質量份之各成分的質量份。
對於實施例1至11及比較例1至13之導電性膠，進行上述之電阻質及剪切強度的評價。將評價結果顯示於下述表1及表2。
Figure 108111518-A0202-12-0018-1
Figure 108111518-A0202-12-0019-3
實施例1至11之導電性膠係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑，其中，相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉之合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份。
由上述表1的結果可知，實施例1至11之導電性膠中，藉由燒結體得到之配線的電阻值低，具有良好的導電性，並且，燒結體之剪切強度優異，具有良好的接合性。
其中，可知特別是實施例2及3中，燒結體所成之配線的電阻值低，具有更良好的導電性，並且，燒結體之剪切強度優異，具有更良好的接合性。實施例2及3之導電性膠中，相對於片狀銀粉與具有25μm以上之中位粒徑D50之銀粉之合計100質量份，片狀銀粉之含量為30至42質量份，具有25μm以上之中位粒徑D50之銀粉的含量為58至70質量份者。
另一方面，上述表2所示之比較例1係不含銀粉(1)及銀粉(2)的導電性膠。比較例2至4及10係不含銀粉(2)的導電性膠。又，比較例7及9係不含銀粉(1)的導電性膠。比較例5及8的導電性膠雖然含有銀粉(1)及銀粉(2-1)兩者，但相對於銀粉(1)及銀粉(2-1)之合計100質量份，銀粉(1)的含量未滿15質量份，銀粉(2-1)的含量超過85質量份。又，比較例6的導電性膠雖然含有銀粉(1)及銀粉(2-1)兩者，但相對於銀粉(1)及銀粉(2-1)之合計100質量份，銀粉(1)的含量超過70質量份，銀粉(2-1)的含量未滿30質量份的導電性膠。比較例11至13係不含中位粒徑D50為25μm以上之銀粉的導電性膠。
由表2之結果可知，比較例1至5、7至10、及13之導電性膠與實施例1至13的導電性膠相比，燒結體所成之配線的電阻值高，導 電性不充分，又，燒結體之剪切強度低，接合性差。關於比較例6之導電性膠，雖然燒結體具有良好的接合性，但燒結體所成之配線的電阻值高，導電性不充分。又，關於比較例11及12的導電性膠，雖然燒結體所成之配線具有良好的導電性，但燒結體的剪切強度低，接合性差。
對於實施例3、及比較例3及7之燒結體所成的配線，將以場發射掃描式電子顯微鏡(FE-SEM)(日本電子製JSM-7000F)所拍攝之影像示於第4A至6B圖。
第4A、4C、及4D圖係分別以倍率1000、5000、10000倍拍攝實施例3之配線的表面者。第4B圖係以倍率700倍拍攝實施例3之配線的剖面者。
第5A、5C、及5D圖係分別以倍率1000、5000、10000倍拍攝比較例3之配線的表面者。第5B圖係以倍率700倍拍攝比較例3之配線的剖面者。
第6A及6B圖係分別以倍率400、1000倍拍攝比較例7之配線的表面者。
藉由第4A至4D圖，可於燒結體中觀察到實施例3之配線中分別來自小粒徑之片狀銀粉(1)、大粒徑之銀粉(2-1)、及小粒徑且具有雙峰性粒度分布的銀粉(3)之構造。可知實施例3之配線中，片狀之銀粒子及小粒徑之銀粒子與大粒徑之銀粒子互相充分地接觸，並且融合。咸信實施例3之配線中，配線內之電子的移動速度會因此而增大，電阻值降低。
另一方面，藉由第5A至5D圖可知，可於燒結體中觀察到比較例3之配線中分別來自小粒徑小片狀銀粉(1)、及小粒徑小且具有雙峰性粒度分布的銀粉(3)之構造。然而，比較例3之配線中，僅由小粒徑之銀粉(1)及(3)構成，不含大粒徑的銀粉(2-1)或(2-2)，故可知銀粒子彼此雖有 一部分接觸，但於其他部分，銀粒子彼此未充分接觸而無充分融合。因此，咸信比較例3之配線與實施例3之配線相比，電阻值增高。
又，由第6A及6B圖可知，比較例7之配線中，僅由大粒徑的銀粉(2-1)構成，不含小粒徑之銀粉(1)及(3)，故銀粒子分別獨立地存在，銀粒子彼此幾乎未融合。咸信於比較例7之配線中之電阻值會因此而極高。
又，對於實施例3及比較例3之燒結後的剪切強度測定用試樣，將以場發射掃描式電子顯微鏡(FE-SEM)(日本電子製JSM-7000F)所拍攝之影像顯示於第7A至8B圖。
第7A及7B圖係分別以倍率1000、2500倍拍攝實施例3之試樣的剖面者。第8A及8B圖係分別以倍率1000、2500倍拍攝比較例3之試樣的剖面者。
藉由第7A及7B圖，可於燒結體中觀察到實施例3之試樣中分別來自小粒徑之片狀銀粉(1)、大粒徑之銀粉(2-1)、及小粒徑且具有雙峰性粒度分布的銀粉(3)之構造。可知實施例3之試樣中，片狀銀粒子及小粒徑之銀粒子與大粒徑之銀粒子互相充分地接觸及融合，使燒結體內部的空隙減少。咸信實施例3之試樣中，燒結體會因此而密合於試驗片，而顯示良好的剪切強度。
另一方面，由第8A及8B圖可知，比較例3之試樣中，僅由小粒徑之銀粉(1)及(3)構成，不含大粒徑的銀粉(2-1)或(2-2)，故可知銀粒子彼此的接觸面積小而未充分融合，使燒結體內部的空隙增加。因此，咸信比較例3之試樣與實施例3的試樣相比，剪切強度較低。
又，由第7A及7B圖與第8A及8B圖之比較可知，比較例3之試樣與實施例3的試樣相比，燒結體部分的厚度較小。關於其原因，咸信是使用晶片貼合機將試驗片(2)裝載於導電性膠上時，由於晶片貼合機之噴嘴荷 重，使得不含大粒徑之銀粉(2-1)或(2-2)的比較例3，其導電性膠受到擠壓而使厚度變小。又，也可能是比較例3由於不含大粒徑之銀粉(2-1)或(2-2)，而含有大量的溶劑，故溶劑會於燒結時蒸發而收縮。
以上，由表1及表2的結果可知，藉由使用含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑的導電膠形成燒結體時之導電性優異，且顯示良好的接合性，其中，相對於前述片狀銀粉、與前述具有25μm以上之中位粒徑D50之銀粉之合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份

Claims (6)

  1. 一種導電性膠，係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、及溶劑，其中相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為15至70質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為30至85質量份，前述溶劑為水、醇系溶劑、二醇醚系溶劑或萜品醇類。
  2. 一種導電性膠，係含有：具有15μm以下之中位粒徑D50之片狀銀粉、具有25μm以上之中位粒徑D50之銀粉、於0.1μm至0.5μm與1μm至15μm具有波峰之具有雙峰性粒度分布的銀粉、及溶劑，其中相對於前述片狀銀粉、前述具有25μm以上之中位粒徑D50之銀粉、及前述具有雙峰性粒度分布之銀粉的合計100質量份，前述片狀銀粉之含量為8至55質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為15至65質量份，前述具有雙峰性粒度分布之銀粉的含量為4至45質量份。
  3. 如申請專利範圍第1項所述之導電性膠，其中，相對於前述片狀銀粉與前述具有25μm以上之中位粒徑D50之銀粉的合計100質量份，前述片狀銀粉之含量為30至42質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為58至70質量份。
  4. 如申請專利範圍第2項所述之導電性膠，其中，相對於前述片狀銀粉、前述具有25μm以上之中位粒徑D50之銀粉、及前述具有雙峰性粒度分布之銀粉的合計100質量份，前述片狀銀粉之含量為23至35質量份，前述具有25μm以上之中位粒徑D50之銀粉的含量為40至63質量份，前述具有雙峰性粒度分布之銀粉的含量為12至35質量份。
  5. 一種燒結體，係將申請專利範圍第1至4項中任一項所述之導電性膠燒結而成者。
  6. 一種燒結體，係將含有基板、申請專利範圍第1至4項中任一項所述之導電性膠、及導電體的積層體燒結而成者。
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