TWI624356B - Metal joint structure using metal nanoparticle, metal joint method, and metal joint material - Google Patents

Metal joint structure using metal nanoparticle, metal joint method, and metal joint material Download PDF

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Publication number
TWI624356B
TWI624356B TW103139044A TW103139044A TWI624356B TW I624356 B TWI624356 B TW I624356B TW 103139044 A TW103139044 A TW 103139044A TW 103139044 A TW103139044 A TW 103139044A TW I624356 B TWI624356 B TW I624356B
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Taiwan
Prior art keywords
metal
nanoparticles
joined
bonding layer
nanoparticle
Prior art date
Application number
TW103139044A
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English (en)
Other versions
TW201529294A (zh
Inventor
Kohei Tatsumi
Shinji Ishikawa
Norie Matsubara
Masamoto Tanaka
Original Assignee
Nippon Steel & Sumitomo Metal Corp
Univ Waseda
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Filing date
Publication date
Priority claimed from JP2013233118A external-priority patent/JP6384895B2/ja
Priority claimed from JP2013233117A external-priority patent/JP6384894B2/ja
Application filed by Nippon Steel & Sumitomo Metal Corp, Univ Waseda filed Critical Nippon Steel & Sumitomo Metal Corp
Publication of TW201529294A publication Critical patent/TW201529294A/zh
Application granted granted Critical
Publication of TWI624356B publication Critical patent/TWI624356B/zh

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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
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    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L24/32—Structure, shape, material or disposition of the layer connectors after 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
    • 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
    • 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
    • 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
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    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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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
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Abstract

本發明於使用金屬奈米粒子之同種或異種金屬接合中，當其中一被接合面金屬為Al系時，可藉由透過含Ni奈米粒子的接合層接合，來獲得具有優良接合強度的接合構造體。
而且，接合層是構成為以含金屬奈米粒子的2個接合層包夾金屬箔，而藉由透過該接合層接合同種或異種被接合面金屬，可緩和因2個具有被接合面金屬的被接合體之熱膨脹量差造成的熱應力。

Description

使用金屬奈米粒子之金屬接合結構及金屬接合方法以及金屬接合材料 發明領域
本發明，係有關於使用金屬奈米粒子之金屬接合構造及金屬接合方法以及金屬接合材料。
發明背景
金屬粒子方面，平均粒徑未達1μm，特別是1至100nm的金屬粒子稱為金屬奈米粒子。金屬奈米粒子，由於具有微細粒徑所導致之高結合性，已証實在較構成奈米金屬粒子金屬之熔點的極低之溫度下即可發生粒子間的結合。而且，亦可期待所獲得之結合體構造上的強度，可保持在該金屬的熔點附近。構成金屬奈米粒子的金屬，以Ag為代表，其他亦可例舉Au、Cu、Ni等(如專利文獻1)。
金屬奈米粒子一般而言，係使用具有有機殼包覆金屬奈米粒子之構造的有機-金屬複合奈米粒子。在室溫之下有機殼可防止奈米粒子的自行凝聚，而維持獨立分散之形態。而在加熱被接合材料表面上所提供的奈米粒子時，有機殼會被分解/去除，而發揮表面活性金屬奈米粒子低溫燒成之機能，則粒子彼此在燒成之同時還會被接合材料之表面與 結合。
在功率半導體的技術領域，將半導體晶片等固定在基板之功率半導體模組可使用在各種領域上。其中，半導體晶片與基板之接著等之中所使用的整合技術，係使用先前之焊接接合技術。
另一方面，近年來伴隨在功率半導體領域方面技術之發展，亦期待元件可實現為可在更高溫下使用的節能元件。然而，在功率半導體模組之接合中所使用的焊接接合方面，卻有在高溫下無法確保接合強度的問題。因而，刻正開發利用其中利用金屬奈米粒子的高結合性在半導體晶片等接合材料上的技術(專利文獻2、3)。
在接合2個被接合材料彼此時，如其中一方或雙方之被接合材料表面為Al，將使接合困難。且在使用Ag奈米粒子之金屬進行接合時，如金屬為Al將使接合強度極低。而且由於Al表面之氧化物安定，接合時亦無法去除氧化皮膜。因此專利文獻1中曾記載Al等難以與Ag奈米粒子接合。
在半導體元件之Al電極與Au線之接合中，係使用超音波熱壓接合法。經由在Al電極上在加壓接合Au線之下並施加超音波，以破壞Al電極表面之氧化皮膜，即可進行Al電極與Au線之金屬接合。然而，由於接合後半導體元件係置於高溫環境下，而會在接合部分之介金屬化合物相中發生孔隙，因此雖然以Al與Au組合初期可獲得高接合強度但並不適於高溫環境下使用。在以Al與Cu接合時，亦會發生孔隙而變差。
先前技術文獻 專利文獻
專利文獻1：日本專利特開2013-12693號公報
專利文獻2：日本專利特開2011-041955號公報
專利文獻3：日本專利特開2011-159994號公報
發明概要
由於使用金屬奈米粒子被接合體之被接合面金屬時，被接合面金屬與金屬奈米粒子之間可正確地組合。例如，在被接合面金屬係鋁(Al)或Al合金時，在被接合面金屬表面上可形成堅固之Al氧化物皮膜，由於其係存在於被接合面金屬與金屬奈米粒子之界面上，因此無法獲得充分之接合強度。
同時，含異種金屬所構成之接合構造的元件材料在昇溫、降溫時，由於各自材料之熱膨脹係數不同，而會發生起因於接合層之熱變形的熱應力。而且，即使在同種金屬所構成之接合構造，在各為不同溫度時，由於2個被接合材料之熱膨脹量不同，亦會發生起因於接合層之熱變形的熱應力。而且，以使用金屬奈米粒子的接合層來說，不用說焊料，就連相較於金屬奈米粒子相同的金屬塊亦硬，而延展性低，故無法好好地緩合伴隨熱變形的熱應力，而會在接合層形成龜裂等缺陷，降低接合強度。
對此，曾有提案藉由使用金屬奈米粒子增厚接合層厚 度，以求使熱應力緩和(專利文獻2)。
同時亦有提案只使接近被接合面中心為金屬奈米粒子之接合層，並對外周附近使用焊料之接合層(專利文獻3)。然而，在面對之被接合面伴隨溫度變化而熱膨脹時，金屬奈米粒子與焊料亦會產生熱變形量之差，因此有導致接合強度減低的可能性。而且，低熔點之焊料亦不適於高溫下使用。
因此，本發明之課題係提供一種在使用金屬奈米粒子之同種或異種金屬接合中，可充分保持接合層的接合強度之金屬接合構造及金屬接合方法以及金屬接合材料。
本發明人等，為解決上述問題經過積極檢討，獲得以下之瞭解。
其中發現在接合2個金屬體時，即使至少其中一者為Al或Al合金(本申請案中，包括兩者有時稱為Al系。)，在使用Ni奈米粒子作為接合中所使用之金屬奈米粒子時，兩者是可接合的。當使用Ni奈米粒子作為金屬奈米粒子時可與Al表面接合之理由未必已然明確，但推想可能係由於在加壓時，Al表面的氧化膜會部分被破壞，而Al與Ni奈米粒子直接接觸時，於溫度上昇時藉由Ni奈米粒子表面的活化力，會使Al與Ni奈米粒子進行金屬結合。同時另一部分，推想係因透過Al氧化物與Ni氧化物中其中一方或雙方之氧化物而接合。而且亦有透過氧化物暫時先使奈米粒子接合，之後在加熱之期間即會進行金屬接合，而得到堅固結合之情 形。
其次本發明人等，特別就用以接合未限定成分的2個被接合體的被接合面金屬之接合構造積極檢討。並特別就活用金屬奈米粒子，而可緩和熱應力之接合構造加以檢討。
其結果發現，藉由使2個被接合體的被接合面金屬之間的接合層，依序形成為含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層，可解決熱應力的問題。即使2個被接合體發生熱膨脹量之差時，由於設置在第1接合層與第2接合層之間的金屬箔變形可吸收熱膨脹量之差，結果可降低使用金屬奈米粒子的第1接合層與第2接合層的剪切變形量，而防止接合強度減低。
同時，亦發現在金屬箔為Al系、Ag系、Au系時，由於前述之瞭解而使用Ni奈米粒子等的接合構造，將可保持堅固之接合強度，同時亦可獲得因金屬箔所致的熱應力緩和效果。
本發明即依據此些瞭解而完成，即本發明主要係如下之各項。
(1)一種金屬接合構造，是2個被接合體之各自的被接合面金屬透過含金屬奈米粒子的接合層接合而成；該構造之特徵在於至少其中一被接合體的被接合面金屬為Al或Al合金，且前述金屬奈米粒子為Ni奈米粒子。
(2)如前述(1)項所載之金屬接合構造，其中前述被接合體之中至少其中一被接合面金屬為Al或Al合金，且前述 接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上。
(3)一種金屬接合方法，是於2個被接合體之各自的被接合面金屬之間形成含金屬奈米粒子的接合層，且加熱後，透過前述接合層接合2個被接合體；該方法之特徵在於至少其中一被接合體的被接合面金屬為Al或Al合金，且前述金屬奈米粒子為Ni奈米粒子，加熱溫度為200℃以上。
(4)如前述(3)項所載之金屬接合方法，其中前述被接合體之中至少其中一被接合面金屬為Al或Al合金，且前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上。
(5)一種金屬接合構造，是2個被接合體之各自的被接合面金屬透過含金屬奈米粒子的接合層接合而成；該構造之特徵在於前述接合層係依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層而成。
(6)如前述(5)項所載之金屬接合構造，其中當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子，而當前述金屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子。
(7)如前述(5)或(6)項所載之金屬接合構造，其中當前述被接合體之中至少其中一被接合面金屬為Al或Al合金時，前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上，而當至少其中一被接合面金屬為Ag、Au或該等之 合金中任一者時，前述接合層所含金屬成分之中由Ag、Au、Cu或Ni中一種以上所構成之金屬奈米粒子之合計為10質量%以上。
(8)如前述(1)、(2)、(5)、(6)或(7)中任一項所載之金屬接合構造，其中前述被接合體中至少其中一者為被接合面披覆有金屬之Si、SiC或化合物半導體。
(9)一種金屬接合方法，是於2個被接合體之被接合面金屬之間形成含金屬奈米粒子的接合層，且加熱後，透過前述接合層接合2個被接合體之被接合面金屬；該方法之特徵在於前述接合層係依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層而成；且當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子，而當前述金屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子，且加熱溫度為200℃以上。
(10)如前述(9)項所載之金屬接合方法，其中當前述接合層所含金屬箔為Al或Al合金時Ni奈米粒子的含量為10質量%以上，而當金屬箔為Ag、Au或該等之合金中任一者時由Ag、Au、Cu或Ni中一種以上所構成之金屬奈米粒子之合計為10質量%以上。
(11)一種金屬接合材料，是依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層而成。
(12)如前述(11)項所載之金屬接合材料，其中當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子， 而當前述金屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子。
本發明，在可在2個被接合體之被接合面金屬之間形成含金屬奈米粒子的接合層，經由接合層中之金屬奈米粒子接合2個被接合體之被接合面金屬所成之接合構造及接合方法中，即使金屬體中其中一方或雙方為Al系，接合所使用之金屬奈米粒子亦可以Ni奈米粒子，使兩者接合。
而且，藉由使2個金屬體之間的接合層係依序形成含金屬奈米粒子的第1接合層、Al系、Au系或Ag系之金屬箔、含金屬奈米粒子的第2接合層而成，即使在金屬體中產生熱膨脹量之差時，亦可經由設置在第1接合層與第2接合層之間的金屬箔變形而吸收熱膨脹量之差，結果可減低第1接合層與第2接合層的剪切變形量，防止接合強度降低。
1‧‧‧第1被接合體
2‧‧‧第2被接合體
3‧‧‧構成第1被接合面之金屬層
4‧‧‧構成第2被接合面之金屬層
5‧‧‧接合層
6‧‧‧第1接合層
7‧‧‧金屬箔
8‧‧‧第2接合層
圖1所示係本發明金屬結合構造之一例(第一態樣)的截面圖。
圖2所示係本發明金屬結合構造之一例(第二態樣)的截面圖。
用以實施發明之形態
本發明中之金屬奈米粒子，係指平均粒徑未達1μm的金屬粒子。以該類微粒子使用在接合構造中之接合層，可在較構成金屬奈米粒子的金屬之熔點極低之溫度下使粒子間發生結合，且獲得之結合體的構造上之強度，可保持至金屬熔點附近。金屬奈米粒子的平均粒徑以500nm以下為佳。在100nm以下時因可增加低溫下的燒結性而更佳。另一方面，在金屬奈米粒子的平均粒徑過小時將使表面的氧化物、有機成分之比例增大，以致降低接合性。因此，金屬奈米粒子的平均粒徑以5nm以上較佳。
對測定金屬奈米粒子平均粒徑之方法，金屬奈米粒子的平均粒徑可直接以高解析力SEM或TEM觀察，即可求出平均粒徑。
本發明係關於透過含金屬奈米粒子之接合層接合2個被接合體的被接合面金屬之接合構造體。其中被接合面金屬，係指接觸接合層並供於接合者，且所指為金屬者。亦即，在被接合體中構成被接合面的金屬，其態樣並無特別之限定。
舉例如，金屬製多面體之1面上形成其他金屬層，即可以該金屬層為被接合面。該情形時，構成該被接合面的金屬層即相當於本申請案中所指之被接合面金屬。
同時，亦可在如半導體、陶瓷或塑料等非金屬多面體之1面上形成。該情形時，即構成該被接合面的金屬層即相當於本申請案中所指之被接合面金屬。
當然，在金屬製多面體時，亦可以其1面作為被 接合面。
所有之情形下，金屬層之形成方法及態樣均無特別之限定。可以如化學方式蒸鍍(CVD)、物理方式蒸鍍(PVD)、電鍍、無電電鍍、金屬箔電鍍/接合等形成金屬層。
以下，本申請案中，包括前述之金屬層，構成被接合面金屬的金屬部分均稱為「金屬體」。
首先，對本發明之第一態樣以圖1加以說明。
圖1，係接合物(非接合體)1、2之接合面上形成有金屬體(圖中形成層狀)3、4者。圖1所示，係透過含金屬奈米粒子之接合層5接合2個金屬體3、4之接合構造體。
本發明之金屬接合構造及金屬接合方法中，其特徵係2個金屬體中其中一者或兩者為Al或Al合金，且金屬奈米粒子為Ni金屬或Ni合金。先前曾被指出，在被接合面為Al系之情形時，則難以使用金屬奈米粒子接合(專利文獻1)。此係由於Al表面之氧化物安定，在接合時無法去除氧化皮膜所致。相對於此於本發明中，係初次得知在接合中使用Ni奈米粒子為金屬奈米粒子時，即使在如金屬體為Al或Al合金時，亦可使兩者接合。對即使使用Ni奈米粒子為金屬奈米粒子時亦可與Al表面接合之理由未必已然明確，推想係由於在加壓時，Al表面的氧化膜會部分被破壞，而Al與Ni奈米粒子直接接觸時，於溫度上昇時藉由Ni奈米粒子表面的活化力，會使Al與Ni奈米粒子進行金屬結合。同時另一部分，推想係因透過Al氧化物與Ni氧化物中其中一方或雙方之氧化物而接合。而且亦有透過氧化物暫時先使奈米 粒子接合，之後在加熱期間即會進行金屬接合，而得到堅固結合之情形。
構成金屬體的Al，意指所包含的Al含量為98.0質量%以上者，而其他為不特定不純物或微量添加元素之構成。而以使用JISH4160中所載者較佳。構成金屬體的Al合金方面，只要合金中Al含量為85質量%以上即可並無特別之限定，而以使用JIS規格中所規定的Al合金較佳。
在要求高電導之情形時，以使用較高純度、高耐熱性，Al-2質量%Si、Al-2質量%Cu、Al-1質量%Si-0.5質量%Cu、Al-1質量%Si-0.1質量%Zr、Al-4質量%Cu等更佳。而且，由於合金化可更提高耐熱性，使用如Al-2.2質量%Si、Al-1質量%Si-0.5質量%Cu-0.6%質量Fe、Al-1質量%Si-1.0質量%Fe-0.2質量%Cu、Al-1質量%Fe-0.5質量%Si-0.2質量%Cu-0.8質量%Mn又更佳。
對Ni奈米粒子與Al或Al合金的界面，已証實在金屬之間、或者透過氧化物可堅固地接合，在350℃以上的高溫下使用亦可維持在高可信賴性之接合狀態。
金屬奈米粒子所構成之Ni奈米粒子以所含Ni為95質量%以上為佳，亦可含Ni以外之合金成分。合金成分，意指如含Ag、Cu、Fe、P之1種或2種以上的合金。
而且，由以上所瞭解當其中一金屬體為Al或Al合金時，另一金屬體，以使用Al、Cu、Ag、Au、Ni或該等之合金較佳。
其次，對本發明之第二態樣以圖2加以說明。
圖2，係在接合物(被接合體)1、2之被接合面上形成金屬體(圖中形成層狀)3、4者。圖1所示，係以2個金屬體3、4，透過含金屬奈米粒子之接合層接合而成的接合構造體，該接合層係以含金屬奈米粒子之2個接合層(本申請案中便利上稱為第1接合層6及第2接合層7。)夾著金屬箔7所構成。
在第一態樣中，在進行以金屬奈米粒子接合時，如圖1所示，係在2個金屬體3、4之間形成含金屬奈米粒子之接合層5。然而，由於具接合構造之元件材料1、2在昇溫、降溫時，在2個被接合材料由不同之材料構成，且各自的材料之熱膨脹係數不同時，或者2個被接合材料在不同溫度時，由於2個被接合材料之熱膨脹量不同，因此接合層會發生起因於熱變形的熱應力。而且，以使用金屬奈米粒子的接合層來說，不用說料，就連相較於金屬奈米粒子相同的金屬塊亦硬，而延展性低，故無法好好地緩和伴隨熱變形的熱應力，而會在接合層形成龜裂等缺陷，降低接合強度。
本發明中，如圖2所示，藉由在2個金屬體之間，依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層，即可成功地解決上述問題。即使在含金屬體的2個被接合體發生熱膨脹量之差時，亦可由設置在第1接合層與第2接合層之間的金屬箔之變形而吸收熱膨脹量之差，結果可減低使用金屬奈米粒子的第1接合層與第2接合層之剪切變形量，因此可防止接合強度降低。
在2個被接合材料由不同之材料所構成，且各自的材料之熱膨脹係數不同時，在為燒結金屬奈米粒子而加 熱時即會發生熱應力的問題。如在圖1所示之構造中，在其中一被接合體1係以Si所構成，另一被接合體2係以Cu所構成時，Si與Cu的熱膨脹率並不同。在為燒結金屬奈米粒子而以300℃進行熱處理時，Si及Cu各以在300℃下相對的熱膨脹值決定長度，在該狀況下進行燒結即形成接合層5。之後降至常溫時，由於2個被接合體的熱收縮量不同，接合層5內即會發生起因於熱應力之熱變形。由於燒結金屬奈米粒子的接合層5延展性低，即使該程度之熱應力接合層內亦會發生龜裂，結果使使用金屬奈米粒子的接合層之剪切強度之值不足。相對於此在如圖2所示之構造時，可由設置在第1接合層與第2接合層之間的金屬箔之變形而吸收熱膨脹量之差，結果可減低第1接合層與第2接合層之剪切變形量，因此可防止接合強度之降低。
本發明之金屬接合構造中所設置的金屬箔，以使用Al或Al合金為佳。Al或Al合金由於延展性佳，因此適於吸收接合構造中所負荷的熱膨脹量之差。
相對於此如本發明第一態樣中之說明，以接合中所使用之金屬奈米粒子使用Ni奈米粒子，及在例如金屬體為Al或Al合金，亦可與金屬奈米粒子接合。
構成金屬箔層之Al，意指所包含的Al含量為98.0質量%以上者，而其他為不特定不純物或微量添加元素之構成。而以使用JISH4160中所載者較佳。構成金屬箔層的Al合金方面，只要合金中Al含量為85質量%以上即可並無特別之限定，可使用延展性及電導性優良之Al合金。而且， 在合金化以可提高箔的耐熱性上，以使用Al-2質量%Si、Al-1質量%Si-0.5質量%Cu-0.6質量%Fe、Al-1質量%Si-1.0質量%Fe-0.2質量%Cu、Al-1質量%Si-0.1質量%Zr、Al-4質量%Cu等更佳。
而且，由於合金化可提高耐熱性，以使用如Al-2.2質量%Si、Al-1質量%Si-0.5質量%Cu-0.6%質量Fe、Al-1質量%Si-1.0質量%Fe-0.2質量%Cu、Al-1質量%Fe-0.5質量%Si-0.2質量%Cu-0.8質量%Mn又更佳。
在構成金屬箔層之金屬為Al時，對接合層第一態樣及第二態樣均相同。
接合層中，亦可含Ni奈米粒子以外之金屬成分。其他之金屬成分，可為Ni以外之金屬奈米粒子，亦可為平均粒徑1μm以上未達100μm的大粒徑金屬粉末。在為金屬奈米粒子時，可使用Ag、Au、Cu、Sn之金屬或合金。
同時，在大粒徑金屬粉末之情形時，可使用Ni、Ag、Au、Cu、Sn之金屬或合金。在任一情形下，由於Al或Al合金所構成之被接合面係在與Ni奈米粒子之間接合、大粒徑金屬粉末係與周圍之金屬奈米粒子接合、Al以外所構成之被接合面係在與金屬奈米粒子之間接合、金屬奈米粒子之間亦接合，其結果，可形成具良好接合力之接合層。且接合層中所含之金屬成分中，Ni奈米粒子合計的含量越多，越可獲得良好之接合力。另一方面，在Ni奈米粒子的含量為10質量%以上時，即可保証本發明有充分之結合力。Ni奈米粒子的含量在50質量%以上時更佳。在80質量%以上 時又更佳。
以往，Al材料係難以與其他之金屬材料(包含Al)熔接。此係由於難以去除Al表面上形成之氧化皮膜。同時，在半導體元件之Al電極與Au線之接合中，係使用超音波熱壓接合法。此經由在Al電極上在加壓接合Au線下並施加超音波，以破壞Al電極表面之氧化皮膜，即可進行Al電極與Au線之金屬接合。
然而，由於接合後半導體元件係置於高溫環境下，而會在接合部分之介金屬化合物相中發生孔隙，因此雖然以Al與Au組合在初期可獲得高接合強度但並不適於高溫接合中利用。相對於此本發明中，對被接合面的Al與Ni奈米粒子的接合部分，即使在300℃以上之高溫環境中在接合部分亦不會生成孔隙，因此不會發生接合強度變差之問題。因此，即使在高溫環境下使用之材料、在重複高溫與低溫間熱循環之環境下使用的材料，亦可維持適當的接合強度。
在金屬箔為Ag、Au或該等之合金中任一者所構成之情形時，在前述含金屬奈米粒子的第1接合層、第2接合層中所含的金屬奈米粒子，可使用由Ag、Au、Cu、Ni中一種以上所構成之金屬奈米粒子。如此Ag奈米粒子、Au奈米粒子、Cu奈米粒子或Ni奈米粒子與Ag金屬箔或Au金屬箔的接合界面上，即使在350℃以上之高溫下使用，亦可維持高可信賴性。
構成金屬箔之Ag，意指Ag含量為90質量%以上 者。再者，Ag合金，意指合金中Ag含量為60質量%以上，合金成分方面，係含如Au、Pd之1種或2種以上的合金。而以使用如Ag-11%Au、Ag-15%Cu-15%Zn、Ag-22%Cu-17%Zn-5%Sn為佳。同時表面亦可施加Au、Pd等之電鍍。
同樣地，構成金屬箔之Au，意指Au含量為90質量%以上者。再者，Au合金，意指合金中Au含量為60質量%以上，合金成分方面，係含如Ag、Cu、Mn、Pd之1種或2種以上的合金。而以使用如Au-11%Ag為佳。同時表面亦可施加Au、Ag、Pd等之電鍍。Ni金屬、Ni合金可使用如前述者。
而且在金屬箔為Ag、Au系時，接合層中，亦可含由Ag、Au、Cu、Ni中一種以上所構成之金屬奈米粒子以外的金屬成分。該其他金屬成分，可為各種金屬之奈米粒子，亦可為平均粒徑1μm以上之大粒徑金屬粉末。在係金屬奈米粒子時，可使用Sn、Zn或該等之合金。
同時，在係大粒徑金屬粉末時，可使用Ni、Ag、Au、Cu、Sn、Zn或該等之合金。在所有之情形下，由於金屬箔表面及被接合面係在與金屬奈米粒子之間接合、大粒徑金屬粉末係與周圍之金屬奈米粒子接合、金屬奈米粒子之間亦可接合，其結果，可形成具良好接合力之接合層。當由Ag、Au、Cu、Ni中一種以上所構成之金屬奈米粒子合計的含量為10質量%以上時，即可保証本發明有充分之結合力。此類金屬奈米粒子合計之含量以50質量%以上為佳。在80質量%以上更佳。
本發明中，由於含金屬奈米粒子之接合層，係以金屬之間的接合形成全體之接合力，因此接合層中無含金屬以外成分之須要。而可如後述地，在形成含金屬奈米粒子之接合層時，是形成金屬奈米粒子糊來披覆接合部分，之後加熱至200℃以上即可實現金屬奈米粒子之接合。金屬奈米粒子糊，係在醚系等溶劑中分散金屬奈米粒子。而且，該金屬奈米粒子是由有機殼所包覆。
因此，在加熱前接合層中係含糊中之溶劑成分及有機殼成分。之後經由加熱至200℃以上，即可使溶劑成分及有機殼成分分解，一部分揮發而自接合層脫離，其餘部分受高溫而碳化殘餘在接合層中。此類碳化而殘餘的成分，係與接合層之接合力無關。即使如在接合層中含金屬以外的成分，在接合層中所含之金屬成分，占接合層中全固體成分之50體積%(除空洞或空隙部分之外)以上，或更好是70體積%以上時，即可充分發揮本發明之效果。
本發明中之金屬箔，只要為厚度5至200μm的金屬材料即可並無特別之限定。舉例如各種金屬以輥壓延而獲得之金屬箔。金屬箔之厚度，以5至100μm為佳，10至50μm更佳。在厚度未達5μm時，會提高在接合時加壓時之龜裂等缺點的可能。若使厚度加厚則與難以維持平坦性、抑制盤捲在捲盤時的變形等生產性之低落、或增加材料成本關聯，因此以在上述上限值以下為佳。再者金屬箔之材質，彈性模數以110GPa以下為佳，85GPa以下更佳。在彈性模數超過110GPa時，會降低應力緩和效果，而因熱應力等使 Si晶片元件損傷等之危險提高。
含金屬奈米粒子的第1接合層、第2接合層之厚度，各在加熱結束後時，以0.5至100μm為佳，3至50μm更佳。
本發明之具接合構造的接合體，可在2個被接合體中其中一側配置半導體元件，在另一側配置金屬基板、樹脂基板、或陶瓷基板，之後整合加熱接合材料及被接合體獲得。本發明特別適用於在Si、SiC、化合物半導體等基板上披覆金屬為被接合金屬。金屬基板之例，可舉如：鋁基板、鐵基板、銅基基板、不銹鋼基板等，樹脂基板之例，可舉如：環氧樹脂基板、酚樹脂基板等，陶瓷基板之例，可舉如：氧化鋁基板、碳化矽基板、氮化物系基板等。
形成本發明金屬接合構造之金屬接合方法方面，可由以下數種方法中選擇。
第1種方法中，係在構成其中一被接合體的被接合面(第1被接合面)之金屬體上披覆含金屬奈米粒子的第1接合層，其次於第1接合層上披覆金屬箔，接著於金屬箔上披覆含金屬奈米粒子的第2接合層，最後披覆構成另一被接合體的被接合面(第2被接合面)之金屬體。
第2個方法中，係在構成其中一被接合體的被接合面(第1被接合面)之金屬體上披覆含金屬奈米粒子的第1接合層，之後將另外含金屬奈米粒子的第2接合層披覆在構成另一被接合體的被接合面(第2被接合面)之金屬體上。其次，使第1接合層與第2接合層相對，其間夾著金屬箔，各使第1接合層、金屬箔、第2接合層接觸。
第3種方法中，係在金屬箔之兩側各披覆含金屬奈米粒子的第1接合層及第2接合層並以其為金屬接合材料。其次，使該金屬接合材料中其中一面(第1接合層側)與構成第1被接合面的金屬體接觸，另一面(第2接合層側)與構成第2被接合面的金屬體接觸，以其形成接合構造。
除了以上述第1至3中任一方法形成接合構造，還可加熱至200℃以上之溫度來接合2個被接合體。經由加熱，可在金屬奈米粒子之間、被接合面與金屬奈米粒子之間、金屬箔表面與金屬奈米粒子之間燒結，而可實現堅固之結合力。該接合體製造時的加熱溫度，在可得到充分之接合強度上，以200℃以上為佳，250℃以上更佳。同時，在加熱溫度超過450℃時，會有半導體元件及樹脂基板等之損傷的顧慮，因此以450℃以下為佳，400℃以下更佳。而且，以在加熱該接合體之同時，於接合材料及被接合體上施加壓力較佳。該壓力以0.1至100MPa為佳，2至30MPa更佳。
在被接合面上或金屬箔上形成含金屬奈米粒子之層時，可先準備含金屬奈米粒子糊，將該金屬奈米粒子糊塗布在被接合面上進行。該金屬奈米粒子糊，可準備有機殼包覆之金屬奈米粒子，並將該金屬奈米粒子分散於預定之溶劑中，成為漿料狀、糊狀、乳劑狀、或蠟狀等組成物。接合層之形成，可以該組成物經由如：氣式噴霧塗布機、輥塗布機、靜電式噴霧塗布機等以層狀塗布在被接合面及金屬箔上製造。
在調製含金屬奈米粒子的組成物上，保護劑方面 可以胺系、羧酸系、高分子系，分散劑可以胺系、羧酸系、醇系，溶劑可以醇系或醚系，配合金屬奈米粒子之種類選擇即可。而且，視其需要，該組成物中，添加選自習知已知之各種陰離子系、陽離子系、非離子系等的分散助劑，亦可賦予組成物期望之流動性等。含金屬奈米粒子糊中溶劑之含量以5至80質量%左右為佳。10至50質量%更佳。
使用含金屬奈米粒子糊形成接合層，之後進行用以燒結金屬奈米粒子之加熱時，金屬奈米粒子糊中之溶劑會被去除，使接合層中之金屬成分成50體積%以上，或更佳時為70體積%以上而可在前述較佳之金屬成分含量範圍。
實施例
〔實施例1〕
如圖1所示，在接合2個被接合體1、2之接合構造中，為適於本發明之第一實施態樣。構成其中一被接合體1材料之大小、構成另一被接合體2材料之大小、其中一金屬體3材料及金屬體之厚度、另一金屬體4材料及金屬體之厚度，係如表1所示。
製作用以形成接合層5之金屬奈米粒子糊。溶劑係使用醚系之萜品醇，並將金屬奈米粒子及其他金屬成分分散於溶劑中。加熱前金屬成分含量如表1所示。金屬成分含量以外的部分，係溶劑及包覆金屬奈米粒子的有機殼。
接合層5方面，係將金屬奈米粒子糊塗布在第1被接合面上，並將第2被接合面披覆在該糊塗布面上，之後以如表1所示之溫度、壓力、保持時間、氣體環境中壓接，進行燒成。
形成接合層5的金屬奈米粒子層中Ni奈米粒子之種類、平均徑、在金屬奈米粒子層全體金屬成分中所占Ni奈米粒子之含量(金屬中含量)、金屬奈米粒子層中Ni奈米粒子以外的金屬成分(其他金屬成分)、加熱前金屬奈米粒子糊中金屬成分含量(加熱前金屬成分含量)、加熱結束之接合後接合層厚度如表1所示。金屬奈米粒子之平均徑係以TEM觀察測定。同時，加熱結束之接合後接合層中，金屬成分含量均為50體積%以上，金屬成分以外的大部分，為溶劑與金屬奈米粒子之有機殼經過加熱之碳化殘渣。
之後對上述完成接合之接合體，進行以下之處理。
(1)接合後冷卻為常溫
(2)接合並冷卻為常溫後再於350℃氮氣氣體環境下熱處理1小時並冷卻為常溫
(3)接合並冷卻為常溫後再於400℃氮氣氣體環境下熱處理1小時並冷卻為常溫
就該3種，各測定接合部分之剪切強度(n=10)。其結果如表1所示。
表1之本發明例No.1、2、5、6，金屬奈米粒子層中金屬成分僅含平均徑30、50nm之Ni奈米粒子，金屬體中其中一方或雙方係由Al或Al合金所形成。同時本發明例No.3係Ni奈米粒子同時含Ag奈米粒子之發明例，本發明例No.4係以平均徑30nm及800nm之Ni奈米粒子混合的發明例。在所有之例，接合部分品質之剪切強度，所有接合後當時、350℃加熱後、400℃加熱後，均有25MPa以上的良好之強度。
另一方面，比較例No.1、2，金屬奈米粒子層中並不含Ni奈米粒子，僅含Ag奈米粒子。比較例No.1係雙方之金屬體均為Al。接合後當時之剪切強度為13MPa之低值，對350℃加熱後、400℃加熱後幾乎未能獲得剪切強度。比較例No.2之金屬體為Ag，該點係在本發明之外。
比較例No.3，與本發明不同，係其中一被接合體為Au線，且不使用金屬奈米粒子層，而以超音波接合進行接合之比較例。接合當時之剪切強度良好，但350℃加熱後、400℃加熱後之剪切強度大幅下降。此係由於高溫環境中，接合部分之介金屬化合物相中產生空隙所致。
〔實施例2〕
如圖2所示，以接合2個被接合體1、2之接合構造中，為適於本發明之第二態樣(表1之本發明例1至9)。比較例1中係使用圖1所示之構造。構成被接合體1、2之材料及大小、金屬體3、4之材料及金屬體的厚度如表2所示。
先製作形成第1接合層6、第2接合層8、接合層5之金屬奈米粒子糊。溶劑方面係使用醚系之萜品醇，並將金屬奈米粒子及其他金屬成分分散於溶劑中。加熱前金屬成分含量如表2所示。金屬成分以外的部分，係溶劑及包覆金屬奈米粒子的有機殼。
如圖2所示之接合構造，係以構成其中一被接合體的被接合面(第1被接合面)之金屬體上以金屬奈米粒子糊經過塗刷法(squeegee method)披覆而作為第1接合層。同樣地，以構成另一被接合體的被接合面(第2被接合面)之金屬體上以金屬奈米粒子糊經過塗刷法披覆而作為第2接合層。接著，使第1接合層與第2接合層相對，其間夾著金屬箔，各使第1接合層、金屬箔、第2接合層接觸。如圖1所示對接合層5，以金屬奈米粒子糊塗布在其中一被接合面上，並以另一被接合面披覆在該糊之塗布面上。所有圖1、圖2所示之實施例，均以表2所示之溫度、壓力、保持時間、氣體環境中壓接，進行燒成。
形成第1接合層6、第2接合層8、接合層5的金屬奈米粒子層中金屬奈米粒子之種類、平均徑、在金屬奈米粒子層全體金屬成分中所占之金屬奈米粒子的含量(金屬中含量)、金屬奈米粒子層中金屬奈米粒子以外的金屬成分(其他金屬成分)、加熱結束之接合後接合層厚度、金屬箔層之種類、厚度係如表1所示。金屬奈米粒子之平均徑係以TEM觀察測定。同時，加熱結束之接合後接合層中，金屬成分含量均為50體積%以上，金屬成分以外之大部分，為 溶劑與金屬奈米粒子的有機殼經過加熱之碳化殘渣。
完成接合之接合體，係在接合後冷卻至常溫後，測定剪切強度(n=10)。其結果如表2所示。所有本發明例1至9、比較例1，推想係由於2個被接合體之熱膨脹率不同，在燒結金屬奈米粒子的上述熱處理完成後，回復常溫時之熱收縮量視被接合體而不同，因此接合部分受熱應力所作用。對於比較例1接合後之剪切強度為12MPa以下之低值。此推想係由於在接合後回復為室溫時作用在接合部分之熱應力，在金屬奈米粒子之接合層5生成缺點。相對此本發明例1至9，係在接合構造中設置金屬箔，因此接合後可實現良好之剪切強度。推想應該係由於金屬箔會吸收熱收縮量之差的變形差，因此可防止金屬奈米粒子使接合層生成缺點。本發明例1、2、5、8、9的金屬箔雖使用Al或Al合金箔，但由於金屬奈米粒子層之金屬奈米粒子係使用Ni奈米粒子，因此使接合部分同樣可獲得良好之品質。
〔實施例3〕
係在實施例2完成接合的接合體中，對表2本發明例1至9，在接合後冷卻為常溫之後於300℃之氮氣氣體環境下處理30分鐘以冷卻為常溫後，再測定接合部分之剪切強度。其結果，對接合後當時之剪切強度並未見強度變差。
產業上利用之可能性
因此本發明，由於在異種或同種金屬間之接合中可獲得具有良好接合強度的接合構造體，因此可利用在以電器/電子工業、機械工業為首之所有產業中。

Claims (13)

  1. 一種金屬接合構造，是2個被接合體之各自的被接合面金屬透過含金屬奈米粒子的接合層接合而成；該構造之特徵在於至少其中一被接合體的被接合面金屬為Al或Al合金，且前述金屬奈米粒子為Ni奈米粒子。
  2. 如請求項1之金屬接合構造，其中前述被接合體之中至少其中一被接合面金屬為Al或Al合金，且前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上。
  3. 一種金屬接合方法，是於2個被接合體之各自的被接合面金屬之間形成含金屬奈米粒子的接合層，且加熱後，透過前述接合層接合2個被接合體；該方法之特徵在於至少其中一被接合體的被接合面金屬為Al或Al合金，且前述金屬奈米粒子為Ni奈米粒子，加熱溫度為200℃以上。
  4. 如請求項3之金屬接合方法，其中前述被接合體之中至少其中一被接合面金屬為Al或Al合金，且前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上。
  5. 一種金屬接合構造，是2個被接合體之各自的被接合面金屬透過含金屬奈米粒子的接合層接合而成；該構造之特徵在於前述接合層係依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層而成。
  6. 如請求項5之金屬接合構造，其中當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子，而當前述金 屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子。
  7. 如請求項5之金屬接合構造，其中當前述被接合體之中至少其中一被接合面金屬為Al或Al合金時，前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上，而當至少其中一被接合面金屬為Ag、Au或該等之合金中任一者時，前述接合層所含金屬成分之中由Ag、Au、Cu或Ni中一種以上所構成之金屬奈米粒子之合計為10質量%以上。
  8. 如請求項6之金屬接合構造，其中當前述被接合體之中至少其中一被接合面金屬為Al或Al合金時，前述接合層所含金屬成分之中Ni奈米粒子的含量為10質量%以上，而當至少其中一被接合面金屬為Ag、Au或該等之合金中任一者時，前述接合層所含金屬成分之中由Ag、Au、Cu或Ni中一種以上所構成之金屬奈米粒子之合計為10質量%以上。
  9. 如請求項1、2、5、6、7或8中任一項之金屬接合構造，其中前述被接合體中至少其中一者為被接合面披覆有金屬之Si、SiC或化合物半導體。
  10. 一種金屬接合方法，是在2個被接合體之被接合面金屬之間形成含金屬奈米粒子的接合層，且加熱後，透過前述接合層接合2個被接合體之被接合面金屬；該方法之特徵在於前述接合層係依序形成含金屬奈米粒子的第1 接合層、金屬箔、含金屬奈米粒子的第2接合層而成；且當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子，而當前述金屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子，且加熱溫度為200℃以上。
  11. 如請求項10之金屬接合方法，其中當前述接合層所含金屬箔為Al或Al合金時Ni奈米粒子的含量為10質量%以上，而當金屬箔為Ag、Au或該等之合金中任一者時由Ag、Au、Cu或Ni中一種以上所構成之金屬奈米粒子之合計為10質量%以上。
  12. 一種金屬接合材料，是依序形成含金屬奈米粒子的第1接合層、金屬箔、含金屬奈米粒子的第2接合層而成。
  13. 如請求項12之金屬接合材料，其中當前述金屬箔為Al或Al合金時前述金屬奈米粒子為Ni奈米粒子，而當前述金屬箔為Ag、Au或該等之合金中任一者時前述金屬奈米粒子為由Ag、Au、Cu或Ni中一種以上所構成之奈米粒子。
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