TW201708553A - 半導體裝置用接合線 - Google Patents

半導體裝置用接合線 Download PDF

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Publication number
TW201708553A
TW201708553A TW105137924A TW105137924A TW201708553A TW 201708553 A TW201708553 A TW 201708553A TW 105137924 A TW105137924 A TW 105137924A TW 105137924 A TW105137924 A TW 105137924A TW 201708553 A TW201708553 A TW 201708553A
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TW
Taiwan
Prior art keywords
wire
bonding wire
bonding
mass
core material
Prior art date
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TW105137924A
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English (en)
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TWI618802B (zh
Inventor
Takashi Yamada
Daizo Oda
Teruo Haibara
Ryo Oishi
Kazuyuki Saito
Tomohiro Uno
Original Assignee
Nippon Micrometal Corp
Nippon Steel & Sumikin Materials Co Ltd
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Publication of TW201708553A publication Critical patent/TW201708553A/zh
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Publication of TWI618802B publication Critical patent/TWI618802B/zh

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    • H—ELECTRICITY
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    • H01L24/42—Wire connectors; Manufacturing methods related thereto
    • H01L24/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
    • 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
    • B23K35/0227—Rods, wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
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    • B23K35/24—Selection of soldering or welding materials proper
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    • B23K35/3013—Au as the principal constituent
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    • B23K35/302—Cu as the principal constituent
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    • B32—LAYERED PRODUCTS
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Abstract

本發明之半導體裝置用接合線具有Cu合金芯材、及形成於其表面之Pd被覆層，可同時實現高溫下之球接合部之接合可靠性提高、及耐力比(=最大耐力/0.2%耐力)：1.1~1.6。 藉由使導線中包含賦予高溫環境下之連接可靠性之元素而提高高溫下之球接合部之接合可靠性，進而，藉由於對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，將導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率設為30%以上，且將接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑設為0.9~1.5μm，而將耐力比設為1.6以下。

Description

半導體裝置用接合線
本發明係關於一種用以將半導體元件上之電極與外部引線等電路佈線基板之佈線連接之半導體裝置用接合線。
當前，作為將半導體元件上之電極與外部引線之間接合之半導體裝置用接合線(以下，稱為「接合線」)，主要使用線徑15~50μm左右之細線。接合線之接合方法一般為超音波併用熱壓接方式，可使用通用接合裝置、使接合線通向其內部而用於連接之毛細管治具等。接合線之接合製程係藉由如下方式完成：將導線前端利用電弧輸熱(arc heat)進行加熱熔融，藉由表面張力而形成球(FAB：Free Air Ball，無空氣焊球)後，將該球部對在150~300℃之範圍內加熱過之半導體元件之電極上進行壓接接合(以下，稱為「球接合」)，繼而於形成電路之後，將導線部對外部引線側之電極進行壓接接合(以下，稱為「楔形接合」)。作為接合線之接合對象的半導體元件上之電極可使用在Si基板上成膜以Al為主體之合金所得之電極結構，外部引線側之電極可使用實施過鍍Ag或鍍Pd之電極結構等。
迄今為止，接合線之材料係以Au為主流，但正以LSI(Large Scale Integration，大型積體電路)用途為中心而發展為由Cu替代。另一方面，在近年來之電動汽車或油電混合車普及之背景下，於車載用器件用中途，對自Au代替為Cu之需求亦正在升高。
關於Cu接合線，提出有使用高純度Cu(純度：99.99質量%以上) 者(例如，專利文獻1)。Cu有比Au容易氧化之缺點，存在接合可靠性、球形成性、楔形接合性等較差之問題。作為防止Cu接合線之表面氧化之方法，提出有以Au、Ag、Pt、Pd、Ni、Co、Cr、Ti等金屬被覆Cu芯材之表面之結構(專利文獻2)。又，提出有於Cu芯材之表面被覆Pd、並以Au、Ag、Cu或該等之合金被覆其表面之結構(專利文獻3)。
[先前技術文獻] [專利文獻]
[專利文獻1]日本專利特開昭61-48543號公報
[專利文獻2]日本專利特開2005-167020號公報
[專利文獻3]日本專利特開2012-36490號公報
車載用器件與一般之電子機器相比，要求嚴酷之高溫高濕環境下之接合可靠性。尤其是將導線之球部接合於電極而成之球接合部之接合壽命成為最大問題。
作為對高溫高濕環境下之球接合部之接合可靠性進行評價之代表性之評價方法，存在HAST(Highly Accelerated Temperature and Humidity Stress Test，高溫高濕環境暴露試驗)。於利用HAST對球接合部之接合可靠性進行評價之情形時，將評價用之球接合部暴露於溫度為130℃、相對濕度為85%之高溫高濕環境中，測定接合部之電阻值之經時變化，或測定球接合部之抗剪強度(shear strength)之經時變化，藉此評價球接合部之接合壽命。
又，作為對170℃以上之高溫環境下之球接合部之接合可靠性進行評價之方法，使用HTS(High Temperature Storage Test，高溫放置試驗)。於利用HTS對球接合部之接合可靠性進行評價之情形時，對暴 露於高溫環境中之評價用之樣品測定球接合部之電阻值之經時變化，或測定球接合部之抗剪強度之經時變化，藉此評價球接合部之接合壽命。
根據本發明者等人之研究，判明：於接合線包含例如Ni、Zn、Rh、In、Ir、Pt等賦予高溫環境下之連接可靠性之元素之情形時，與不含該元素者相比，130℃以上之高溫環境下之球接合部之接合可靠性提高。
此處，由下述(1)式定義耐力比。
耐力比=最大耐力/0.2%耐力 (1)
於楔形接合中，接合線嚴重變形。若於變形時導線產生加工硬化，則接合後之導線變硬，其結果為，楔形接合之接合強度降低。為了維持楔形接合強度，由上述(1)式定義之耐力比較佳為1.6以下。但是，於為了提高高溫環境下之球接合部之接合可靠性而使導線中含有上述元素時，耐力比增大並超過1.6。因此，引起楔形接合之接合強度降低。
本發明之目的在於提供一種半導體裝置用接合線，其係具有Cu合金芯材與形成於其表面之Pd被覆層者，可提高高溫下之球接合部之接合可靠性，並且可使由(1)式定義之耐力比為1.1~1.6。
即，本發明之主旨係如下所述。
[1]一種半導體裝置用接合線，其係具有Cu合金芯材、及形成於上述Cu合金芯材之表面之Pd被覆層者，且其特徵在於：上述接合線包含賦予高溫環境下之連接可靠性之元素，於對上述接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，導線長度方向(導線軸方向)之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率為30%以上，且上述接合線之垂直於導 線軸之方向之芯材剖面中之平均結晶粒徑為0.9~1.5μm。
[2]如上述[1]記載之半導體裝置用接合線，其特徵在於：由下述(1)式定義之耐力比為1.1~1.6。
耐力比=最大耐力/0.2%耐力 (1)
[3]如上述[1]或[2]記載之半導體裝置用接合線，其特徵在於：上述Pd被覆層之厚度為0.015~0.150μm。
[4]如上述[1]至[3]中任一項記載之半導體裝置用接合線，其特徵在於：於上述Pd被覆層上進而具有包含Au與Pd之合金表皮層。
[5]如上述[4]記載之半導體裝置用接合線，其特徵在於：上述包含Au與Pd之合金表皮層之厚度為0.050μm以下。
[6]如上述[1]至[5]中任一項記載之半導體裝置用接合線，其特徵在於：上述接合線包含選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素，且上述元素相對於導線整體之濃度總計為0.011~2質量%。
[7]如上述[1]至[6]中任一項記載之半導體裝置用接合線，其特徵在於：上述接合線包含選自Ga、Ge之1種以上之元素，且上述元素相對於導線整體之濃度合計為0.011~1.5質量%。
[8]如上述[1]至[7]中任一項記載之半導體裝置用接合線，其特徵在於：上述接合線包含選自As、Te、Sn、Sb、Bi、Se之1種以上之元素，上述元素相對於導線整體之濃度合計為0.1~100質量ppm，且Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm。
[9]如上述[1]至[8]中任一項記載之半導體裝置用接合線，其特徵在於：上述接合線進而包含選自B、P、Mg、Ca、La之至少1種以上之元素，且上述元素相對於導線整體之濃度分別為1~200質量ppm。
[10]如上述[1]至[9]中任一項記載之半導體裝置用接合線，其特徵在於：於上述接合線之最表面存在Cu。
[11]如上述[1]至[10]中任一項記載之半導體裝置用接合線，其特 徵在於：Cu合金芯材含有總計0.1~3.0質量%之元素週期表第10族之金屬元素，且導線最表面之Cu濃度為1原子%以上。
根據本發明，可提高高溫環境下之球接合部之接合可靠性，且可使由(1)式定義之耐力比為1.1~1.6。
本發明之半導體裝置用接合線具有Cu合金芯材、及形成於上述Cu合金芯材之表面之Pd被覆層。於本發明中，接合線包含賦予高溫環境下之連接可靠性之元素，於對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率為30%以上，且接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑為0.9~1.5μm。
關於作為半導體裝置之封裝體的塑模樹脂(環氧樹脂)，於分子骨架中包含氯(Cl)。於作為HAST評價條件之130℃、相對濕度85%之高溫高濕環境下，分子骨架中之Cl會水解而以氯化物離子(Cl-)之形式溶出。於將不具Pd被覆層之Cu接合線接合於Al電極之情形時，若將Cu/Al接合界面置於高溫下，則Cu與Al會相互擴散，最終形成作為金屬間化合物之Cu9Al4。Cu9Al4容易受到Cl等鹵素所致之腐蝕，因自塑模樹脂溶出之Cl而進行腐蝕，導致接合可靠性降低。於Cu導線具有Pd被覆層之情形時，Pd被覆Cu導線與Al電極之接合界面成為Cu/Pd濃化層/Al之結構，故而，與不具Pd被覆層之Cu導線相比，Cu9Al4金屬間化合物之生成得到抑制，但是，車載用器件所要求之高溫高濕環境下之接合可靠性不充分。
對此，認為：若如本發明般含有賦予高溫環境下之連接可靠性之元素，則有接合部中之Cu9Al4金屬間化合物之生成進一步得到抑制之傾向。
就改善球接合部之高溫環境下之接合可靠性(尤其是175℃以上之HTS中之成績)之觀點而言，賦予高溫環境下之連接可靠性之元素相對於導線整體之濃度總計較佳為0.011質量%以上，更佳為0.030質量%以上，進而較佳為0.050質量%以上、0.070質量%以上、0.09質量%以上、0.10質量%以上、0.15質量%以上、或0.20質量%以上。下文對賦予高溫環境下之連接可靠性之元素詳細地進行說明。
如上所述，由下述(1)式定義耐力比。
耐力比=最大耐力/0.2%耐力 (1)
於楔形接合中，接合線嚴重變形。若於變形時導線產生加工硬化，則接合後之導線變硬，其結果為，楔形接合之接合強度降低。為了維持良好之楔形接合強度，由上述(1)式定義之耐力比較佳為1.6以下。但是，於為了提高高溫環境下之球接合部之接合可靠性而含有可充分地發揮效果之量之賦予高溫環境下之連接可靠性之元素時，耐力比增大並超過1.6。認為使芯材之Cu中含有上述元素之結果為產生耐力比之增大、即硬度之增加。因此，導致楔形接合之接合強度降低。另一方面，於欲在先前之製造方法之範圍內降低耐力比時，結果耐力比未達1.1，楔形接合性較差。
於是，對接合線即便含有上述賦予高溫環境下之連接可靠性之元素亦可將(1)式之耐力比保持於1.1~1.6之較佳範圍內的結晶組織進行研究。其結果發現：於將(1)式之耐力比保持於較佳範圍內時，重要的是控制接合線中之芯材之結晶結構，尤其是(i)對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100 >之方位比率(以下，亦簡稱為「<100>方位比率」)；及(ii)接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑(以下，亦簡稱為「平均結晶粒徑」)。詳細而言，得知若利用通常之製造方法製造接合線，則無法同時實現<100>方位比率為30%以上、及平均結晶粒徑為0.9μm以上且1.5μm以下，其結果為耐力比未達1.1或超過1.6。可知與此相對，藉由如下所述般設計製造方法，可使接合線之垂直於導線軸之方向之芯材剖面中之導線長度方向之結晶方位中，包括相對於導線長度方向之角度差為15度以內為止之<100>之方位比率為30%以上，使接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑為0.9~1.5μm，其結果為可使(1)式之耐力比為1.1~1.6。
<100>方位比率為30%以上時，與楔形接合時之變形相伴之導線之加工硬化較小，故而可使耐力比為1.6以下。然而，即便於此情形時，平均結晶粒徑未達0.9μm時，0.2%耐力亦較高(缺乏延展性)，故而耐力比未達1.1，而楔形接合性較差。於平均結晶粒徑超過1.5μm之情形時，<100>方位比率未達30%，進而0.2%耐力較低，故而可推斷耐力比超過1.6，而楔形接合性較差。
再者，即便於導線之結晶結構滿足上述條件之情形時，若導線中之賦予高溫環境下之連接可靠性之元素之含量過多，則亦有耐力比增大之情形。就實現耐力比為1.6以下，抑制接合線之硬質化而抑制楔形接合性之降低之觀點而言，賦予高溫環境下之連接可靠性之元素相對於導線整體之濃度總計較佳為2.0質量%以下、1.8質量%以下、或1.6質量%以下。
於使接合線中含有賦予高溫環境下之連接可靠性之元素時，採用使Cu芯材中含有該等元素之方法、使該等元素覆著於Cu芯材或導線表面而含有之方法之任一者均可發揮上述本發明之效果。該等成分之添加量極微量，故而添加方法之變化範圍廣泛，無論用何種方法進 行添加，只要包含該成分，便顯現效果。
於本發明之接合線中，Pd被覆層之厚度就獲得良好之FAB形狀之觀點、及進一步改善車載用器件所要求之高溫高濕環境下之球接合部之接合可靠性之觀點而言，較佳為0.015μm以上，更佳為0.02μm以上，進而較佳為0.025μm以上、0.03μm以上、0.035μm以上、0.04μm以上、0.045μm以上、或0.05μm以上。另一方面，若Pd被覆層之厚度過厚，則FAB形狀亦會降低，故而Pd被覆層之厚度較佳為0.150μm以下，更佳為0.140μm以下、0.130μm以下、0.120μm以下、0.110μm以下、或0.100μm以下。
對上述接合線之Cu合金芯材、Pd被覆層之定義進行說明。Cu合金芯材與Pd被覆層之邊界係以Pd濃度為基準進行判定。將Pd濃度為50原子%之位置設為邊界，將Pd濃度為50原子%以上之區域判定為Pd被覆層，將Pd濃度未達50原子%之區域判定為Cu合金芯材。該根據之原因在於：於Pd被覆層中，若Pd濃度為50原子%以上，則可自Pd被覆層之結構獲得特性之改善效果。Pd被覆層可包含Pd單層之區域、及Pd與Cu於導線之深度方向具有濃度梯度之區域。於Pd被覆層中，形成該具有濃度梯度之區域之原因為存在Pd與Cu之原子因製造步驟中之熱處理等而擴散之情況。於本發明中，所謂濃度梯度，係指濃度向深度方向變化之程度於每0.1μm為10mol%以上。進而，Pd被覆層亦可包含不可避免之雜質。
於本發明之接合線中，Pd被覆層中之Pd之最大濃度就可進一步享有本發明之效果之觀點而言，較佳為60原子%以上，更佳為70原子%以上、80原子%以上、或90原子%以上。Pd被覆層中之Pd之最大濃度較佳為100原子%，但於本發明之接合線中，即便於Pd被覆層中之Pd之最大濃度未達100原子%、例如為99.9原子%以下、99.8原子%以下、99.7原子%以下、99.6原子%以下、99.5原子%以下、99.0原子% 以下、98.5原子%以下、98原子%以下、97原子%以下、96原子%以下、或95原子%以下之情形時，亦可達成所期待之效果。
於本發明之接合線中，Pd被覆層中之Pd濃度為99.0原子%以上之區域之厚度可為40nm以下，例如亦可為35nm以下、30nm以下、25nm以下、20nm以下、15nm以下、10nm以下、或5nm以下。
本發明之接合線亦可於Pd被覆層之表面進而具有包含Au與Pd之合金表皮層。藉此，本發明之接合線可進一步提高接合可靠性，並且可進而改善楔形接合性。
對上述接合線之包含Au與Pd之合金表皮層之定義進行說明。包含Au與Pd之合金表皮層與Pd被覆層之邊界係以Au濃度為基準進行判定。將Au濃度為10原子%之位置設為邊界，將Au濃度為10原子%以上之區域判定為包含Au與Pd之合金表皮層，將未達10原子%之區域判定為Pd被覆層。又，即便為Pd濃度為50原子%以上之區域，只要Au存在10原子%以上，則判定為包含Au與Pd之合金表皮層。該等根據之原因在於：若Au濃度為上述之濃度範圍，則可自Au表皮層之結構期待特性之改善效果。包含Au與Pd之合金表皮層為Au-Pd合金，將其設為包含Au與Pd於導線之深度方向具有濃度梯度之區域的區域。於包含Au與Pd之合金表皮層中，形成該具有濃度梯度之區域之原因為Au與Pd之原子因製造步驟中之熱處理等而擴散。進而，包含Au與Pd之合金表皮層亦可包含不可避免之雜質與Cu。
於本發明之接合線中，包含Au與Pd之合金表皮層可與Pd被覆層反應而提高包含Au與Pd之合金表皮層、Pd被覆層、Cu合金芯材之間之密接強度，抑制楔形接合時之Pd被覆層或包含Au與Pd之合金表皮層之剝離。藉此，本發明之接合線可進而改善楔形接合性。就獲得良好之楔形接合性之觀點而言，包含Au與Pd之合金表皮層之厚度較佳為0.0005μm以上，更佳為0.001μm以上、0.002μm以上、或0.003μm 以上。就抑制偏芯而獲得良好之FAB形狀之觀點而言，包含Au與Pd之合金表皮層之厚度較佳為0.050μm以下，更佳為0.045μm以下、0.040μm以下、0.035μm以下、或0.030μm以下。再者，包含Au與Pd之合金表皮層可藉由與Pd被覆層相同之方法而形成。
於本發明中，作為賦予高溫環境下之連接可靠性之元素，例如可列舉元素週期表第9族之元素(Co、Rh、Ir)、元素週期表第10族之元素(Ni、Pd、Pt)、元素週期表第11族之元素(Ag、Au等)、元素週期表第12族之元素(Zn等)、元素週期表第13族之元素(Al、Ga、In等)、元素週期表第14族之元素(Ge、Sn等)、元素週期表第15族之元素(P、As、Sb、Bi等)、元素週期表第16族之元素(Se、Te等)等。該等元素可以單獨一種、或組合兩種以上而含於接合線中。
於本發明中，接合線較佳為包含選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素作為賦予高溫環境下之連接可靠性之元素。該等元素相對於導線整體之濃度總計較佳為0.011~2質量%。
於作為半導體裝置之封裝體之塑模樹脂(環氧樹脂)中，包含矽烷偶合劑。矽烷偶合劑具有提高有機物(樹脂)與無機物(矽或金屬)之密接性之作用，故而可提高與矽基板或金屬之密接性。進而，於要求更高溫下之可靠性之面向車載之半導體等要求較高之密接性之情形時，添加「含硫之矽烷偶合劑」。塑模樹脂所包含之硫一旦於175℃以上(例如，175℃~200℃)之條件下使用，則會游離。而且，若於175℃以上之高溫下游離之硫與Cu接觸，則Cu之腐蝕變激烈，而生成硫化物(Cu2S)或氧化物(CuO)。若於使用有Cu接合線之半導體裝置中產生Cu之腐蝕，則尤其會導致球接合部之接合可靠性降低。
於是，藉由使接合線包含選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素，且將上述元素相對於導線整體之濃度設為總計0.011~2質量%，可提高高溫環境下之接合可靠性(尤其是175℃以上之HTS 中之成績)。就改善球接合部之高溫環境下之接合可靠性(尤其是175℃以上之HTS中之成績)之觀點而言，上述元素相對於導線整體之濃度總計較佳為0.011質量%以上，更佳為0.050質量%以上，進而較佳為0.070質量%以上、0.090質量%以上、0.10質量%以上、0.15質量%以上、或0.20質量%以上。於以下說明中，亦將選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素稱為「元素MA」。
於本發明中，接合線較佳為包含選自Ga、Ge之1種以上之元素作為賦予高溫環境下之連接可靠性之元素，且上述元素相對於導線整體之濃度合計為0.011~1.5質量%。再者，選自Ga、Ge之1種以上之元素可代替元素MA、或與元素MA一併含於導線中。於以下說明中，亦將選自Ga、Ge之1種以上之元素稱為「元素MB」。
於形成球接合部之FAB時，導線中之Ga、Ge亦擴散至Pd被覆層。認為球接合部中之Cu與Al界面之Pd濃化層中存在之Ga、Ge會進一步提高由Pd濃化層帶來之Cu與Al之相互擴散抑制效果，結果，抑制容易於高溫高濕環境下腐蝕之Cu9Al4之生成。又，亦有導線所包含之Ga、Ge具有直接阻礙Cu9Al4之形成之效果之可能性。
進而，使用含有特定量之選自Ga、Ge之至少1種以上之Pd被覆Cu接合線形成球部，利用掃描式電子顯微鏡(SEM：Scanning Electron Microscope)對FAB進行觀察，結果於FAB之表面觀察到大量直徑數十nm 左右之析出物。若利用能量分散型X射線分析(EDS：Energy Dispersive X-ray Spectroscopy)對析出物進行分析，則確認到Ga、Ge濃化。根據如上之情況，認為藉由FAB上所觀察到之該析出物存在於球部與電極之接合界面，溫度為130℃、相對濕度為85%之高溫高濕環境下之球接合部之接合可靠性顯著提高，但詳細之機制並不明確。
作為Ga、Ge之存在部位，較佳為Cu合金芯材中，但藉由包含於Pd被覆層、或下述之包含Au與Pd之合金表皮層，亦可獲得充分之作 用效果。向Cu合金芯材中添加Ga、Ge之方法容易進行準確之濃度管理，導線生產性、品質穩定性提高。又，藉由Ga、Ge之一部分因熱處理所引起之擴散等而亦含於Pd被覆層或合金表皮層，各層界面之密接性優化，亦能夠進一步提高導線生產性。
另一方面，就獲得良好之FAB形狀之觀點、抑制接合線之硬質化而獲得良好之楔形接合性之觀點而言，Ga、Ge相對於導線整體之濃度合計為1.5質量%以下，較佳為1.4質量%以下，更佳為1.3質量%以下、或1.2質量%以下。
於本發明中，接合線較佳為包含選自As、Te、Sn、Sb、Bi、Se之1種以上之元素，上述元素相對於導線整體之濃度合計為0.1~100質量ppm，且Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm。再者，選自As、Te、Sn、Sb、Bi、Se之1種以上之元素可代替元素MA及/或元素MB、或與元素MA及/或元素MB一併含於導線中。於以下說明中，亦將選自As、Te、Sn、Sb、Bi、Se之1種以上之元素稱為「元素MC」。
若接合線包含選自As、Te、Sn、Sb、Bi、Se之至少1種以上之元素，上述元素相對於導線整體之濃度合計為0.1~100質量ppm，且Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm，則可進一步改善車載用器件所要求之高溫高濕環境下之球接合部之接合可靠性。尤其是可提高溫度為130℃、相對濕度為85%之高溫高濕環境下之球接合部之接合壽命而改善接合可靠性，故而較佳。上述元素相對於導線整體之濃度合計較佳為0.1質量ppm以上，更佳為0.5質量ppm以上，進而較佳為1質量ppm以上，進而更佳為1.5質量ppm以上、2質量ppm以上、2.5質量ppm以上、或3質量ppm以上。另一方面，就獲得良好之FAB形狀之觀點而言，上述元素相對於導線整體之濃度合計較佳為100質量ppm以下，更佳為95質量ppm以下、90質量ppm以下、85質量ppm以 下、或80質量ppm以下。又，於Sn濃度、Sb濃度超過10質量ppm之情形時，或於Bi濃度超過1質量ppm之情形時，FAB形狀不良，因此藉由設為Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm，可進一步改善FAB形狀，故而較佳。
本發明之接合線較佳為進而包含選自B、P、Mg、Ca、La之至少1種以上之元素，且上述元素相對於導線整體之濃度分別為1~200質量ppm。藉此，可改善高密度安裝所要求之球接合部之壓扁形狀，即改善球接合部形狀之真圓性。上述元素相對於導線整體之濃度分別較佳為1質量ppm以上，更佳為2質量ppm以上、3質量ppm以上、4質量ppm以上、或5質量ppm以上。就抑制球之硬質化而抑制球接合時之晶片損傷(chip damage)之觀點而言，上述元素相對於導線整體之濃度分別較佳為200質量ppm以下，更佳為150質量ppm以下、120質量ppm以下、100質量ppm以下、95質量ppm以下、90質量ppm以下、85質量ppm以下、或80質量ppm以下。
於如本發明般Pd被覆Cu接合線含有提高高溫環境下之連接可靠性之元素之情形時，若進而於接合線之最表面存在Cu，則有接合部中之Cu9Al4金屬間化合物之生成進一步得到抑制之傾向。於Pd被覆Cu接合線含有提高高溫環境下之連接可靠性之元素之情形時，若進而於接合線之最表面存在Cu，則藉由接合線所包含之上述元素與Cu之相互作用，而於FAB形成時促進FAB表面之Pd濃化，球接合界面之Pd濃化更顯著地顯現。可推斷藉此由Pd濃化層帶來之Cu與Al之相互擴散抑制效果進而變強，容易因Cl之作用而腐蝕之Cu9Al4之生成量變少，球接合部之高溫高濕環境下之接合可靠性進一步提高。
於在Pd被覆層之最表面存在Cu之情形時，若Cu之濃度為30原子%以上，則存在導線表面之耐硫化性降低，接合線之使用壽命降低，故而不適於實用之情況。因此，於在Pd被覆層之最表面存在Cu之情 形時，Cu之濃度較佳為未達30原子%。
又，於在Au表皮層之最表面存在Cu之情形時，若Cu之濃度為35原子%以上，則存在導線表面之耐硫化性降低，接合線之使用壽命降低，故而不適於實用之情況。因此，於在Au表皮層之最表面存在Cu之情形時，Cu之濃度較佳為未達35原子%。
此處，所謂最表面，係指在不實施濺射等之狀態下，藉由歐傑電子光譜裝置對接合線之表面進行測定之區域。
於本發明中，較佳為Cu合金芯材含有總計0.1~3.0質量%之元素週期表第10族之金屬元素，且導線最表面之Cu濃度為1~10原子%。若設為此種構成，則可進一步改善對於鍍Pd之引線框架或Pd鍍層上實施有鍍Au之引線框架之楔形接合性。又，藉由使Cu合金芯材中含有特定量之元素週期表第10族之金屬元素，接合線與電極之間之球接合部即便於高濕加熱條件下，亦可實現優異之球接合性。
作為Cu合金芯材中之元素週期表第10族之金屬元素，較佳為選自由Ni、Pd及Pt所組成之群中之1種以上。於較佳之一實施形態中，Cu合金芯材包含Ni作為元素週期表第10族之金屬元素。例如，Cu合金芯材中，作為元素週期表第10族之金屬元素，可單獨含有Ni，亦可將Ni與Pd、Pt之一者或兩者組合含有。於另一較佳之一實施形態中，Cu合金芯材包含Pd、Pt之一者或兩者作為元素週期表第10族之金屬元素。
若Cu合金芯材中之元素週期表第10族之金屬元素之濃度總計為0.1質量%以上，則可充分地控制接合界面中之Cu、Al之相互擴散，即便於作為嚴酷之高濕加熱評價試驗之HAST試驗中，接合部之壽命亦提高至380小時以上。作為此處之接合部之評價，於HAST試驗後將樹脂開封並去除，其後，藉由拉力試驗對接合部之斷裂情況進行評價。就充分地獲得上述HAST試驗可靠性之改善效果之觀點而言，Cu 合金芯材中之元素週期表第10族之金屬元素之濃度總計為0.1質量%以上，較佳為0.2質量%以上，更佳為0.3質量%以上、0.4質量%以上、0.5質量%以上、或0.6質量%以上。又，就獲得低溫接合下與Al電極之初始接合強度良好且HAST試驗中之長期可靠性、或向BGA(Ball Grid Array，球柵陣列)、CSP(Chip Size Package，晶片尺寸封裝)等基板、帶材等之接合之量產裕度優異之接合線之觀點、減少晶片損傷之觀點而言，Cu合金芯材中之元素週期表第10族之金屬元素之濃度總計為3.0質量%以下，較佳為2.5質量%以下、或2.0質量%以下。若Cu合金芯材中之元素週期表第10族之金屬元素之濃度總計超過3.0質量%，則必須以低負荷進行球接合，以避免產生晶片損傷，而與電極之初始接合強度降低，結果，存在HAST試驗可靠性變差之情況。本發明之接合線中，藉由將Cu合金芯材中之元素週期表第10族之金屬元素之總計濃度設為上述較佳之範圍內，HAST試驗中之可靠性進一步提高。例如，可實現HAST試驗之至產生不良之壽命超過450小時之接合線。其亦存在相當於先前之Cu接合線之1.5倍以上之長壽命化之情形，亦可應對嚴酷之環境下之使用。
再者，作為自接合線製品求出Cu合金芯材所包含之上述元素之濃度之方法，例如可列舉：使接合線之剖面露出而對Cu合金芯材之區域進行濃度分析之方法；一面利用濺射等自接合線之表面朝向深度方向進行切削，一面對Cu合金芯材之區域進行濃度分析之方法。例如，於Cu合金芯材包含具有Pd之濃度梯度之區域之情形時，只要對接合線之剖面進行線分析，對不具Pd之濃度梯度之區域(例如，Pd之濃度向深度方向變化之程度於每0.1μm未達10mol%之區域、Cu合金芯材之軸心部)進行濃度分析即可。
於本發明之接合線中，藉由使用含有特定量之元素週期表第10族之金屬元素之Cu合金芯材，且將導線最表面之Cu濃度設為1原子% 以上，可大幅改善對於鍍Pd之引線框架之楔形接合性、尤其是剝離性，並且可實現良好之楔形接合性與FAB形狀，可抑制導線表面之氧化而抑制品質之經時劣化。就可進一步改善楔形接合性之觀點而言，於本發明之接合線中，導線最表面之Cu濃度較佳為1.5原子%以上，更佳為2原子%以上、2.5原子%以上、或3原子%以上。導線最表面之Cu濃度之上限如上所述，就實現良好之楔形接合性與FAB形狀之觀點、抑制導線表面之氧化而抑制品質之經時劣化之觀點而言，於包含含有特定量之元素週期表第10族之金屬元素之Cu合金芯材的本發明之接合線中，導線最表面之Cu濃度較佳為10原子%以下，更佳為9.5原子%以下、或9原子%以下。
對於Pd被覆層、包含Au與Pd之合金表皮層之濃度分析，一面利用濺射等自接合線之表面朝向深度方向進行切削一面進行分析之方法、或使導線剖面露出而進行線分析、點分析等之方法較為有效。該等濃度分析所使用之解析裝置可利用掃描式電子顯微鏡或穿透式電子顯微鏡所配備之歐傑電子光譜分析裝置、能量分散型X射線分析裝置、電子探針微量分析器等。作為使導線剖面露出之方法，可利用機械研磨、離子蝕刻法等。關於接合線中之Ni、Zn、Rh、In、Ir、Pt等微量元素之分析，可利用ICP(inductively coupled plasma，感應耦合電漿)發射光譜分析裝置或ICP質譜分析裝置對將接合線用強酸溶解而成之液體進行分析，以接合線整體所包含之元素之濃度之形式進行檢測。
(製造方法)
繼而，對本發明之實施形態之接合線之製造方法進行說明。接合線係藉由如下方式而獲得：於製造用於芯材之Cu合金之後，加工成較細之線狀，形成Pd被覆層、Au層，並進行熱處理。亦存在形成Pd被覆層、Au層之後，再次進行拉線(wire drawing)與熱處理之情 況。對Cu合金芯材之製造方法、Pd被覆層、包含Au與Pd之合金表皮層之形成方法、熱處理方法詳細地進行說明。
芯材所使用之Cu合金係藉由將成為原料之Cu與添加之元素一起熔解，並使之凝固而獲得。熔解可利用電弧加熱爐、高頻加熱爐、電阻加熱爐等。為了防止來自大氣中之O2、H2等氣體之混入，較佳為於真空氛圍或Ar或N2等惰性氛圍中進行熔解。
於Cu合金芯材之表面形成Pd被覆層、Au層之方法有鍍敷法、蒸鍍法、熔融法等。鍍敷法可應用電解鍍敷法、無電鍍敷法之任一者。於稱作衝擊電鍍(strike plating)、閃熔電鍍(flash plating)之電解鍍敷中，鍍敷速度較快，與基材之密接性亦良好。無電鍍敷所使用之溶液分為置換型與還原型，於厚度較薄之情形時，僅利用置換型鍍敷鍍便足夠，但於厚度較厚之情形時，有效的是在置換型鍍敷之後階段性地實施還原型電鍍。
於蒸鍍法中，可利用濺射法、離子鍍覆法、真空蒸鍍等物理吸附、及電漿CVD(Chemical Vapor Deposition，化學氣相沈積)等化學吸附。均為乾式，無需形成Pd被覆層、Au層後洗淨，無需擔憂洗淨時之表面污染等。
藉由於形成Pd被覆層、Au層後進行熱處理，Pd被覆層之Pd擴散至Au層中，形成包含Au與Pd之合金表皮層。亦可並非於形成Au層之後藉由熱處理形成包含Au與Pd之合金表皮層，而從最初開始便覆著包含Au與Pd之合金表皮層。
針對Pd被覆層、包含Au與Pd之合金表皮層之形成，於拉線至最終線徑後形成之方法、於形成於粗徑之Cu合金芯材上之後進行複數次拉線直至成為目標線徑之方法之任一者均有效。於前者之以最終線徑形成Pd被覆層、包含Au與Pd之合金表皮層之情形時，製造、品質管理等較為簡便。於後者之將Pd被覆層、包含Au與Pd之合金表皮層 與拉線組合之情形時，就與Cu合金芯材之密接性提高方面而言較為有利。作為各個形成法之具體例，可列舉：一面於電解鍍敷溶液中連續地掃動導線一面於最終線徑之Cu合金芯材形成Pd被覆層、包含Au與Pd之合金表皮層之方法；或於將較粗之Cu合金芯材浸漬於電解鍍浴或無電鍍浴中形成Pd被覆層、包含Au與Pd之合金表皮層之後對導線進行拉伸達到最終線徑之方法等。
於形成Pd被覆層、包含Au與Pd之合金表皮層之後，存在進行熱處理之情況。藉由進行熱處理，於包含Au與Pd之合金表皮層、Pd被覆層、Cu合金芯材之間，原子擴散而提高密接強度，故而可抑制加工中包含Au與Pd之合金表皮層或Pd被覆層之剝離，就生產性提高方面而言有效。為了防止來自大氣中之O2之混入，較佳為於真空氛圍或Ar或N2等惰性氛圍中進行熱處理。
藉由如上所述般調整對接合線實施之擴散熱處理或退火熱處理之條件，芯材之Cu藉由晶界擴散、晶內擴散等而於Pd被覆層或包含Au與Pd之表皮合金層中擴散，使Cu到達至接合線之最表面，而可使最表面存在Cu。作為用以使最表面存在Cu之熱處理，可使用如上所述用以形成包含Au與Pd之合金表皮層之熱處理。於進行用以形成合金表皮層之熱處理時，藉由選擇熱處理溫度與時間，可使最表面存在Cu、或不存在Cu。進而，亦可將最表面之Cu濃度調整為特定之範圍(例如，1~50原子%之範圍)。亦可藉由除形成合金表皮層時以外進行之熱處理使Cu擴散至最表面。
如上所述，於使接合線中含有賦予高溫環境下之連接可靠性之元素時，採用使Cu芯材中含有該等元素之方法、使該等元素覆著於Cu芯材或導線表面而含有之方法之任一者均可發揮上述本發明之效果。關於B、P、Mg、Ca、La，亦相同。
作為上述成分之添加方法，最簡便之方法為添加至Cu合金芯材 之起始材料。例如，將高純度之銅與上述成分元素原料作為起始原料進行稱量後，將其於高真空下或氮氣或氬氣等惰性氛圍下加熱而熔解，藉此製成添加有目標濃度範圍之上述成分之錠，設為包含目標濃度之上述成分元素之起始材料。因此，於較佳之一實施形態中，本發明之接合線之Cu合金芯材係以選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素相對於導線整體之濃度總計為0.011~2質量%之方式包含上述元素。該濃度之合計之較佳之數值範圍如上所述。於另一較佳之一實施形態中，本發明之接合線之Cu合金芯材係以選自Ga、Ge之1種以上之元素相對於導線整體之濃度總計為0.011~1.5質量%之方式包含上述元素。該濃度之合計之較佳之數值範圍如上所述。於另一較佳之一實施形態中，本發明之接合線之Cu合金芯材係以選自As、Te、Sn、Sb、Bi、Se之至少1種以上之元素相對於導線整體之濃度合計為0.1~100質量ppm、且Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm之方式包含上述元素。該濃度之較佳之數值範圍如上所述。於較佳之一實施形態中，Cu合金芯材之Cu之純度為3N以下(較佳為2N以下)。於先前之Pd被覆Cu接合線中，就黏結性(bondability)之觀點而言，有使用高純度(4N以上)之Cu芯材而避免使用低純度之Cu芯材之傾向。含有特定元素之本發明之接合線於如上所述般使用Cu之純度較低之Cu合金芯材之情形時，尤佳地實現車載用器件所要求之高溫高濕環境下之球接合部之接合可靠性。於另一較佳之一實施形態中，本發明之接合線之Cu合金芯材係以選自B、P、Mg、Ca、La之至少1種以上之元素相對於導線整體之濃度分別為1~200質量ppm之方式包含上述元素。該濃度之較佳之數值範圍如上所述。於另一較佳之一實施形態中，本發明之接合線之Cu合金芯材係以總計為0.1~3.0質量%之方式包含元素週期表第10族之金屬元素。該濃度之較佳之數值範圍如上所述。
亦可藉由於導線製造步驟之中途使上述成分覆著於導線表面而含有。於此情形時，組入至導線製造步驟之何處均可，亦可反覆進行複數次。亦可組入至複數個步驟。可向Pd被覆前之Cu表面添加，可向Pd被覆後之Pd表面添加，可向Au被覆後之Au表面添加，亦可組入至各被覆步驟。作為覆著方法，可自(1)水溶液之塗佈乾燥熱處理、(2)鍍敷法(濕式)、(3)蒸鍍法(乾式)中選擇。
於採用水溶液之塗佈乾燥熱處理之方法之情形時，首先，利用包含上述成分元素之水溶性之化合物製備適當濃度之水溶液。藉此，可將上述成分納入至導線材料中。組入至導線製造步驟之何處均可，亦可反覆進行複數次。亦可組入至複數個步驟。可向Pd被覆前之Cu表面添加，可向Pd被覆後之Pd表面添加，可向Au被覆後之Au表面添加，亦可組入至各被覆步驟。
於使用鍍敷法(濕式)之情形時，鍍敷法可應用電解鍍敷法、無電鍍敷法之任一者。於電解鍍敷法中，除通常之電解鍍敷以外，亦可應用被稱作閃熔電鍍之鍍敷速度較快、與基材之密接性亦良好之鍍敷法。無電鍍敷所使用之溶液有置換型與還原型。通常於鍍層厚度較薄之情形時應用置換型鍍敷，於較厚之情形時應用還原型鍍敷，可應用任一者，只要按照欲添加之濃度進行選擇，並調整鍍液濃度、時間即可。電解鍍敷法、無電鍍敷法皆組入至導線製造步驟之何處均可，亦可反覆進行複數次。亦可組入至複數個步驟。可向Pd被覆前之Cu表面添加，可向Pd被覆後之Pd表面添加，可向Au被覆後之Au表面添加，亦可組入至各被覆步驟。
於蒸鍍法(乾式)中，存在濺射法、離子鍍覆法、真空蒸鍍法、電漿CVD等。由於為乾式，故而優點為無需預處理、後處理，亦無需擔憂污染。通常，蒸鍍法之問題在於目標之元素之添加速度較慢，但由於上述成分元素之添加濃度相對較低，故而就本發明之目的而言，為 適合之方法之一。
各蒸鍍法組入至導線製造步驟之何處均可，亦可反覆進行複數次。亦可組入至複數個步驟。可向Pd被覆前之Cu表面添加，可向Pd被覆後之Pd表面添加，可向Au被覆後之Au表面添加，亦可組入至各被覆步驟。
對如下製造方法進行說明，該製造方法係用以於對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，將導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率設為30%以上，且將接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑設為0.9~1.5μm。
對於接合線而言，若使Cu合金芯材中含有賦予高溫環境下之連接可靠性之元素，則導線之材料強度(硬度)變高。因此，於對Cu芯線之接合線進行拉線加工時，將拉線時之縮面率設為低為5~8%之縮面率。又，於拉線後之熱處理中，硬度仍然較高，故而為了軟質化至可用作接合線之等級，而以600℃以上之溫度進行熱處理。由於為較高之熱處理溫度，故而導線長度方向之<100>方位比率未達30%，同時芯材剖面中之平均結晶粒徑超過1.5μm，耐力比超過1.6。另一方面，若欲降低耐力比而降低熱處理溫度，則芯材剖面中之平均結晶粒徑未達0.9μm，耐力比未達1.1，楔形接合性較差。
與此相對，於本發明中，於使用模具之拉線時，在總模具數中之一半以上之模具中，將縮面率設為10%以上，進而將拉線後之熱處理中之熱處理溫度設為低為500℃以下之溫度。其結果，可於對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，將導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率設為30%以上，且將接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑設為0.9~1.5μm。應用最新之 拉線加工技術，關於潤滑劑，將潤滑劑所包含之非離子系界面活性劑之濃度設計為高於先前，關於模具形狀，將模具之漸近角(Approach angle)設計為較先前者和緩，將模具之冷卻水溫度設定為略低於先前，藉由如上等之協同效應，而儘管Cu合金芯材中含有Ni等成分總計0.03質量%以上而硬質化，亦能實現縮面率為10%以上之拉線加工。
於測定導線剖面之結晶方位時，較佳為使用電子背散射繞射法(EBSD，Electron Backscattered Diffraction)。EBSD法具有可對觀察面之結晶方位進行觀察並圖示鄰接之測定點間之結晶方位之角度差的特徵，即便為接合線之類之細線，亦可相對較簡便地並且高精度地觀察結晶方位。關於粒徑測定，可藉由針對利用EBSD法獲得之測定結果利用裝置所配備之解析軟體而求出。本發明所規定之結晶粒徑係對測定區域內所包含之晶粒之等效直徑(與晶粒之面積相當之圓之直徑；圓當量徑)進行算術平均而得者。
本發明並不限定於上述實施形態，可於本發明之主旨之範圍內適當進行變更。
[實施例]
以下，一面示出實施例，一面對本發明之實施形態之接合線具體地進行說明。
<本發明例1~59及比較例1~16>
(樣品之製作)
首先，對樣品之製作方法進行說明。成為芯材之原材料之Cu係使用純度為99.99質量%以上、剩餘部分由不可避免之雜質構成者。Au、Pd、Ni、Zn、Rh、In、Ir、Pt係使用純度為99質量%以上、剩餘部分由不可避免之雜質構成者。以導線或芯材之組成成為目標組成之方式，調配向芯材中添加之元素(Ni、Zn、Rh、In、Ir、Pt)。關於 Ni、Zn、Rh、In、Ir、Pt之添加，亦能以單質進行調配，但於為單質且高熔點之元素或添加量為極微量之情形時，亦可預先製作包含添加元素之Cu母合金，以成為目標添加量之方式進行調配。於本發明例27~47中，進而含有Ga、Ge、As、Te、Sn、Sb、Bi、Se、B、P、Mg、Ca、La中之1種以上。
芯材之Cu合金係藉由連續鑄造而以成為數mm之線徑之方式進行製造。對所獲得之數mm之合金進行拉拔加工，製作0.3~1.4mm之導線。拉線係使用市售之潤滑劑，拉線速度係設為20~150m/分鐘。於為了去除導線表面之氧化膜而利用鹽酸等進行過酸洗處理之後，以覆蓋芯材之Cu合金之整個表面之方式形成1~15μm之Pd被覆層。進而，一部分之導線係於Pd被覆層之上形成0.05~1.5μm之包含Au與Pd之合金表皮層。Pd被覆層、包含Au與Pd之合金表皮層之形成係使用電解鍍敷法。鍍液係使用市售之半導體用鍍液。其後，主要使用縮面率為10~21%之模具進行拉線加工，進而於中途，以200~500℃進行1至3次之熱處理，藉此將直徑加工至20μm。於加工後，以最終斷裂伸長率成為約5~15%之方式進行熱處理。熱處理方法係一面連續地掃動導線一面進行，一面通入N2或Ar氣體一面進行。將導線之進給速度設為10~90m/分鐘，將熱處理溫度設為350~500℃，將熱處理時間設為1~10秒。
(評價方法)
關於導線中之Ni、Zn、Rh、In、Ir、Pt、Ga、Ge、As、Te、Sn、Sb、Bi、Se、B、P、Mg、Ca、La含量，係利用ICP發射光譜分析裝置，以接合線整體所包含之元素之濃度之形式進行分析。
Pd被覆層、包含Au與Pd之合金表皮層之濃度分析係一面利用濺射等自接合線之表面朝向深度方向進行切削一面實施歐傑電子光譜分析。根據所獲得之深度方向之濃度分佈，求出Pd被覆層之厚度、Pd之 最大濃度、包含Au與Pd之合金表皮層之厚度。
關於接合線之垂直於導線軸之方向之芯材剖面中之導線長度方向之結晶方位中，相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率，係利用EBSD法對觀察面(即，垂直於導線軸之方向之芯材剖面)之結晶方位進行觀察之後算出。EBSD測定資料之解析係利用專用軟體(TSL Solutions製造之OIM analisis等)。關於垂直於導線軸之方向之芯材剖面中之平均結晶粒徑，係利用EBSD法對觀察面之結晶方位進行觀察之後算出。EBSD測定資料之解析係利用專用軟體(TSL Solutions製造之OIM analisis等)。結晶粒徑係對測定區域內所包含之晶粒之等效直徑(與晶粒之面積相當之圓之直徑；圓當量徑)進行算術平均而得者。
關於0.2%耐力與最大耐力，係藉由將標距設為100mm進行拉伸試驗而評價。作為拉伸試驗裝置，使用英斯特朗公司製造之萬能材料試驗機5542型。0.2%耐力係使用裝置所配備之專用軟體而算出。又，將斷裂時之負荷設為最大耐力。根據下述(1)式算出耐力比。
耐力比=最大耐力/0.2%耐力 (1)
導線接合部中之楔形接合性之評價係於BGA基板之楔形接合部接合1000根，並根據接合部之剝離之產生頻度而進行判定。所使用之BGA基板係實施過鍍Ni及鍍Au者。於本評價中，假定較通常更為嚴格之接合條件，將載置台溫度設定為較一般之設定溫度區域低之150℃。於上述之評價中，於產生11個以上不良之情形時，判斷為有問題，設為×記號，若不良為6~10個，則判斷為可實用但稍有問題，設為△記號，於不良為1~5個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表1~表4之「楔形接合性」一欄中進行記載。
高溫高濕環境或高溫環境下之球接合部之接合可靠性係製作接 合可靠性評價用之樣品，進行HTS評價，並根據球接合部之接合壽命而進行判定。接合可靠性評價用之樣品係藉由使用市售之打線接合機對在一般之金屬框架上之Si基板上成膜厚度0.8μm之Al-1.0%Si-0.5%Cu之合金而形成之電極進行球接合，並利用市售之環氧樹脂進行密封而製作。球係一面以流量0.4~0.6L/min通入N2+5%H2氣體一面形成，其大小係設為33~34μm之範圍。
關於HTS評價，係使用高溫恆溫器將製作之接合可靠性評價用之樣品暴露於溫度200℃之高溫環境。球接合部之接合壽命係設為每500小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HTS評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上述之評價中，若接合壽命未達500小時，則判斷為無法實用，設為×記號，若為500小時以上且未達1000小時，則判斷為可實用但要求改善，設為△記號，若為1000小時以上且未達3000小時，則判斷為實用上無問題，設為○記號，若為3000小時以上，則判斷為尤其優異，設為◎記號，於表1~表4之「HTS」一欄中進行記載。
球形成性(FAB形狀)之評價係選取進行接合前之球並進行觀察，判定球表面有無氣泡、原本為真球之球有無變形。於產生上述任一情況之情形時，判斷為不良。為了抑制熔融步驟中之氧化，球之形成係一面以流量0.5L/min吹送N2氣體一面進行。球之大小係設為34μm。針對1條件，觀察50個球。觀察係使用SEM。於球形成性之評價中，於產生5個以上不良之情形時，判斷為有問題，設為×記號，若不良為3~4個，則判斷為可實用但稍有問題，設為△記號，於不良為1~2個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判 斷為優異，設為◎記號，於表1~表4之「FAB形狀」一欄中進行記載。
關於溫度為130℃、相對濕度為85%之高溫高濕環境下之球接合部之接合壽命，可利用以下之HAST評價進行評價。關於HAST評價，係使用不飽和型壓力鍋試驗機將製作之接合可靠性評價用之樣品暴露於溫度130℃、相對濕度85%之高溫高濕環境中，施加5V之偏壓。球接合部之接合壽命係設為每48小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HAST評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上述之評價中，若接合壽命未達144小時，則判斷為無法實用，設為×記號，若為144小時以上且未達288小時，則判斷為實用上無問題，設為○記號，若為288小時以上且未達384小時，則判斷為優異，設為◎記號，若為384小時以上，則判斷為尤其優異，設為◎◎記號，於表1~表4之「HAST」一欄中進行記載。
球接合部之壓扁形狀之評價係自正上方觀察進行過接合之球接合部，根據其真圓性進行判定。接合對象係使用在Si基板上成膜厚度1.0μm之Al-0.5%Cu之合金所得之電極。觀察係使用光學顯微鏡，針對1條件，觀察200處。將與真圓之偏差較大之橢圓狀者、變形具有各向異性者判斷為球接合部之壓扁形狀不良。於上述之評價中，於不良為1~3個之情形時，判斷為無問題，設為○記號，於全部獲得良好之真圓性之情形時，判斷為尤其優異，設為◎記號，於表1~表4之「壓扁形狀」一欄中進行記載。
[表1]
(評價結果)
本發明例1~59之接合線具有Cu合金芯材、及形成於Cu合金芯材之表面之Pd被覆層，且Pd被覆層之厚度處於較佳範圍之0.015~0.150μm之範圍內，FAB形狀均為良好。又，該等接合線包含選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素，上述元素相對於導線整體之濃度合計為0.011~2質量%，因此根據HTS評價所得之球接合部 高溫可靠性亦為良好。
又，關於本發明例，將拉線時之縮面率設為10%以上，將拉線後之熱處理中之熱處理溫度設為低為500℃以下之溫度，故而可於對接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，將導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率設為30%以上，且可將接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑設為0.9~1.5μm。其結果為，儘管導線中含有Ni、Zn、Rh、In、Ir、Pt，耐力比(=最大耐力/0.2%耐力)仍均處於1.1~1.6之範圍內。因此，楔形接合性均為良好之結果。
另一方面，比較例4~7、12~14中，將熱處理溫度設為高為600℃以上之溫度，因此導線長度方向之<100>方位比率未達30%。又，比較例2、6、8、9、14中，將熱處理溫度設為高為620℃以上之溫度，因此導線長度方向之<100>方位比率未達30%，並且芯材剖面中之平均結晶粒徑超過1.5μm。因此，比較例2、4~9、12~14中，耐力比均超過1.6，楔形接合性均為不良或存在問題。
又，比較例1、3中，將模具之縮面率設為未達10%，故而芯材剖面中之平均結晶粒徑未達0.9μm，耐力比未達1.1，楔形接合性均為不良。比較例10及11中，導線長度方向之<100>方位比率未達30%，並且芯材剖面中之平均結晶粒徑未達0.9μm，楔形接合性均為不良。比較例15中，雖然平均結晶粒徑為0.9~1.5μm，並且導線長度方向之<100>方位比率為30%以上，但由於未包含賦予高溫環境下之連接可靠性之元素，故而HTS、HAST、及楔形連接性均為不良。比較例16中，由於未包含賦予高溫環境下之連接可靠性之元素，故而HTS及HAST不良。
<本發明例2-1~2-44>
(樣品)
首先，對樣品之製作方法進行說明。成為芯材之原材料之Cu係使用純度為99.99質量%以上、剩餘部分由不可避免之雜質構成者。Ga、Ge、Ni、Ir、Pt、Pd、B、P、Mg係使用純度為99質量%以上、剩餘部分由不可避免之雜質構成者。以導線或芯材之組成成為目標組成之方式，調配作為向芯材中添加之元素的Ga、Ge、Ni、Ir、Pt、Pd、B、P、Mg。關於Ga、Ge、Ni、Ir、Pt、Pd、B、P、Mg之添加，亦能以單質進行調配，但於為單質且高熔點之元素或添加量為極微量之情形時，亦可預先製作包含添加元素之Cu母合金，以成為目標添加量之方式進行調配。
芯材之Cu合金係藉由如下方式進行製造：將原料裝填至加工成直徑為3~6mm之圓柱型之碳坩鍋中，使用高頻爐，於真空中或N2或Ar氣體等惰性氛圍中加熱至1090~1300℃而加以熔解後，進行爐內冷卻。對所獲得之3~6mm之合金進行拉拔加工而加工至0.9~1.2mm後，使用模具連續地進行拉線加工等，藉此製作300~600μm之導線。拉線係使用市售之潤滑劑，拉線速度係設為20~150m/分鐘。於為了去除導線表面之氧化膜而利用鹽酸進行酸洗處理之後，以覆蓋芯材之Cu合金之整個表面之方式形成1~15μm之Pd被覆層。進而，一部分之導線係於Pd被覆層之上形成0.05~1.5μm之包含Au與Pd之合金表皮層。Pd被覆層、包含Au與Pd之合金表皮層之形成係使用電解鍍敷法。鍍液係使用市售之半導體用鍍液。其後，藉由反覆進行200~500℃之熱處理與拉線加工而將直徑加工至20μm。於加工後，以最終斷裂伸長率成為約5~15%之方式一面通入N2或Ar氣體一面進行熱處理。熱處理方法係一面連續地掃動導線一面進行，一面通入N2或Ar氣體一面進行。將導線之進給速度設為20~200m/分鐘，將熱處理溫度設為200~600℃，將熱處理時間設為0.2~1.0秒。
Pd被覆層、包含Au與Pd之合金表皮層之濃度分析中，一面利用Ar離子自接合線之表面朝向深度方向進行濺射一面使用歐傑電子光譜分析裝置進行分析。被覆層及表皮合金層之厚度係根據所獲得之深度方向之濃度分佈(深度之單位係經SiO2換算)而求出。將Pd之濃度為50原子%以上且Au之濃度未達10原子%之區域設為Pd被覆層，將Pd被覆層之表面之Au濃度為10原子%以上之範圍之區域設為合金表皮層。將被覆層及合金表皮層之厚度及Pd最大濃度分別記載於表5及表6中。Cu合金芯材中之Pd之濃度係藉由使導線剖面露出並利用掃描式電子顯微鏡所配備之電子探針微量分析器進行線分析、點分析等方法測定。作為使導線剖面露出之方法，利用機械研磨、離子蝕刻法等。接合線中之Ga、Ge、Ni、Ir、Pt、B、P、Mg之濃度係利用ICP發光分光分析裝置、ICP質譜分析裝置對將接合線用強酸溶解而成之液體進行分析，以接合線整體所包含之元素之濃度之形式進行檢測。
將藉由上述程序所製作之各樣品之構成示於下述表5及表6中。
(評價方法)
將導線表面設為觀察面，進行結晶組織之評價。作為評價方法，使用電子背散射繞射法(EBSD，Electron Backscattered Diffraction)。EBSD法具有可對觀察面之結晶方位進行觀察並圖示鄰接之測定點間之結晶方位之角度差的特徵，即便為接合線之類之細線，亦可相對較簡便地並且高精度地觀察結晶方位。
於將如導線表面般之曲面作為對象而實施EBSD法之情形時，必須加以注意。若對曲率較大之部位進行測定，則難以進行高精度之測定。然而，藉由將供於測定之接合線平面地固定於直線上，並對該接合線之中心附近之平坦部進行測定，可進行高精度之測定。具體而言，設為如下之測定區域即可。圓周方向之尺寸係以導線長度方向之 中心為軸設為線徑之50%以下，導線長度方向之尺寸係設為100μm以下。較佳為若將圓周方向之尺寸設為線徑之40%以下，且將導線長度方向之尺寸設為40μm以下，則可藉由測定時間之縮短而提高測定效率。為了進一步提高精度，較理想為測定3處以上而獲得考慮到不均之平均資訊。測定位置以不靠近之方式隔開1mm以上即可。
關於接合線之垂直於導線軸之方向之芯材剖面中之導線長度方向之結晶方位中，相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率、及垂直於導線軸之方向之芯材剖面中之平均結晶粒徑(μm)，係藉由與本發明例1~59相同之方法求出。又，關於0.2%耐力及最大耐力，係藉由與本發明例1~59相同之方法進行評價，並根據上述(1)式算出耐力比。
高溫高濕環境或高溫環境下之球接合部之接合可靠性係製作接合可靠性評價用之樣品，進行HAST及HTS評價，根據各試驗中之球接合部之接合壽命而進行判定。接合可靠性評價用之樣品係使用市售之打線接合機對在一般之金屬框架上之Si基板上成膜厚度0.8μm之Al-1.0%Si-0.5%Cu之合金而形成之電極進行球接合，並利用市售之環氧樹脂進行密封而製作。球係一面以流量0.4~0.6L/min通入N2+5%H2氣體一面形成，其大小係設為33~34μm之範圍。
關於HAST評價，係使用不飽和型壓力鍋試驗機將製作之接合可靠性評價用之樣品暴露於溫度130℃、相對濕度85%之高溫高濕環境中，施加7V之偏壓。球接合部之接合壽命係設為每48小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HAST評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上 述之評價中，若接合壽命未達96小時，則判斷為實用上有問題，設為×記號，若為96小時以上且未達144小時，則判斷為可實用但稍有問題，設為△記號，若為144小時以上且未達288小時，則判斷為實用上無問題，設為○記號，若為288小時以上，則判斷為尤其優異，設為◎記號，於表5及表6之「HAST」一欄中進行記載。
關於HTS評價，係使用高溫恆溫器將製作之接合可靠性評價用之樣品暴露於溫度200℃之高溫環境中。球接合部之接合壽命係設為每500小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HTS評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上述之評價中，若接合壽命為500小時以上且未達1000小時，則判斷為可實用但要求改善，設為△記號，若為1000小時以上且未達3000小時，則判斷為實用上無問題，設為○記號，若為3000小時以上，則判斷為尤其優異，設為◎記號。
球形成性(FAB形狀)之評價係選取進行接合前之球並進行觀察，判定球表面有無氣泡、原本為真球之球有無變形。於產生上述任一情況之情形時，判斷為不良。為了抑制熔融步驟中之氧化，球之形成係一面以流量0.5L/min吹送N2氣體一面進行。球之大小係設為34μm。針對1條件，觀察50個球。觀察係使用SEM。於球形成性之評價中，於產生5個以上不良之情形時，判斷為有問題，設為×記號，若不良為3~4個，則判斷為可實用但稍有問題，設為△記號，於不良為1~2個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表5及表6之「FAB形狀」一欄中進行記載。
導線接合部中之楔形接合性之評價係於引線框架之引線部分接合1000根，並根據接合部之剝離之產生頻度而進行判定。引線框架係使用實施過1~3μm之鍍Ag之Fe-42原子%Ni合金引線框架。於本評價中，假定較通常更為嚴格之接合條件，將載置台溫度設定為較一般之設定溫度區域低之150℃。於上述之評價中，於產生11個以上不良之情形時，判斷為有問題，設為×記號，若不良為6~10個，則判斷為可實用但稍有問題，設為△記號，於不良為1~5個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表5及表6之「楔形接合性」一欄中進行記載。
球接合部之壓扁形狀之評價係自正上方觀察進行過接合之球接合部，根據其真圓性進行判定。接合對象係使用在Si基板上成膜厚度1.0μm之Al-0.5%Cu之合金所得之電極。觀察係使用光學顯微鏡，針對1條件，觀察200處。將與真圓之偏差較大之橢圓狀者、變形具有各向異性者判斷為球接合部之壓扁形狀不良。於上述之評價中，於產生6個以上不良之情形時，判斷為有問題，設為×記號，若不良為4~5個，則判斷為可實用但稍有問題，設為△記號，於1~3個之情形時，判斷為無問題，設為○記號，於全部獲得良好之真圓性之情形時，判斷為尤其優異，設為◎記號，於表5及表6之「壓扁形狀」一欄中進行記載。
[偏斜]
於評價用之引線框架以電路長度5mm、電路高度0.5mm接合100根。作為評價方法，自晶片水平方向觀察導線直立部而利用通過球接合部之中心之垂線與導線直立部之間隔最大時之間隔(偏斜間隔)進行評價。於偏斜間隔小於導線徑之情形時，判斷為偏斜良好，於偏斜間隔大於導線徑之情形時，由於直立部傾斜，故而判斷為偏斜不良。藉由光學顯微鏡觀察100根接合之導線，數出偏斜不良之根數。於產生7 個以上不良之情形時，判斷為有問題，設為×記號，若不良為4~6個，則判斷為可實用但稍有問題，設為△記號，於不良為1~3個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表5及表6之「偏斜」一欄中進行記載。
(評價結果)
如表5及表6所示，本發明例2-1~2-44之接合線具有Cu合金芯材、及形成於Cu合金芯材之表面之Pd被覆層，且接合線包含選自Ga、Ge之1種以上之元素，上述元素相對於導線整體之濃度合計為0.011~1.5質量%。確認藉此本發明例2-1~2-44之接合線於溫度為130℃、相對濕度為85%之高溫高濕環境下之HAST試驗中獲得球接合部可靠性。
關於在Pd被覆層上進而具有包含Au與Pd之合金表皮層之本發明例，確認藉由使包含Au與Pd之合金表皮層之厚度為0.0005~0.050μm，而獲得優異之楔形接合性。
於接合線進而包含選自Ni、Ir、Pt、Pd之至少1種以上之元素之本發明例中，確認利用HTS評價所得之球接合部高溫可靠性更為良好。
接合線進而包含選自B、P、Mg之至少1種以上之元素之本發明例中，確認藉由使上述元素相對於導線整體之濃度分別為1~200質量ppm，球接合部之壓扁形狀良好。
<本發明例3-1~3-50>
(樣品)
首先，對樣品之製作方法進行說明。成為芯材之原材料之Cu係使用純度為99.99質量%以上、剩餘部分由不可避免之雜質構成者。As、Te、Sn、Sb、Bi、Se、Ni、Zn、Rh、In、Ir、Pt、Ga、Ge、Pd、B、P、Mg、Ca、La係使用純度為99質量%以上、剩餘部分由不 可避免之雜質構成者。以導線或芯材之組成成為目標組成之方式，調配作為向芯材中添加之元素的As、Te、Sn、Sb、Bi、Se、Ni、Zn、Rh、In、Ir、Pt、Ga、Ge、Pd、B、P、Mg、Ca、La。關於As、Te、Sn、Sb、Bi、Se、Ni、Zn、Rh、In、Ir、Pt、Ga、Ge、Pd、B、P、Mg、Ca、La之添加，亦能以單質進行調配，但於為單質且高熔點之元素或添加量為極微量之情形時，亦可預先製作包含添加元素之Cu母合金，以成為目標添加量之方式進行調配。
芯材之Cu合金係藉由如下方式製造：將原料裝填至加工成直徑為3~6mm之圓柱型之碳坩鍋中，使用高頻爐，於真空中或N2或Ar氣體等惰性氛圍中加熱至1090~1300℃而使原料熔解後，進行爐內冷卻。對所獲得之3~6mm之合金進行拉拔加工而加工至0.9~1.2mm後，使用模具連續地進行拉線加工等，藉此製作300~600μm之導線。拉線係使用市售之潤滑劑，拉線速度係設為20~150m/分鐘。於為了去除導線表面之氧化膜而利用鹽酸進行過酸洗處理之後，以覆蓋芯材之Cu合金之整個表面之方式形成1~15μm之Pd被覆層。進而，一部分之導線係於Pd被覆層之上形成0.05~1.5μm之包含Au與Pd之合金表皮層。Pd被覆層、包含Au與Pd之合金表皮層之形成係使用電解鍍敷法。鍍液係使用市售之半導體用鍍液。其後，藉由反覆進行200~500℃之熱處理與拉線加工而將直徑加工至20μm。於加工後，以最終斷裂伸長率成為約5~15%之方式一面通入N2或Ar氣體一面進行熱處理。熱處理方法係一面連續地掃動導線一面進行，一面通入N2或Ar氣體一面進行。將導線之進給速度設為20~200m/分鐘，將熱處理溫度設為200~600℃，將熱處理時間設為0.2~1.0秒。
Pd被覆層、包含Au與Pd之合金表皮層之濃度分析中，一面利用濺射等自接合線之表面朝向深度方向進行切削一面實施歐傑電子光譜分析。根據所獲得之深度方向之濃度分佈，求出Pd被覆層之厚度、包 含Au與Pd之合金表皮層之厚度及Pd最大濃度。
關於本發明例3-1~3-50，使芯材中含有選自As、Te、Sn、Sb、Bi、Se之元素。
關於本發明例3-34~3-44，使接合線之最表面存在Cu。因此，於表7中設置「導線表面Cu濃度」之欄，記載藉由歐傑電子光譜裝置對接合線之表面進行測定之結果。藉由選擇接合線之熱處理溫度與時間而使最表面含有特定濃度之Cu。關於本發明例3-1~3-33、3-45~3-50，設為使最表面不存在Cu之熱處理條件，即便利用歐傑電子光譜裝置亦未檢測出Cu。
將藉由上述程序所製作之各樣品之構成示於表7及表8中。
(評價方法)
將導線表面設為觀察面，進行結晶組織之評價。作為評價方法，使用電子背散射繞射法(EBSD，Electron Backscattered Diffraction)。EBSD法具有可對觀察面之結晶方位進行觀察並圖示鄰接之測定點間之結晶方位之角度差的特徵，即便為接合線之類之細線，亦可相對較簡便地並且高精度地觀察結晶方位。
於將如導線表面般之曲面作為對象而實施EBSD法之情形時，必須加以注意。若對曲率較大之部位進行測定，則難以進行高精度之測定。然而，藉由將供於測定之接合線平面地固定於直線上，並對該接合線之中心附近之平坦部進行測定，可進行高精度之測定。具體而言，設為如下之測定區域即可。圓周方向之尺寸係以導線長度方向之中心為軸設為線徑之50%以下，導線長度方向之尺寸係設為100μm以下。較佳為若將圓周方向之尺寸設為線徑之40%以下，且將導線長度 方向之尺寸設為40μm以下，則可藉由測定時間之縮短而提高測定效率。為了進一步提高精度，較理想為測定3處以上而獲得考慮到不均之平均資訊。測定位置以不靠近之方式隔開1mm以上即可。
關於接合線之垂直於導線軸之方向之芯材剖面中之導線長度方向之結晶方位中，相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率、及垂直於導線軸之方向之芯材剖面中之平均結晶粒徑(μm)，係藉由與本發明例1~59相同之方法求出。又，關於0.2%耐力及最大耐力，係藉由與本發明例1~59相同之方法進行評價，並根據上述(1)式算出耐力比。
高溫高濕環境或高溫環境下之球接合部之接合可靠性係製作接合可靠性評價用之樣品，進行HAST及HTS評價，根據各試驗中之球接合部之接合壽命而進行判定。接合可靠性評價用之樣品係使用市售之打線接合機對在一般之金屬框架上之Si基板上成膜厚度0.8μm之Al-1.0%Si-0.5%Cu之合金而形成之電極進行球接合，並藉由市售之環氧樹脂進行密封而製作。球係一面以流量0.4~0.6L/min通入N2+5%H2氣體一面形成，其大小係設為33~34μm之範圍。
關於HAST評價，係使用不飽和型壓力鍋試驗機將製作之接合可靠性評價用之樣品暴露於溫度130℃、相對濕度85%之高溫高濕環境中，施加5V之偏壓。球接合部之接合壽命係設為每48小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HAST評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上述之評價中，若接合壽命未達96小時，則判斷為實用上有問題，設為×記號，若為96小時以上且未達144小時，則判斷為可實用但稍有問 題，設為△記號，若為144小時以上且未達288小時，則判斷為實用上無問題，設為○記號，若為288小時以上且未達384小時，則判斷為優異，設為◎記號，若為384小時以上，則判斷為尤其優異，設為◎◎記號，於表7及表8之「HAST」一欄中進行記載。
關於HTS評價，係使用高溫恆溫器將製作之接合可靠性評價用之樣品暴露於溫度200℃之高溫環境中。球接合部之接合壽命係設為每500小時實施一次球接合部之抗剪試驗而抗剪強度之值成為初期所獲得之抗剪強度之1/2的時間。高溫高濕試驗後之抗剪試驗係藉由酸處理而去除樹脂，使球接合部露出後進行。
HTS評價之抗剪試驗機係使用DAGE公司製造之試驗機。抗剪強度之值係使用隨機選擇之球接合部之10處之測定值的平均值。於上述之評價中，若接合壽命為500小時以上且未達1000小時，則判斷為可實用但要求改善，設為△記號，若為1000小時以上且未達3000小時，則判斷為實用上無問題，設為○記號，若為3000小時以上，則判斷為尤其優異，設為◎記號，於表7及表8之「HTS」一欄中進行記載。
球形成性(FAB形狀)之評價係選取進行接合前之球並進行觀察，判定球表面有無氣泡、原本為真球之球有無變形。於產生上述任一情況之情形時，判斷為不良。為了抑制熔融步驟中之氧化，球之形成係一面以流量0.5L/min吹送N2氣體一面進行。球之大小係設為34μm。針對1條件，觀察50個球。觀察係使用SEM。於球形成性之評價中，於產生5個以上不良之情形時，判斷為有問題，設為×記號，若不良為3~4個，則判斷為可實用但稍有問題，設為△記號，於不良為1~2個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表7及表8之「FAB形狀」一欄中進行記載。
導線接合部中之楔形接合性之評價係於引線框架之引線部分接 合1000根，並根據接合部之剝離之產生頻度而進行判定。引線框架係使用實施過1~3μm之鍍Ag之Fe-42原子%Ni合金引線框架。於本評價中，假定較通常更為嚴格之接合條件，將載置台溫度設定為較一般之設定溫度區域低之150℃。於上述之評價中，於產生11個以上不良之情形時，判斷為有問題，設為×記號，若不良為6~10個，則判斷為可實用但稍有問題，設為△記號，於不良為1~5個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表7及表8之「楔形接合性」一欄中進行記載。
球接合部之壓扁形狀之評價係自正上方觀察進行過接合之球接合部，根據其真圓性進行判定。接合對象係使用在Si基板上成膜厚度1.0μm之Al-0.5%Cu之合金之電極。觀察係使用光學顯微鏡，針對1條件，觀察200處。將與真圓之偏差較大之橢圓狀者、變形具有各向異性者判斷為球接合部之壓扁形狀不良。於上述之評價中，於產生6個以上不良之情形時，判斷為有問題，設為×記號，若不良為4~5個，則判斷為可實用但稍有問題，設為△記號，於1~3個之情形時，判斷為無問題，設為○記號，於全部獲得良好之真圓性之情形時，判斷為尤其優異，設為◎記號，於表7及表8之「壓扁形狀」一欄中進行記載。
[偏斜]
於評價用之引線框架以電路長度5mm、電路高度0.5mm接合100根。作為評價方法，自晶片水平方向觀察導線直立部而利用通過球接合部之中心之垂線與導線直立部之間隔最大時之間隔(偏斜間隔)進行評價。於偏斜間隔小於導線徑之情形時，判斷為偏斜良好，於偏斜間隔大於導線徑之情形時，由於直立部傾斜，故而判斷為偏斜不良。藉由光學顯微鏡觀察100根接合之導線，數出偏斜不良之根數。於產生7個以上不良之情形時，判斷為有問題，設為×記號，若不良為4~6 個，則判斷為可實用但稍有問題，設為△記號，於不良為1~3個之情形時，判斷為無問題，設為○記號，於未產生不良之情形時，判斷為優異，設為◎記號，於表7及表8之「偏斜」一欄中進行記載。
(評價結果)
本發明例3-1~3-50之接合線具有Cu合金芯材、及形成於Cu合金芯材之表面之Pd被覆層，且接合線包含選自As、Te、Sn、Sb、Bi、Se之至少1種以上之元素，上述元素相對於導線整體之濃度合計為0.1~100質量ppm。確認藉此本發明例3-1~3-50之接合線於溫度為130℃、相對濕度為85%之高溫高濕環境下之HAST試驗中獲得球接合部可靠性。
關於在Pd被覆層上進而具有包含Au與Pd之合金表皮層之本發明例，確認藉由使包含Au與Pd之合金表皮層之層厚為0.0005~0.050μm，而獲得優異之楔形接合性。
本發明例3-21~3-33、3-35、3-37、3-39~3-44中，確認：藉由使接合線進而包含選自Ni、Zn、Rh、In、Ir、Pt、Ga、Ge之至少1種以上之元素，且使上述元素相對於導線整體之濃度分別為0.011~1.2質量%，使Cu合金芯材所包含之Pd之濃度為0.05~1.2質量%，而使利用HTS評價所得之球接合部高溫可靠性良好。
本發明例3-22~3-26、3-29~3-32中，藉由使接合線進而包含選自B、P、Mg、Ca、La之至少1種以上之元素，且使上述元素相對於導線整體之濃度分別為1~100質量ppm，而使FAB形狀良好，並且使楔形接合性良好。
本發明例3-34~3-44中，導線含有As、Te、Sn、Sb、Bi、Se，並且於導線之最表面存在Cu。藉此，本發明例3-34~3-44中，HAST評價結果為◎◎或◎，可見使最表面存在Cu之效果。
<本發明例4-1~4-15>
作為接合線之原材料，分別準備用以製造Cu合金芯材之純度為99.99質量%以上之Cu，作為添加元素之Ni、Pd、Pt、Au、P、B、Be、Fe、Mg、Ti、Zn、Ag、Si，被覆層形成用之純度為99.99質量%以上之Pd、表皮合金層形成用之純度為99.99質量%以上之Au。稱量Cu與添加元素原料作為起始原料之後，將其於高真空下加熱而熔解，藉此獲得直徑10mm左右之銅合金錠。其後，對該錠進行鍛造、壓延、拉線而製作直徑500μm之Cu合金導線。繼而，利用電解鍍敷於Cu合金導線表面以成為1~3μm厚度之方式施以Pd被覆層，且於被覆層之表面以成為0.05~0.2μm厚度之方式施以Au表皮層，獲得複層導線。將Pd被覆層、AuPd表皮合金層之最終厚度記載於表8中。此處，芯材與被覆層之邊界係設為Pd濃度為50原子%之位置，被覆層與表皮合金層之邊界係設為Au濃度為10原子%之位置。其後，以拉線速度100~700m/min、模具縮面率8~30%進行連續拉線加工而製成表8中所記載之最終線徑。表皮合金層之厚度、Au最大濃度、表面Cu濃度、被覆層之厚度係藉由於拉線加工間實施2次至3次之熱處理而進行控制。關於彼時之條件，於導線直徑為200~250μm時，為溫度500~700℃、速度10~70m/min，於導線直徑為70~100μm時，為溫度450~650℃、速度20~90m/min，於最終線徑較細之情形時，進而於導線直徑為40~70μm時，為溫度300~500℃、速度30~100m/min。其後，於最終線徑下以表8之溫度、速度30~120m/min實施熱處理。又，為了使Cu擴散至表面，僅於1次熱處理中將熱處理爐中之氧濃度設定為較通常高之0.2~0.7%。該熱處理較佳為儘可能最後進行，其原因為：若於Cu到達至表面後反覆進行拉線加工，則容易引起Cu之氧化。藉由於其以外之熱處理中將熱處理爐中之氧濃度設為未達0.2%，而抑制表皮合金層之過度之氧化，並且控制穩定之厚度、組成等。以此方式獲得直徑為15~25μm之接合線。
被覆層、表皮合金層之濃度分析、Cu合金芯材中之Ni、Pd、Pt、Au之濃度分析中，一面利用Ar離子自接合線之表面朝向深度方向進行濺射一面使用AES(Auger Electron Spectroscopy，歐傑電子光譜分析)裝置進行分析。被覆層及表皮合金層之厚度係根據所獲得之深度方向之濃度分佈(深度之單位係經SiO2換算)而求出。觀察元素分佈時，亦利用EPMA(electron probe micro-analysis，電子探針微量分析)、EDX(Energy Dispersive X-ray Spectroscopy，能量分散型X射線分析)裝置等進行分析。將Pd之濃度為50原子%以上、且Au之濃度未達10原子%之區域設為被覆層，將被覆層之表面之Au濃度為10原子%以上之範圍之區域設為表皮合金層。將被覆層及表皮合金層之厚度及組成記載於表8中。接合線中之P、B、Be、Fe、Mg、Ti、Zn、Ag、Si之濃度係藉由ICP發射光譜分析裝置、ICP質譜分析裝置等進行測定。關於接合線之垂直於導線軸之方向之芯材剖面中之導線長度方向之結晶方位中，相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率、及垂直於導線軸之方向之芯材剖面中之平均結晶粒徑(μm)，係藉由與本發明例1~59相同之方法求出。又，關於0.2%耐力及最大耐力，係藉由與本發明例1~59相同之方法進行評價，並根據上述(1)式算出耐力比。
接合線之連接係使用市售之自動打線接合機。於即將進行接合之前藉由電弧放電於接合線之前端製作球部，其直徑係以成為接合線之直徑之1.7倍之方式進行選擇。球部製作時之氛圍係設為氮氣。
作為接合線之接合對象，分別使用形成於Si晶片上之厚度1μm之Al電極、及表面鍍Pd之引線框架之引線。將所製作之球部與加熱至260℃之上述電極進行球接合之後，將接合線之母線部與加熱至260℃之上述引線進行楔形接合，並再次製作球部，藉此連續地反覆進行接合。電路長度係設為3mm與5mm兩種，電路高度係設為0.3mm與0.5 mm兩種。
關於接合線之楔形接合性，對接合性、魚尾對稱性進行評價。關於接合性，對100根進行過楔形接合之狀態之接合線之接合部進行觀察，將接合部剝離者計數為NG。關於魚尾對稱性，對100根進行過楔形接合之狀態之接合線之接合部進行觀察，評價其對稱性。對自魚尾狀壓接部之中央至左端之長度、至右端之長度進行測量，將其差為10%以上者計數為NG。接合性與魚尾對稱性係將NG為0個之情形設為◎，將1~10個之情形設為○，將11個以上之情形設為×。
關於接合線之1st接合性(球接合性)，對HTS試驗、HAST試驗、FAB形狀進行評價。關於HTS試驗，係藉由與本發明例1~59相同之方法進行。為了對HAST試驗中之球接合部之健全性進行評價，而將進行過接合之半導體裝置放置於溫度130℃、相對濕度85%RH(Relative Humidity)、5V之高溫高濕爐中，每隔48小時取出並對其進行評價。作為評價方法，測定電阻，將電阻上升者設為NG。將直至成為NG之時間為480小時以上之情形設為◎，將384小時以上且未達480小時之情形設為○，將未達384小時之情形設為×。
關於FAB形狀，於引線框架製作100根FAB，藉由SEM進行觀察。將真球狀者設為OK，將偏芯、收縮設為NG，對其數量進行計數。FAB形狀係將NG為0個之情形設為◎，將1~5個之情形設為○，將6~10個之情形設為△，將11個以上之情形設為×。◎與○為合格，△為雖然合格但品質略微不良。表9中之Ni、Pd及Pt之濃度(質量%*)表示Cu合金芯材中之濃度。
關於本發明例4-1~4-15，Cu合金芯材含有總計0.1~3.0質量%之選自Ni、Pd及Rt之一種以上之元素(元素週期表第10族之金屬元素)，且接合線最表面中之Cu濃度為1~10原子%。藉此，關於本發明例4-1~4-15，楔形接合部中之接合性及魚尾對稱性優異，HTS、FAB形狀及HAST亦良好。

Claims (11)

  1. 一種半導體裝置用接合線，其係具有Cu合金芯材、及形成於上述Cu合金芯材之表面之Pd被覆層者，且其特徵在於：上述接合線包含賦予高溫環境下之連接可靠性之元素，於對上述接合線之垂直於導線軸之方向之芯材剖面測定結晶方位之結果中，導線長度方向之結晶方位中相對於導線長度方向之角度差為15度以下之結晶方位<100>之方位比率為30%以上，且上述接合線之垂直於導線軸之方向之芯材剖面中之平均結晶粒徑為0.9~1.5μm。
  2. 如請求項1之半導體裝置用接合線，其中由下述(1)式定義之耐力比為1.1~1.6，耐力比=最大耐力/0.2%耐力 (1)。
  3. 如請求項1或2之半導體裝置用接合線，其中上述Pd被覆層之厚度為0.015~0.150μm。
  4. 如請求項1至3中任一項之半導體裝置用接合線，其於上述Pd被覆層上進而具有包含Au與Pd之合金表皮層。
  5. 如請求項4之半導體裝置用接合線，其中上述包含Au與Pd之合金表皮層之厚度為0.050μm以下。
  6. 如請求項1至5中任一項之半導體裝置用接合線，其中上述接合線包含選自Ni、Zn、Rh、In、Ir、Pt之至少1種以上之元素，且上述元素相對於導線整體之濃度總計為0.011~2質量%。
  7. 如請求項1至6中任一項之半導體裝置用接合線，其中上述接合線包含選自Ga、Ge之1種以上之元素，且上述元素相對於導線整體之濃度合計為0.011~1.5質量%。
  8. 如請求項1至7中任一項之半導體裝置用接合線，其中上述接合線包含選自As、Te、Sn、Sb、Bi、Se之1種以上之元素，上述元素相對於導線整體之濃度合計為0.1~100質量ppm，且Sn≦10質量ppm、Sb≦10質量ppm、Bi≦1質量ppm。
  9. 如請求項1至8中任一項之半導體裝置用接合線，其中上述接合線進而包含選自B、P、Mg、Ca、La之至少1種以上之元素，且上述元素相對於導線整體之濃度分別為1~200質量ppm。
  10. 如請求項1至9中任一項之半導體裝置用接合線，其中於上述接合線之最表面存在Cu。
  11. 如請求項1至10中任一項之半導體裝置用接合線，其中Cu合金芯材含有總計0.1~3.0質量%之元素週期表第10族之金屬元素，且導線最表面之Cu濃度為1原子%以上。
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