TW201843310A - 接合用成形體及其之製造方法 - Google Patents
接合用成形體及其之製造方法 Download PDFInfo
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- TW201843310A TW201843310A TW107110891A TW107110891A TW201843310A TW 201843310 A TW201843310 A TW 201843310A TW 107110891 A TW107110891 A TW 107110891A TW 107110891 A TW107110891 A TW 107110891A TW 201843310 A TW201843310 A TW 201843310A
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- Prior art keywords
- precursor
- bonding
- active agent
- core
- powder
- Prior art date
Links
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Classifications
-
- 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
- B23K35/22—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
- B22F1/17—Metallic particles coated with metal
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
-
- 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
- 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
- B23K35/22—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
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- 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
- B23K35/3601—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 with inorganic compounds as principal constituents
- B23K35/3603—Halide salts
-
- 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
- B23K35/40—Making wire or rods for soldering or welding
-
- 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
- H01L24/27—Manufacturing methods
-
- 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
-
- 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
- H01L24/31—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
-
- 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
- H01L24/74—Apparatus for manufacturing arrangements for connecting or disconnecting semiconductor or solid-state bodies
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Abstract
一種藉由Cu芯Sn殼粉末(2)之經壓縮的集合體而構成的接合用成形體(1)。於接合用成形體之表面部及內部之開空孔存在有除去粉末表面之氧化物用之活性劑含有物(4)。接合用成形體為分別含有55~95質量%之比例的Cu且45~5質量%之比例的Sn,接合用成形體具有20~400μm之厚度。
Description
本發明係關於中介存在於被接合構件的半導體晶片元件、LED晶片元件等之電子零件與基板之間,適於使用在將被接合構件的電子零件安裝於基板的接合用成形體及其製造方法。尚,本國際申請係根據在2017年3月31日已申請的日本國專利申請第71964號(日本特願2017-71964)主張優先權,將日本特願2017-71964之全內容援用於本國際申請。
近年,注目於在超過200℃的高溫亦進行動作,如SiC般的寬能隙半導體。作為在高溫下動作的半導體晶片元件之接合方法,注目於使包含Cu和Sn的接合材料中介存在於半導體晶片元件與基板之間,以高於Sn之融點的溫度加熱,將前述接合材料設為由Cu6
Sn5
或Cu3
Sn所構成的組成之金屬間化合物(Inter-Metallic Compound:IMC)的過渡液相燒結法(Transient Liquid Phase Sintering:TLP法)的接合方法。開示有根據此接合方法的適於高溫用途之Cu芯Sn殼粉末成形體(例如,參照非專利文獻1)。
非專利文獻1之Cu芯Sn殼粉末成形體係將粒徑30μm之Cu粒子滴下至無電解Sn鍍敷液而以約2~3μm厚之Sn層被覆後,將此等之粒子加壓而作為適於以下之用途之成形體。成形體中之各Cu粒子係以Sn層被覆而形成Cu芯Sn殼粉末構造。若將成形體加熱至232℃,則外殼之Sn層為熔融而與附近粒子之熔融Sn一體化,存在於粒子間之間隙的空隙係被排出至接合層外而緻密化。在此方法中Cu粒子係均勻地分布於接合面。若延長回流時間,則藉由Cu芯和Sn殼之相互擴散而形成Cu6
Sn5
及Cu3
Sn化合物。最後外殼之Sn係被完全地消耗而成為金屬間化合物(IMC)。Cu粒子係被Cu-Sn金屬間化合物(Cu6
Sn5
或Cu3
Sn)包圍,因為Cu6
Sn5
及Cu3
Sn之融點分別為415℃及676℃,所以至少可耐至415℃之高溫。 [先前技術文獻] [專利文獻]
非專利文獻1:Tianqi Hu et al., "Cu@SnCore-Shell Structure Powder Preform for High-Temperature Applications Based on Transient Liquid Phase Bonding", IEEE Transactions on Power Electronics, February 2016
[發明所欲解決之課題]
然而,記載於非專利文獻1的Cu芯Sn殼粉末成形體係於成形前之Cu芯Sn殼粉末之表面形成自然氧化膜的情況係將此成形體配置於被接合構件的半導體晶片元件與基板之間,即使回流,外殼之Sn亦難以浸潤至Cu粒子表面,難以用高強度將半導體晶片元件接合於基板。
本發明之目的係提供解決上述課題,初期接合強度高,且實現在冷熱循環試驗後亦維持高的接合強度的接合的接合用成形體及其製造方法。 [用以解決課題之手段]
本發明之第1之觀點係一種接合用成形體,其係藉由Cu芯Sn殼粉末經壓縮的集合體而構成的接合用成形體,其特徵為:於前述接合用成形體之表面部及內部之開空孔存在除去前述粉末表面之氧化物用之活性劑含有物,前述接合用成形體分別含有55~95質量%之比例的Cu且45~5質量%之比例的Sn,前述接合用成形體為具有20~400μm之厚度。在本說明書中,所謂「開空孔」係稱存在於接合用成形體內部的空孔之中,連通於接合用成形體之外表面的空孔(open pore),所謂「閉空孔」係稱在上述空孔之中,不連通於接合用成形體之外表面的空孔(closed pore)。
本發明之第2之觀點係一種接合用成形體之製造方法,其係包含在惰性氣體環境下,將平均粒徑為0.5~50μm之Cu芯Sn殼粉末以10~1000MPa之壓力進行壓製成形或輥軋壓延成形而得到厚度20~400μm之顆粒狀或薄片狀之成形體前驅物的步驟、與在惰性氣體環境下,將除去前述粉末表面之氧化物用之液狀之活性劑含有物貯藏於容器而於前述活性劑含有物中浸漬前述成形體前驅物的步驟、與在惰性氣體環境下,將前述已浸漬的成形體前驅物與前述容器一起減壓而由前述成形體前驅物內部之開空孔將存在於前述開空孔的氣體進行除氣的步驟、與在惰性氣體環境下,將已由前述開空孔除氣氣體的前述成形體前驅物復壓至常壓而於前述開空孔填充活性劑含有物的步驟、將附著於已填充活性劑含有物於前述開空孔的成形體前驅物之表面的剩餘之活性劑含有物而得到接合用成形體的步驟;前述Cu芯Sn殼粉末為分別含有55~95質量%之比例的Cu且45~5質量%之比例的Sn。 [發明的效果]
本發明之第1之觀點之接合用成形體係於藉由Cu芯Sn殼粉末之經壓縮的集合體而構成的接合用成形體之表面部及內部之開空孔,存在除去前述粉末表面之氧化物用之活性劑含有物。藉由此構造性的特徵,保存接合用成形體時,可防止接合用成形體之表面部和相臨上述開空孔的外殼之Sn之氧化。又,即使於接合用成形體之表面部及外殼之Sn層之表面形成自然氧化膜,於如電子零件與基板般的被接合構件之接合面配置此接合用成形體而接合之加熱(以下,稱為接合加熱。),則活性劑含有物中之活性劑可除去上述表面部及外殼之Sn層之氧化物,藉由此,Sn在短時間熔融而浸潤於Cu芯粒子表面而液相燒結快速地進行,同時Sn係與相鄰的Cu芯Sn殼粉末之外殼之Sn連接,可設為已一體化的接合層。如繼續接合加熱,則芯之Cu和殼之Sn之相互擴散產生而形成Cu芯粒子為被Cu6
Sn5
及Cu3
Sn化合物包圍而成的有高溫耐性的緻密的接合層,可實現初期接合強度高,且在冷熱循環試驗後亦維持高的接合強度的接合。又,在因於接合用成形體內部Cu殘存,使用此之接合用成形體而形成接合層的情況,於接合層亦可得到高的熱傳導性或導電性。
在本發明之第2之觀點之接合用成形體之製造方法係藉由壓製成形或輥軋壓延成形,可從接合加熱前之階段作為於內部空隙少的成形體,此結果,於接合加熱時變為容易使接合層緻密化。又,不僅如非專利文獻1般,僅將Cu芯Sn殼粉末加壓而製作成形體,而是將Cu芯Sn殼粉末進行壓製成形或輥軋壓延成形而製作成形體前驅物後,使成形體前驅物中之開空孔之內壁及成形體前驅物之表面部附著活性劑含有物,所以在非專利文獻1之方法係於Cu芯Sn殼粉末間形成間隙,亦即閉空孔及開空孔雙方者,但藉由此方法而接合用成形體之表面部及上述開空孔之內壁係以活性劑含有物被覆。該結果,可製作粉末相互間之接點多且活性劑含有物存在於上述表面部和上述開空孔的接合用成形體。特別是在上述表面部及上述開空孔成為沒有與大氣接觸,防止在保存接合用成形體時之氧化,同時於接合加熱時,活性劑除去上述表面部及上述開空孔表面之氧化物,液相燒結成為迅速地進行。
接下來,將用以實施本發明之形態,根據圖面來進行說明。
<第2之實施形態> 如第1圖所示,本發明之第1之實施形態之接合用成形體1係將於Cu芯Sn殼粉末2進行壓製成形而製作為20~400μm之顆粒狀或薄片狀。
[Cu芯Sn殼粉末] 作為接合用成形體之原料的Cu芯Sn殼粉末2係如第1(a)圖之放大圖所示,藉由以Cu所構成的芯2a、與以被覆此芯2a的Sn所構成的殼2b而構成。此Cu芯Sn殼粉末2之平均粒徑為0.5~50μm,理想為1.0~20μm。平均粒徑為未達下限值之0.5μm係在進行壓製成形或後述的輥軋壓延成形時,不僅難以製作均勻的密度之成形體前驅物,而且已知在25℃等之通常之操作材料的溫度下係在二層構造粒子之Cu與Sn界面,Cu之擴散為以數小時進行,在接合加熱時Sn液相產生之前之昇溫途中,外殼之Sn幾乎全量會成為Cu6
Sn5
,有接合性能惡化的不良狀況。另一方面,若平均粒徑為超過上限值之50μm,則於接合加熱時Sn為熔融而變得容易一體化,雖然Cu與Sn為相互擴散而形成金屬間化合物,但成為需要許多時間,有本發明之效果之一的短時間接合變為無法實現的不良狀況。又,在得到薄於被配置於二層構造的粉末之中心的Cu之粒徑的成形體前驅物的情況係有不僅使外殼之Sn且亦有使Cu變形的必要,但因為Cu係比Sn更硬而難以變形,所以若平均粒徑超過上限值之50μm,則Cu露出於最表面,Cu氧化而浸潤性變差,又因為表面部之Sn之存在比例減少,所以關於接合的液相之Sn為難以露出於接合面,有使接合性惡化的不良狀況。在此,粉末之平均粒徑(體積基準)係藉由雷射繞射散射法(堀場製作所公司製,LA960)而測定的值。
又,Cu芯Sn殼粉末2係在將Cu芯Sn殼粉末設為100質量%時,分別含有55~95質量%之比例的Cu、45~5質量%之比例的Sn。理想的含量係Cu為60~85質量%,Sn為40~15質量%。在Cu之含量超過95質量%而Sn之含量未達5質量%係有接合加熱時之燒結性低,接合層不一體化而接合強度低且熱阻抗變大的不良狀況。又,若Cu之含量未達55質量%而Sn之含量超過45質量%,則有接合層之最終組成物之高溫耐熱性低且變得無法得到所期待的性能的不良狀況。
作為製造Cu芯Sn殼粉末2的方法係可舉出將芯和殼雙方以濕式法製造的方法、和於芯使用Cu微細粉末,僅殼以濕式法製造的方法。在前者之製造方法係首先投入還原劑於Cu離子及Sn離子共存的水溶液,使氧化還原電位高的Cu還原析出,接著以覆蓋此Cu之方式使氧化還原電位低的Sn還原析出而製造Cu芯Sn殼構造之粉末前驅物。還原劑係亦可設為階段性地投入僅還原Cu的弱還原劑和亦還原Sn的強還原劑,分離Cu之還原析出反應和Sn之還原析出反應的操作。又,在後者之製造方法係亦可事先準備Cu微細粉末,使此高分散於含有Sn離子的水溶液,投入還原劑於此而在分散Cu微細粉末表面使Sn還原析出。又,於水溶液係在防止經合成的Cu芯Sn殼構造之粉末前驅物之凝聚的目的,亦可於水溶液調製時投入羥丙基甲基纖維素或聚乙烯吡咯啶酮等之分散劑。洗淨經合成的Cu芯Sn殼構造之粉末前驅物後,以回收乾燥,可得到Cu芯Sn殼構造之微細的粉末。
[成形體前驅物之製造] 如第1圖(b)及(c)所示之方式,在如氮、氬般的惰性氣體環境下,將Cu芯Sn殼粉末2以單軸壓製機10進行壓製成形而製作成形體前驅物3。單軸壓製機10係具有成為模具的模頭10a、上沖頭10b及下沖頭10c。藉由此單軸壓製機10,於製造成形體前驅物3係首先於模頭10a組合下沖頭10c的狀態,稱量特定量Cu芯Sn殼粉末2,由模頭10a之上沖頭插入孔投入至下沖頭10c上(第1圖(b))。無圖示,但以治具將Cu芯Sn殼粉末2由上方進行拍打而設為略均等的厚度。接著將上沖頭10b插入模頭10a而使其下降(第1圖(c))。藉由此上沖頭10b之加壓力,Cu芯Sn殼粉末2係變形,產生粉末間之互相纏繞或接著而成為獨立的成形體前驅物3。以如此的方式進行,用單軸壓製機10將Cu芯Sn殼粉末2進行單軸壓製而以成為20~400μm之特定之厚度之方式成形。成形壓力係因為以Cu芯Sn殼粉末2之粒徑或組成而變化,所以設為對應分別之微細粉末之粒徑、組成、形狀的壓力,故無法個別地限定,但在10~1000MPa之範圍進行壓製成形。此時,以觀察成形體前驅物3之剖面而由Cu和Sn之金屬成分以外所構成的空隙部之面積成為5%~0.1%之方式,決定投入粉末量,以成為上述特定之厚度之方式調整壓力。無圖示,但上述空隙部係由閉空孔及開空孔構成。已壓縮的集合體的成形體前驅物中,以符號2a表示芯之Cu(第1圖(c))。
在單軸壓製成形後,將上沖頭10b脫模,以第1圖(d)所示之方式,取出成形體前驅物3。藉由模具之形狀,可得顆粒狀或薄片狀之成形體前驅物。此成形體前驅物之形狀及尺寸係對應於被接合構件的電子零件之接合面之形狀及尺寸而決定。以單軸壓製成形所得到的成形體前驅物係藉由Cu芯Sn殼粉末之經壓縮的集合體而構成。成形體前驅物中之Cu係以55~95質量%之比例、Sn係以45~5質量%之比例分別包含。
[成形體前驅物之向活性劑含有物中之浸漬] 如第1圖(e)所示,將用以除去成形體前驅物內部之粉末表面之氧化物之液狀之活性劑含有物4貯藏於容器5。尚,液狀之活性劑含有物之黏度係調整為10-2
~10Pa・s。在如氮、氬般的惰性氣體環境下,於貯藏的活性劑含有物4中,浸漬上述已得到的成形體前驅物3。活性劑含有物4係含有活性劑成分的助焊劑、或含有活性劑成分的溶劑。作為活性劑係氫鹵酸胺鹽為理想,具體而言係可舉出三乙醇胺、二苯胍、乙醇胺、丁胺、胺基丙醇、聚氧乙烯油胺、聚氧乙烯月桂胺、聚氧乙烯硬脂胺、二乙胺、三乙胺、甲氧基丙胺、二甲基胺基丙胺、二丁基胺基丙胺、乙基己胺、乙氧基丙胺、乙基己氧基丙胺、雙丙胺、異丙胺、二異丙胺、哌啶、2,6-二甲基哌啶、苯胺、甲胺、乙胺、丁胺、3-胺基-1-丙烯、異丙胺 、二甲基己胺、環己胺等之胺之氫氯酸鹽或氫溴酸鹽。其中,環己胺氫溴酸鹽為理想。
作為上述溶劑係可舉出二乙二醇單己醚、二乙二醇單丁醚、二乙二醇單丁醚乙酸酯、四乙二醇、2-乙基-1,3-己二醇、α-萜品醇等之沸點為180℃以上的有機溶劑。此等之中,α-萜品醇為理想。在由含有活性劑成分的溶劑所構成的活性劑含有物係例如可舉出使活性劑成分含有於將癸二酸以5質量%之濃度溶解於α萜品醇的溶劑。
又,於助焊劑係於活性劑以外亦可包含上述溶劑、松香、搖變劑。於由含有活性劑成分的助焊劑所構成的活性劑含有物係例如可舉出無鉛焊料用之泛用助焊劑(92MS,荒川化學製)。被包含於助焊劑或溶媒的活性劑之含有比例係在助焊劑或溶媒中為0.01~2質量%,理想為0.5~1質量%。
[向成形體前驅物內部之開空孔之活性劑含有物之填充] 在如氮、氬般的惰性氣體環境下,將已浸漬於上述活性劑含有物中的成形體前驅物3與容器5一起減壓。減壓(真空度)係對應於活性劑含有物之黏度或被使用於活性劑含有物的溶劑之蒸氣壓而變化,但在被使用於活性劑含有物的溶劑之中,對於在25℃的蒸氣壓為最高值而以2倍以上之真空度,設定於0.1~5kPa之範圍,至成為不會在此減壓下由成形體前驅物確認有氣體產生之時間,保持30~600秒鐘。由此,使存在於成形體前驅物3內部之開空孔的氣體膨脹,由開空孔除氣。真空度及減壓時間為在未達上述範圍之下限值係上述除氣為無法充分地進行。在真空度及減壓時間為超過上述範圍之上限值的情況係蒸氣壓高的溶媒揮發而使填充於開空孔內的活性劑含有物之組成大幅地偏離,有無法發揮所期待的防氧化或除去表面氧化膜之機能的不良狀況。在進行上述減壓後,就上述惰性氣體環境下之原樣,將與容器5一起浸漬於活性劑含有物中的成形體前驅物3,花費300~1200秒鐘而復壓至常壓。由此,活性劑含有物4被填充於成形體前驅物3內部之開空孔。復壓而於開空孔填充活性劑含有物後,將成形體前驅物由容器取出,在惰性氣體環境下,擦拭除去已附著於成形體前驅物之表面的活性劑含有物,藉由必要而進行乾燥,得到第1圖(f)所示的接合用成形體1。
<第2之實施形態> 如第2圖所示,本發明之第2之實施形態之接合用成形體6係將與第1之實施形態相同之Cu芯Sn殼粉末2(第2圖(a))進行輥軋壓延成形而製作為20~400μm之薄片狀或顆粒狀。
[成形體前驅物之製造] 如第2圖(b)所示之方式,在如氮、氬般的惰性氣體環境下,將Cu芯Sn殼粉末2以粉末壓延機20進行粉末輥軋壓延成形而製作成形體前驅物7。粉末壓延機20係具有一對之圓柱狀之輥20a、20b和連接於此等之輥上面而設置的料斗20c。輥20a和輥20b係於相互相反方向旋轉,在第2圖係將被投入料斗20c的Cu芯Sn殼粉末2壓延於下方,壓延體係以導輥20d~20g而被導引於水平方向之方式構成。在輥軋壓延時之壓力係成為線壓,因為實際上難以確認及管理施加於被壓延成形的Cu芯Sn殼粉末的壓力,所以壓力係無法限定,但與第1之實施形態之單軸壓製成形同樣地,以成形體前驅物7成為20~400μm之特定之厚度之方式調整輥間間隙,同時觀察成形體前驅物7之剖面而空隙部成為5%~0.1%之方式,調整藉由料斗20c所得的Cu芯Sn殼粉末2之投入量。無圖示,但上述空隙部係由閉空孔及開空孔構成。已壓縮的集合體的成形體前驅物中,以符號2a表示芯之Cu(第2圖(b))。
在輥軋壓延成形係藉由將經壓延的成形體前驅物切斷至特定之尺寸,如第2圖(c)所示之方式,可得到薄片狀或顆粒狀之成形體前驅物7。此成形體前驅物7之形狀及尺寸係對應於被接合構件的電子零件之接合面之形狀及尺寸而決定。以輥軋壓延成形所得到的成形體前驅物係藉由Cu芯Sn殼粉末之經壓縮的集合體而構成。成形體前驅物中之Cu係以55~95質量%之比例、Sn係以45~5質量%之比例分別包含。
[成形體前驅物之向活性劑含有物中之浸漬及活性劑含有物向成形體前驅物內部之開空孔之填充] 第2之實施形態之活性劑含有物係與第1之實施形態之活性劑含有物相同,又,如第2圖(d)及(e)所示,輥軋壓延成形後之成形體前驅物之向活性劑含有物中之浸漬方法及活性劑含有物向成形體前驅物內部之開空孔之填充方法係因為與第1之實施形態相同,所以省略重複之說明。以如此的方式進行,得到第2之實施形態之接合用成形體6。在第2圖(d)及(e),各要素之符號係與附上第1圖(e)及(f)所示的要素的符號相同。
[使用接合用成形體的接合方法] 接著,說明關於使用以上述第1及第2之實施形態之方法製造的接合用成形體而將矽晶片元件接合於銅板之基板,將矽晶片元件安裝於基板之一例。首先將上述接合用成形體配置於銅板上,於接合用成形體之上搭載經Au濺鍍2.5mm□之背面的矽晶片元件。接著,使用接合爐,例如Malcom公司製SRS-1C,在氮氣環境下,施加0.1~100MPa之荷重,同時以最高溫度250~350℃條件進行1~15分鐘加熱保持處理。藉由此之接合加熱而接合用成形體中之活性劑除去粉末之外殼之Sn層之氧化物,而Sn為在短時間熔融,藉由Cu和Sn之相互擴散而以包圍芯之Cu之方式形成Cu-Sn之金屬間化合物(IMC),矽晶片元件與銅板為以高的接合強度接合。
此接合加熱之條件係依接合用成形體中之Cu芯Sn殼粉末之平均粒徑,上述加熱溫度及加熱時間為由上述範圍決定。Cu芯Sn殼粉末之平均粒徑越小,在上述範圍內決定較低的加熱溫度及較短的加熱時間,Cu芯Sn殼粉末之平均粒徑越大,在上述範圍內決定較高的加熱溫度及較長的加熱時間。在加熱溫度未達250℃或加熱時間未達1分鐘係即使平均粒徑為0.5μm,Sn亦難以熔融而不形成Cu-Sn之金屬間化合物粉末,接合強度不變高。又,在加熱溫度超過350℃的情況或加熱時間超過15分鐘的情況係有對於被接合構件的矽晶片元件帶來熱損傷的不良狀況。 [實施例]
接著將本發明之實施例與比較例一起詳細地說明。
<實施例1> 準備平均粒徑為0.5μm,Cu比例為75質量%且Sn之比例為25質量%之Cu芯Sn殼粉末。在此,Cu芯Sn殼粉末之Cu和Sn之組成比例係藉由ICP發光分光法(Thermo Fisher Scientific公司製,iCAP-6500 Duo)而測定。又,芯殼構造之晶體結構為主要由Cu及Sn構成之情事係藉由粉末X光繞射法(PANalytical公司製,多目的X光繞射裝置Empyrean)而確認。將上述Cu芯Sn殼粉末使用模具而以500MPa,單軸壓製300秒鐘,得到厚度100μm且3mm□之顆粒狀之成形體前驅物。
另一方面,以泛用助焊劑(荒川化學製92MS)之含量為成為10質量%之方式,得到將泛用助焊劑以有機溶劑之α-萜品醇稀釋的液狀之活性劑含有物。將此活性劑含有物50ml放入100ml玻璃燒杯之容器。將上述成形體前驅物浸漬於已貯藏於此容器的活性劑含有物中。將已浸漬成形體前驅物的已放入活性劑含有物的容器,放入真空乾燥器,在室溫下,以附屬之油旋轉真空泵將真空乾燥器庫內減壓,使存在連通於成形體前驅物之外表面的開空孔的氣體膨脹而由成形體前驅物除氣。真空度係設為1kPa,將此保持300秒後,花費600秒導入氮氣而慢慢回到常壓,使活性劑含有物填充於上述成形體前驅物之連通外表面的開空孔。將已填充活性劑含有物的成形體前驅物由容器取出,擦拭除去附著於表面的剩餘之活性劑含有物,得到厚度100μm且3mm□之顆粒狀之接合用成形物。
<實施例2~5及比較例1、2> 在實施例2~5及比較例1、2係如表1所示,關於用以製作接合用成形體之Cu芯Sn殼粉末之平均粒徑,使用與實施例1不同的平均粒徑之Cu芯Sn殼粉末,以與實施例1同樣之方式進行而得到接合用成形體。
<實施例6~9及比較例3、4> 在實施例6~9及比較例3、4係如表1所示,關於用以製作接合用成形體之Cu芯Sn殼粉末之Cu和Sn之組成,使用與實施例1不同的Cu和Sn之組成之Cu芯Sn殼粉末,以與實施例1同樣之方式進行而得到接合用成形體。
<實施例10~13及比較例5、6> 在實施例10~13及比較例5、6係如表1所示,關於製作接合用成形體時之單軸壓製成形時之成形荷重,以與實施例1不同的成形荷重,以與實施例1同樣之方式進行而得到接合用成形體。施加荷重的時間係與實施例1相同之300秒鐘。
<實施例14~17以及比較例7、8> 在實施例14~17以及比較例7、8係如表2所示,改變Cu芯Sn殼粉末之投入至模具的量,關於可得到的接合用成形體之厚度,成為與實施例1係不同的厚度。此外係以與實施例1相同的方式進行而得到接合用成形體。
<實施例18~22以及比較例9、10> 在實施例18~22以及比較例9、10係如表2所示,將成形方法變更為輥軋壓延成形,調整粉末壓延機之輥間間隙,關於可得到的接合用成形體之厚度,成為與實施例1係不同的厚度。此外係以與實施例1相同的方式進行而得到接合用成形體。
<比較評估> 將實施例1~22以及比較例1~10所得到的32種之接合用成形體分別裝於銅板上,於此搭載將背面經Au濺鍍2.5mm□之矽晶片元件。於矽晶片元件施加1MPa之荷重而已密著於銅板的狀態,使用回流爐,在氮環境下,以最高溫度300℃保持5分鐘,接合銅板和矽晶片元件,得到32種之接合樣本。關於此等之接合樣本,接著藉由所敘述的方法,進行初期接合強度試驗和冷熱循環試驗,進行評估。將該評估結果表示於表1及表2。
(1) 初期接合強度 接合強度係藉由晶片抗切測試機(A&D公司製,TENSILON萬能試驗機RTF-1310),分別固定32種之接合樣本之銅板,由矽晶片元件側面對與銅板平行方向施加力,測量矽晶片元件被剝落時之力或被破壞時之力(單位為牛頓,N),將此值除以接合面積2.5mm×2.5mm=6.25mm2
的值設為接合強度(單位為MPa)。
(2) 冷熱循環 將32種之接合樣本分別放入冷熱循環試驗機(espec 公司製,冷熱衝擊試驗裝置TSA―73ES),設定為下限溫度-40℃、上限溫度200℃,重複1000次降溫和昇溫,以與上述(1)之初期接合強度相同之方法測定接合強度,將以初期接合強度相除者設為冷熱循環特性。此係意味著如為1.00則已維持初期強度,如為0.50則意味著降低至初期強度之一半。
若由表1及表2比較實施例1~22與比較例1~10則可了解以下之情事。
在比較例1係因為使用平均粒徑為0.3μm的過度微細的Cu芯Sn殼粉末,所以經壓製成形的成形體之厚度偏差大,成形體為銅板和矽晶片元件(以下,稱為基板和元件。)之各面無法充分地接觸而無法實現充分的接合。
在比較例2係因為使用平均粒徑為60μm的過度粗大的Cu芯Sn殼粉末,所以液相之Sn產生,基板與元件之初期接合係該時為合適,但因為Cu擴散至Sn需要時間,所以在5分鐘之熱處理係無法充分地產生金屬間化合物,於冷熱循環試驗中亦進行伴隨體積變化的反應,無法充分地維持接合強度。
在比較例3係因為Cu芯Sn殼粉末中之Cu之含量過少至50質量%,Sn之含量為過多至50質量%,所以Cu芯會消滅,無法充分地緩和在冷熱循環試驗產生的應力而無法充分地維持接合強度。
在比較例4係因為Cu芯Sn殼粉末中之Cu之含量過多至97質量%,Sn之含量為過少至3質量%,所以Sn液相之產生量不充分且無法在與基板或元件之界面浸潤擴大而無法接合。因此無法進行初期接合強度試驗和冷熱循環試驗。
在比較例5係因為單軸壓製成形時之成形荷重為過低至5MPa,所以無法事先設為緻密的成形體。因此,已熔融的Sn相互間之接觸為困難,無法得到已一體化的接合層而初期接合強度為低的值。
在比較例6係因為單軸壓製成形時之成形荷重為過高至2000MPa,所以成形體變硬而成形物為難以變形,插入至基板與元件之間而即使加壓加熱,亦無法追隨基板或元件之彎曲而變形而無法充分地確保接觸面,所以已熔融的Sn無法充分地浸潤擴大,初期接合強度不成為充分高的值。
在比較例7係因為單軸壓製成形後之成形體之厚度為過薄至15μm,所以由接合層產生的Sn液相量不充分且無法充分地浸潤擴大於基板或元件而初期接合強度之值不成為充分的值。
在比較例8係因為單軸壓製成形後之成形體之厚度為過厚至450μm,所以Sn液相係因為充分地產生所以可得初期接合強度,但因為熱阻抗不小,所以難以由成形體放熱而無法在冷熱循環試驗維持初期強度。
在比較例9係因為輥軋壓延成形後之成形體之厚度為過薄至15μm,所以由接合層產生的Sn液相量不充分且無法充分地浸潤擴大於基板或元件而初期接合強度之值不充分。
在比較例10係因為輥軋壓延成形後之成形體之厚度為過厚至450μm,所以Sn液相係因為充分地產生所以可得初期接合強度,但因為熱阻抗不小,所以難以由成形體放熱而無法在冷熱循環試驗維持初期強度。
對於此,實施例1~22之接合樣本係因為具備規定於第1之觀點的要件,且使用以規定於第2之觀點的要件而製造的接合用成形體而得到的樣本,所以初期接合強度係高至37~59MPa,又,冷熱循環係在0.68~0.98之範圍,未見到因冷熱循環試驗所致的接合強度之降低。 [產業上之可利用性]
本發明係可合適地利用於曝露於高溫環境的電子零件之安裝。
1‧‧‧接合用成形體
2‧‧‧Cu芯Sn殼粉末
2a‧‧‧芯
2b‧‧‧殼
3‧‧‧成形體前驅物
4‧‧‧活性劑含有物
5‧‧‧容器
10‧‧‧單軸壓製機
10a‧‧‧模頭
10b‧‧‧上沖頭
10c‧‧‧下沖頭
20‧‧‧粉末壓延機
20a‧‧‧輥
20b‧‧‧輥
20c‧‧‧料斗
20d‧‧‧導輥
20e‧‧‧導輥
20f‧‧‧導輥
20g‧‧‧導輥
[第1圖]模式性地表示藉由壓製成形而製造本發明之第1之實施形態之接合用成形體的步驟的圖。 [第2圖]模式性地表示藉由輥軋壓延成形而製造本發明之第2之實施形態之接合用成形體的步驟的圖。
Claims (2)
- 一種接合用成形體,其係藉由Cu芯Sn殼粉末之經壓縮的集合體而構成的接合用成形體,其特徵為: 於前述接合用成形體之表面部及內部之開空孔存在有除去前述粉末表面之氧化物用之活性劑含有物, 前述接合用成形體分別含有55~95質量%之比例的Cu且45~5質量%之比例的Sn, 前述接合用成形體具有20~400μm之厚度。
- 一種接合用成形體之製造方法,其特徵為:包含在惰性氣體環境下,將平均粒徑為0.5~50μm之Cu芯Sn殼粉末,以10~1000MPa之壓力進行壓製成形或輥軋壓延成形而得到厚度20~400μm之顆粒狀或薄片狀之成形體前驅物的步驟,與 在惰性氣體環境下,將除去前述粉末表面之氧化物用之液狀之活性劑含有物貯藏於容器而將前述成形體前驅物浸漬於前述活性劑含有物中的步驟,與 在惰性氣體環境下,將前述已浸漬的成形體前驅物與前述容器一起減壓而由前述成形體前驅物內部之開空孔使存在於前述開空孔的氣體除氣的步驟,與 在惰性氣體環境下,將由前述開空孔已除氣氣體的前述成形體前驅物復壓至常壓而於前述開空孔填充活性劑含有物的步驟,與 除去附著於在前述開空孔經填充活性劑含有物的成形體前驅物之表面的剩餘之活性劑含有物而得到接合用成形體的步驟; 前述Cu芯Sn殼粉末含有55~95質量%之比例的Cu且45~5質量%之比例的Sn。
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CN104209661A (zh) * | 2014-08-19 | 2014-12-17 | 西安三威安防科技有限公司 | 一种焊锡膏的制备方法 |
JP6434885B2 (ja) | 2015-10-07 | 2018-12-05 | 大日本コンサルタント株式会社 | 斜張橋の架設方法 |
CN105290418B (zh) * | 2015-10-14 | 2018-09-07 | 哈尔滨工业大学深圳研究生院 | 一种微纳米铜球表面镀附具有可焊性厚度的厚锡层的镀附方法 |
CN106181132B (zh) * | 2016-07-15 | 2018-07-20 | 哈尔滨工业大学深圳研究生院 | 一种基于Ag@Sn核-壳结构的高温钎料制备方法 |
CN106271177B (zh) * | 2016-09-23 | 2018-10-26 | 哈尔滨工业大学深圳研究生院 | 一种互连钎料及其互连成形方法 |
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EP3603875A4 (en) | 2020-12-16 |
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TWI734903B (zh) | 2021-08-01 |
JP6897237B2 (ja) | 2021-06-30 |
WO2018180326A1 (ja) | 2018-10-04 |
JP2018171636A (ja) | 2018-11-08 |
CN110418692B (zh) | 2021-11-12 |
CN110418692A (zh) | 2019-11-05 |
KR102393695B1 (ko) | 2022-05-02 |
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