TW201611198A - 低壓燒結粉末 - Google Patents

低壓燒結粉末 Download PDF

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Publication number
TW201611198A
TW201611198A TW104111292A TW104111292A TW201611198A TW 201611198 A TW201611198 A TW 201611198A TW 104111292 A TW104111292 A TW 104111292A TW 104111292 A TW104111292 A TW 104111292A TW 201611198 A TW201611198 A TW 201611198A
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Taiwan
Prior art keywords
sintered
film
metal particles
slurry
acid
Prior art date
Application number
TW104111292A
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English (en)
Inventor
戈夏爾夏密克
恰奇尼馬雅庫瑪
羅伊寶拉米希谷帕塔
沙卡蘇利
魯斯托基安紐布哈弗
Original Assignee
阿爾發金屬公司
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Application filed by 阿爾發金屬公司 filed Critical 阿爾發金屬公司
Publication of TW201611198A publication Critical patent/TW201611198A/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
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • 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
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
    • 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
    • B22F7/02—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 layers
    • B22F7/04—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 layers with one or more layers not made from powder, e.g. made from solid metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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    • B23K1/0016—Brazing of electronic components
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    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3006—Ag as the principal constituent
    • 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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    • B23K35/22—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
    • 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
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    • B23K35/3613—Polymers, e.g. resins
    • 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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    • B23K35/3618—Carboxylic acids or salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F7/02—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 layers
    • B22F7/04—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 layers with one or more layers not made from powder, e.g. made from solid metal
    • B22F2007/042—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 layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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    • B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
    • B22F2301/255—Silver or gold
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

一種燒結粉末，包含：平均最長尺寸從100nm至50μm的第一類型金屬顆粒。

Description

低壓燒結粉末
本發明係關於一種燒結粉末、一種燒結漿料及包含該燒結粉末的膜、以及一種使用該燒結粉末形成的燒結接點。
燒結接點提供了焊接接點的替代方案。典型的形成燒結接點的方法涉及將金屬粉末(時常處於粉末壓塊的形式)放在兩個待接合的工件之間，然後將該金屬粉末燒結。產生的金屬原子之原子擴散在該兩個工件之間形成了黏合。
在電子工業中金屬奈米粉末已被用於形成燒結接點，並且被視為是無鉛焊接的可用替代方案。奈米材料與對應的塊體材料之間的不同行為被認為是由於奈米材料具有較高的表面積對體積比。
含銀奈米顆粒的燒結粉末是習知的。由銀奈米顆粒的原子擴散所形成的燒結接點可以在明顯低於塊體熔化溫度的溫度下進行處理，也可用於高溫的應用。諸如高溫穩定性、高的電和熱傳導性、以及良好的機械性能等潛在優勢使得這種燒結粉末有望成為晶粒黏附應用的候選品。然而，這種燒結粉末的燒結溫度對於有效用於大多數的電子應用來說仍然太高。
燒結溫度可以藉由在燒結過程中施加外部壓力來降低。銀漿料的壓力輔助低溫燒結已被證明是晶粒黏附方法中焊料回流的可行替代方案。高壓的施加已被證明可顯著降低燒結溫度，而且可以以相對較快的速率實現晶粒黏附所需的性質，從而導致燒結接點在幾分鐘內形成。然而，大的外部壓力使得製程的自動化困難。此外，施加大的外部壓力可能會導致工件損壞。
分配焊接漿料用於各種應用是習知的，但大多數是作為波焊或網版印刷不可行時的替代方案。在各種表面黏著應用上焊接漿料可被分配在印刷電路板、積體電路封裝、及電元件連接器上。通常焊接漿料的問題包括：滴出、跳點、及不一致的分配。在電子產業中通常將軟和硬的焊料用於晶粒黏附和分配。軟焊料在熱循環條件下容易疲勞失效。另一方面，硬焊料和玻璃基質複合物被用來使裝置能夠在更高的接面溫度下運行，但硬焊料和玻璃基質複合物的較高彈性模數和處理溫度會在裝置中產生高的機械應力，而且這些材料也具有相對低的熱和電傳導度。
本發明尋求解決至少一些與現有技術相關的問題或至少對該等問題提供商業上可接受的替代解決方案。
在第一態樣中，本發明提供一種燒結粉末，包含：第一類型金屬顆粒，具有100nm至50μm的平均最長尺寸。
本文中定義的各個態樣或實施例可以與任何其他的態樣或實施例組合，除非有明確相反的指示。特定言之，可以將任何被指示為較佳或有利的特徵與任何其他被指示為較佳或有利的特徵組合。
本文中使用的術語「燒結粉末」可以包含能夠形成燒結接點的粉末。燒結接點是由被放在兩個待接合工件之間的金屬顆粒原子擴散所形成的。術語「燒結粉末」可以包含微粒。燒結粉末可以包含規則形狀的顆粒(例如球體)或不規則形狀的顆粒(例如細絲、板、棒或薄片)。
本文中使用的術語「包覆劑」可以包含當存在於金屬顆粒的表面上時減少金屬顆粒附聚、能夠在粉末生產的過程中控制粒徑、及減少顆粒的表面氧化或其他污染的物種。
本發明人驚奇地發現到，本文所述的燒結粉末可以在低溫下、且只施加極低壓力(通常大致上沒有壓力)下進行燒結。結果，使用該燒結粉末在工件之間形成燒結接點可以在減少對工件的損傷下發生。此外，由於高壓的施加不是必要的，故燒結接點的形成是簡化的，而且可以更容易被自動化。此外，與奈米尺寸的顆粒相比，可以藉由只使用少量的包覆劑來避免第一類型金屬顆粒附聚。因此，與只包含奈米尺寸顆粒的燒結粉末相比，所得燒結接點中包含的殘餘有機物量減少了，從而改良了接點的機械性能。
第一類型金屬顆粒具有從100nm至50μm的平均最長尺寸。大於50μm的平均最長尺寸可能會導致低的表面積對體積比，因此需要更高的燒結溫度及/或壓力。小於100nm的平均最長尺寸可能需要不利水平的包覆劑。通常第一類型金屬顆粒的大部分顆粒具有從100nm至50μm的最長尺寸，更通常是大致上所有形成第一類型金屬顆粒的顆粒都具有從100nm至50μm的最長尺寸。當形成微粒的顆粒是球形的時，該最長尺寸將是球的直徑。本文所指的平均最長直徑可以使用粒徑分析儀以動態光散射法或雷射散射法進行量測。
第一類型金屬顆粒可以全都包含相同的金屬。或者，一些顆粒可以包含不同的金屬。此外，個別的顆粒可以包含兩種或更多種不同的金屬。本文中使用的術語「金屬」可以包含合金或核-殼結構。因此，該等顆粒可以包含一種或更多種合金或一種或更多種金屬的合金或核-殼結構。
較佳的是，至少一部分的第一類型金屬顆粒被至少部分塗覆包覆劑。使用包覆劑可有助於減少顆粒的附聚。這種附聚是不利的，因為可能會提高燒結粉末的燒結溫度。因此，使用包覆劑使得工件之間的燒結接點能夠在較低溫度下形成，因此，可以有助於減少因曝露於高的燒結溫度而對工件造成的損壞。此外，使用包覆劑可有助於避免金屬劣化，例如因金屬曝露於空氣所造成的損壞。
在本實施例中，金屬顆粒可以大致上被包覆劑包覆，或被包覆劑完全包覆。提高包覆劑對金屬顆粒的包覆率可以有助於進一步減少金屬顆粒的附聚，並因此進一步降低燒結溫度。此外，大多數的金屬顆粒可以被包覆劑包覆，或大致上所有的金屬顆粒可以都被包覆劑包覆。
包覆劑較佳包含羧酸酯及/或胺官能基。
燒結粉末較佳包含多達5wt%的包覆劑，更佳為0.1至3wt%的包覆劑，甚至更佳約0.5wt%的包覆劑。在這方面所用的術語「wt%」是基於燒結粉末的總重量計。假使燒結粉末包含超過5wt%的包覆劑，則在燒結之前可能需要較高的溫度來熔化包覆劑。此外，所得燒結接點中所含的有機物之量可能會增加。假使燒結粉末包含少於0.1wt%的包覆劑，則包覆劑可能不足以覆蓋金屬的表面。這可能會導致顆粒的附聚增加，並因此提高燒結溫度。第一類型金屬顆粒的大小與低量包覆劑的組合可產生強的生成接點、低的需求燒結溫度和壓力、及減少的顆粒附聚的組合。
第一類型金屬顆粒較佳具有從100nm至20μm、更佳從150nm至15μm、甚至更佳從200nm至10μm的平均最長直徑。
第一類型金屬顆粒較佳具有從1至3μm的D50值(即在50%累積分佈的粒徑值)。這可以提供特別有利的燒結特性。D50可以使用粒徑分析儀以動態光散射法或雷射散射法進行量測。
第一類型金屬顆粒較佳具有從3.5至5.5g/cc的振實密度。振實密度可以在標準程序下使用振實密度計進行量測。較高的振實密度表示在燒結之前金屬顆粒存在較低的附聚程度。
該燒結粉末可以包含平均最長尺寸小於100μm的第二類型金屬顆粒，其中該第二類型金屬顆粒被至少部分塗覆包覆劑。第一和第二類型金屬顆粒的組合增加了形成燒結粉末的顆粒之接觸點。這可以產生更好的燒結而且還 改良粉末的形態。因此，使用這種粉末形成的接點之熱循環性可提高。此外，較大的第一類型顆粒通常只需要低水平的包覆劑。因此，相較於只包含奈米大小的顆粒的燒結粉末，該燒結粉末中的包覆劑總量可以減少，從而最大限度地減少存在於任何形成接點中的殘餘有機物。結果，熱傳導率和諸如熱循環的高溫性能可得到改良。通常第二類型金屬顆粒的多數顆粒具有小於100μm的最長尺寸，更通常是大致上形成第二類型金屬顆粒的所有顆粒都具有小於100μm的最長尺寸。
在一個實施例中，第二類型金屬顆粒較佳具有從1至100nm、較佳從5至75nm的平均最長尺寸。在本實施例中，通常第二類型金屬顆粒的多數顆粒具有在這些範圍內的最長尺寸，更通常是大致上形成第二類型金屬顆粒的所有顆粒都具有在這些範圍內的最長尺寸。
燒結粉末較佳包含1至19wt%的第一類型金屬顆粒及81至99wt%的第二類型金屬顆粒，較佳5至15wt%的第一類型金屬顆粒及85至95wt%的第二類型金屬顆粒。這樣的範圍特別適合用於提供改良熱傳導率和熱循環性能、及低燒結溫度的組合。在較佳的實施例中，微粒包含約10wt%的第一類型顆粒及約90wt%的第二類型顆粒。
第一類型金屬顆粒及/或第二類型金屬顆粒較佳包含銀或銀的一種合金或多種合金或核-殼結構。銀具有優異的電和熱傳導性，因此能夠形成具有高的電及/或熱傳導率的燒結接點。因此，使用銀金屬使燒結粉末特別適用於電子應用，例如晶粒黏附和微電子封裝。適當的銀合金包括例如AgSn、AgPd、AuAg、AgCu及AgNi。金屬顆粒可以包含塗覆銀的顆粒之核-殼結構，例如塗覆銀的銅、塗覆銀的鎳、塗覆銀的CuNi、塗覆銀的CuNiZn及塗覆銀的BN。
第一類型金屬顆粒的包覆劑可以是無機及/或有機的。有機包覆劑的實例包括聚合物和配位體。第一類型金屬顆粒的包覆劑較佳包含胺及/或羧酸官 能基。這樣的包覆劑可與金屬顆粒形成弱鍵結。因此打斷鍵結所需的溫度可以降低，此可有助於降低燒結溫度。在這方面，包含酸官能基的包覆劑是特別較佳的。
第一類型金屬顆粒的包覆劑較佳包含直鏈羧酸(C6至C22)或支鏈脂族羧酸。一個較佳的實例是油酸。油酸與金屬顆粒形成特別弱的鍵結。此外，油酸在減少金屬顆粒附聚上特別有效。
第二類型金屬顆粒的包覆劑可以是無機及/或有機的。有機包覆劑的實例包括聚合物和配位體。第二類型金屬顆粒的包覆劑較佳包含胺及/或羧酸官能基。這樣的包覆劑可與金屬顆粒形成弱鍵結。因此打斷鍵結所需的溫度可以降低，此可有助於降低燒結溫度。在這方面，包含胺官能基的包覆劑是特別較佳的。
第二類型金屬顆粒的包覆劑較佳包含直鏈烷胺(C6至C18)或支鏈脂族烷胺。一個較佳的實例是辛胺。辛胺與金屬顆粒形成特別弱的鍵結。此外，辛胺在減少金屬顆粒附聚上特別有效。
在特別較佳的實施例中，該燒結粉末包含：從1至10wt%的第一類型金屬顆粒，該第一類型金屬顆粒具有從100nm至20μm的平均最長尺寸，該金屬顆粒至少部分塗覆有油酸包覆劑；以及從90至99wt%的第二類型金屬顆粒，該第二類型金屬顆粒具有從5至75nm的平均最長尺寸，其中該第二類型金屬顆粒係至少部分塗覆有辛胺包覆劑。
在進一步的態樣中，本發明提供一種燒結粉末，包含：具有小於10μm的平均最長尺寸的金屬顆粒，其中至少一些該金屬顆粒係至少部分塗覆有包覆劑。
這樣的燒結粉末可以在特別低的溫度下進行燒結且僅施加極低的壓力，通常大致上沒有壓力。結果，使用該燒結粉末在工件之間形成燒結接點可 以在減少對工件的損傷下發生。此外，由於高壓的施加不是必要的，故燒結接點的形成是簡化的，而且可以更容易被自動化。
金屬顆粒較佳具有1至100nm、更佳5至75nm、甚至更佳5至65nm的平均最長尺寸。這種平均最長尺寸可以在提供高的表面積對體積比特別有效。平均最長尺寸小於1nm的金屬顆粒可能難以處理，而且還可能更容易劣化。
金屬顆粒可以具有500nm至5μm的平均最長尺寸。較大的粒徑可以需要較少的包覆劑。因此，由於生成的接點中殘餘有機物減少，故電阻率是遠較低的。在本發明的一個態樣中，金屬顆粒具有100nm至10μm、較佳500nm至3μm的平均最長直徑，並且包含少於3wt%的包覆劑，通常包含約0.5wt%的包覆劑。
當金屬顆粒具有在以上指示範圍中的平均最長尺寸時，通常大部分的顆粒具有在該範圍內的最長尺寸，更典型的是大致上所有的顆粒都具有在該範圍內的最長尺寸。
微粒通常表現出不同的粒徑。例如，最大10%顆粒的平均最長尺寸與最小10%顆粒的平均最長尺寸之間的差異可以大於20nm，通常大於30nm，甚至更通常是大於60nm，還甚至更通常是從60至150nm。不同粒徑可以有助於降低燒結粉末的燒結溫度，這可能是由於顆粒之間的大接觸點。此外，這種不同尺寸可以有助於提高填充分率。
包覆劑可以是無機及/或有機的。有機包覆劑的實例包括聚合物和配位體。包覆劑較佳包含胺及/或羧酸官能基。這種包覆劑可以與金屬顆粒形成弱鍵結。因此，打斷鍵結所需的溫度可以降低，這可以有助於降低燒結溫度。在這方面，包含胺官能基的包覆劑是特別較佳的。
包覆劑較佳包含直鏈烷胺(C6至C18)或支鏈脂族烷胺。一個較佳的實例是辛胺。辛胺與金屬顆粒形成特別弱的鍵結。此外，辛胺在減少金屬顆粒附聚上特別有效。
金屬較佳包含銀或銀的一種合金或多種合金或核-殼結構。銀具有優異的電和熱傳導性，因此能夠形成具有高的電及/或熱傳導率的燒結接點。因此，使用銀金屬使燒結粉末特別適用於電子應用，例如晶粒黏附和微電子封裝。或者，金屬可以包含其他的金屬，例如銅和金。
在進一步的態樣中，本發明提供一種燒結粉末，包含：平均最長直徑小於10μm的微粒，其中至少一些形成該微粒的顆粒包含至少部分塗覆有包覆劑的金屬。
在進一步的態樣中，本發明提供一種燒結粉末，包含：平均最長直徑小於10μm的微粒，其中至少一些形成該微粒的顆粒包含至少部分塗覆有包覆劑的金屬，其中該微粒包含最長直徑從大於100nm至50μm的第一類型顆粒及最長直徑從1至100nm的第二類型顆粒，其中該微粒包含5至15wt%的該第一類型顆粒及85至95wt%的該第二類型顆粒。
在進一步的態樣中，本發明提供一種使用本文所述的燒結粉末形成的燒結接點。這種燒結接點可以表現出特別高的強度及/或特別高的電和熱傳導率。此外，該燒結接點可以在熱衝擊之後表現出非常小的切變強度變化，通常大致上沒有切變強度的變化。
在進一步的態樣中，本發明提供一種包含本文所述的燒結接點之LED(發光二極體)、MEMS(微機電系統)、OLED(有機發光二極體)或PV電池(光伏電池)。
在進一步的態樣中，本發明提供一種燒結漿料，包含：本文所述的燒結粉末； 黏結劑；溶劑；以及可選的流變改質劑及/或有機銀化合物及/或活化劑及/或界面活性劑及/或潤濕劑及/或過氧化氫或有機過氧化物。
該漿料可以是可印刷的及/或可分配的及/或可噴射的及/或針可轉移的。該漿料可以具有特別有利於分配的黏度和流動特性，這意味著該漿料可被用於一對一取代焊料。
與所屬技術領域中習知的燒結漿料相比，本發明的燒結漿料在室溫下表現出高的穩定性。這意味著不需要低溫貯藏燒結漿料。此乃本發明之燒結漿料特別重要的優點。
黏結劑及/或溶劑的選擇通常使得黏結劑及/或溶劑能夠在低於燒結粉末之目標燒結溫度的溫度下被從漿料中去除(例如藉由蒸發及/或燒掉)。這可以有助於促進金屬顆粒幾乎完全燒結。當燒結過程中有機材料保持在接點中時，可能會發生金屬顆粒不充分燒結。此舉可能會產生弱的燒結接點。
黏結劑可用於將漿料黏結在一起，使得處理和精確定位在所需燒結接點的位置更為容易。適當的黏結劑之實例包括、但不限於熱塑性聚合物，例如聚(甲基丙烯酸甲酯)、聚醯胺、聚乙烯、聚丙烯、聚苯乙烯；或熱固性聚合物，例如聚氨酯、聚氰酸酯、環氧樹脂、聚醯亞胺、三聚氰胺樹脂及雙馬來醯亞胺樹脂。特別較佳的實例包括羥丙基甲基纖維素、三乙醯甘油及聚乙酸乙烯酯。黏結劑較佳包含環氧基樹脂。環氧基樹脂可以是在將漿料黏結在一起時特別有效的，以使漿料更容易處理而且可以更容易精確定位在所需燒結接點的位置。此外，使用環氧樹脂可以導致燒結之前有更強的接點形成，這意味著在燒結之前不需要將待接合的工件保持在一起。當包覆劑包含胺官能基時，使用環氧樹 脂是特別有利的。在這種情況下，胺作為形成交聯結構的硬化劑。這可以在燒結之前產生特別強的接合。
溶劑較佳包含單萜醇及/或二醇及/或二醇醚，較佳為萜品醇及/或二乙二醇單正丁基醚。單萜醇及/或二醇醚可以是在漿料中分散金屬顆粒特別有效的，從而導致金屬顆粒均勻分佈在團簇凝聚及/或附聚減少的有機成分基質中。使用單萜醇及/或二醇醚可用以提高燒結漿料的流動能力和印刷能力。
可以添加流變改質劑來控制漿料的黏度。適當的流變改質劑之實例包括、但不限於短或長鏈(C=2至30)羧酸或二羧酸或羥基羧酸，例如月桂酸、硬脂酸、新癸酸、硬脂酸、油酸、草酸、丙二酸、琥珀酸、己二酸、馬來酸、檸檬酸、乳酸，或短或長鏈(C=2至30)胺，例如丁胺、己胺、辛胺、十二烷胺、十六烷胺、Thixcin R及Crayvallac Super、或上述中之兩者或更多者的組合。
在燒結過程中，有機銀化合物可以分解成金屬銀，從而可以提高燒結接點的熱傳導率。此外，有機銀化合物的存在可增加漿料對接合界面的潤濕性。有機銀化合物可以包含短或長鏈羧酸(C=1至30)中之一者或更多者，例如硬脂酸銀、棕櫚酸銀、油酸銀、月桂酸銀、新癸酸銀、癸酸銀、辛酸銀、己酸銀、乳酸銀、草酸銀、檸檬酸銀、乙酸銀及琥珀酸銀。在一些實施例中，可以省去有機銀化合物。
可以添加活化劑來從被印刷的表面去除任何可能存在的金屬氧化物及/或去除可能存在燒結粉末中的任何氧化物。可以使用芳基或烷基羧酸作為活化劑，例如己二酸、琥珀酸及戊二酸中之一者或更多者。
可以添加界面活性劑到燒結漿料中以有助於將燒結粉末分散在燒結漿料中。合適的界面活性劑之實例包括、但不限於Disperbyk 163、IGEPAL CA-630、月桂基葡糖苷及TritonX 100。
燒結漿料較佳進一步包含過氧化物。合適的過氧化物之實例包括、但不限於過氧化氫或有機過氧化物，例如叔丁基氫過氧化物和叔丁基過氧-2-乙基己酸酯。過氧化物將氧引入漿料中，在晶粒黏附法中過氧化物可幫助晶粒區域下方的漿料進行燒結。氧也可以使金屬顆粒能夠在惰性氛圍下進行燒結，該惰性氛圍例如氮氣氛圍。燒結漿料較佳包含多達3wt%的過氧化氫或有機過氧化物，較佳為0.5至2wt%的過氧化氫或有機過氧化物，更佳為0.7至1.8wt%的過氧化氫或有機過氧化物。液體過氧化物對於控制流變性和銀沉澱是較佳的。
燒結漿料較佳包含：從1至15wt%的黏結劑；及/或從1至30wt%的溶劑；及/或多達5wt%的流變改質劑；及/或多達10wt%的有機銀化合物；及/或多達2wt%的活化劑；及/或多達6wt%的界面活性劑；及/或多達2wt%的過氧化氫或有機過氧化物。
這些範圍內的黏結劑及/或溶劑含量可有助於提供具有特別理想的流動能力和印刷能力的燒結漿料。燒結漿料較佳包含2至8wt%的黏結劑。在一個實施例中，燒結漿料包含約4.5wt%的黏結劑。燒結漿料較佳包含5至30wt%的溶劑。在一個實施例中，燒結漿料包含約26wt%的溶劑。燒結漿料可以包含0至5wt%的流變改質劑及/或0至2wt%的活化劑及/或0至6wt%的界面活性劑及/或0至2wt%的過氧化氫或有機過氧化物。燒結漿料可以包含從62至90wt%的燒結粉末。燒結粉末可以形成燒結漿料的剩餘部分。
在進一步的態樣中，本發明提供一種燒結漿料，包含：本文中揭示的燒結粉末； 有機銀化合物；溶劑；以及可選的活化劑及/或流變改質劑及/或界面活性劑及/或過氧化氫或有機過氧化物。
在燒結過程中，有機銀化合物可以分解成金屬銀，金屬銀可以提高燒結接點的導熱率。此外，有機銀化合物的存在提高了漿料對接合界面的潤濕性。有機銀化合物可以包含短或長鏈羧酸(C=1至30)中之一者或更多者，例如硬脂酸銀、棕櫚酸銀、油酸銀、月桂酸銀、新癸酸銀、癸酸銀、辛酸銀、己酸銀、乳酸銀、草酸銀、檸檬酸銀、乙酸銀及琥珀酸銀。在一些實施例中，可以省去有機銀化合物。
燒結漿料較佳進一步包含脂肪酸及/或潤濕劑，較佳為以下中之一者或更多者：短或長鏈(C=2至30)羧酸或二羧酸或羥基羧酸，更佳為月桂酸、硬脂酸、新癸酸、硬脂酸、油酸、草酸、丙二酸、琥珀酸、己二酸、馬來酸、檸檬酸或乳酸；或短或長鏈(C=2至30)胺，更佳為丁胺、己胺、辛胺、十二烷胺或十六烷胺；或界面活性劑，更佳為triton X100、IGEPAL CA-630或月桂基葡糖苷。
脂肪酸的存在有助於將漿料黏結在一起。換句話說，脂肪酸的存在避免了個別黏結劑的需求，例如以上討論的環氧基樹脂黏結劑。因此，漿料中的有機物之總量較少，從而產生較強的最終接點。
燒結漿料較佳進一步包含過氧化物。合適的過氧化物之實例包括、但不限於過氧化氫或有機過氧化物，例如叔丁基氫過氧化物和叔丁基過氧-2-乙基己酸酯。過氧化物將氧引入漿料中，在晶粒黏附法中過氧化物可幫助晶粒區域下方的漿料進行燒結。氧也可以使金屬顆粒能夠在惰性氛圍下進行燒結，該惰性氛圍例如氮氣氛圍。燒結漿料較佳包含多達3wt%的過氧化氫或有機過氧化 物，較佳為0.5至2wt%的過氧化氫或有機過氧化物，更佳為0.7至1.8wt%的過氧化氫或有機過氧化物。液體過氧化物對於控制流變性和銀沉澱是較佳的。
燒結漿料可以包含膜成形劑，例如聚醯胺、聚異丁烯、聚醯胺蠟流變改質劑及蓖麻油基觸變劑。
燒結漿料較佳為大致上不含樹脂，更佳為完全不含樹脂。樹脂的存在可能降低銀的熱和電傳導。溶劑較佳包含單萜醇及/或二醇及/或二醇醚，更佳包含萜品醇及/或二乙二醇單正丁基醚。
燒結漿料較佳包含：從1至30wt%的溶劑；及/或多達50wt%的有機銀化合物，較佳從0.1至25wt%，更佳從0.1至10wt%，甚至更佳從0.1至9wt%；及/或多達5wt%的流變改質劑；及/或多達2wt%的活化劑；及/或多達6wt%的界面活性劑；及/或多達2wt%的過氧化氫或有機過氧化物。
燒結漿料可以包含0至5wt%的流變改質劑及/或0至2wt%的活化劑及/或0至6wt%的界面活性劑及/或0至2wt%的過氧化氫或有機過氧化物。燒結粉末可以形成燒結漿料的剩餘部份。
在進一步的態樣中，本發明提供一種燒結膜，該燒結膜包含本文所述的燒結粉末及黏結劑。該膜可被應用於晶圓層次、晶粒層次、封裝/基材層次、及/或模組層次。這種膜可以例如藉由將本文所述的燒結漿料印刷到聚酯片上、加熱該漿料以至少部分去除溶劑並形成膜、然後從聚酯片移除該膜來獲得。本文所述的膜是特別有利的，因為可以藉由在稍微升高的溫度下簡單地將晶粒按壓到該膜上而將該膜轉移到晶粒上。轉移膜是替代的施加方法，可被有利地提 供於某些情況。該膜可以被形成在聚合物、玻璃、金屬或陶瓷基材或直接在晶圓上。該膜可以在包含聚酯的聚合物基材上。該膜可以被形成在聚合物基材上，其中該聚合物基材包含釋放塗層。該膜可以藉由印刷或澆鑄材料來施加漿料組成物而生產。該膜可以藉由印刷在連續層中來生產。或者，該膜可以藉由印刷以形成離散形狀的陣列來生產。
在進一步的態樣中，本發明提供一種晶粒黏附方法，包含以下步驟：(i)將本文所述的燒結膜放在晶粒與待接合基材之間；以及(ii)燒結該燒結膜，其中該燒結之進行未施加壓力。
這種「低壓」或「無壓」燒結是特別有利的，因為可以使製程的自動化更簡單。此外，可以減少對工件的損壞。優於採用加壓燒結的方法的進一步優點包括：晶粒貼裝所需時間較短(高UPH)、貼裝的低壓要求(對於處理薄晶圓非常有利)、與商用晶粒黏合機的相容性及在外部加熱設備中燒結(批次處理以改良UPH)。
燒結較佳是在150至400℃的溫度下進行長達120分鐘。這樣的條件可以產生特別有效燒結的燒結膜，同時避免損傷工件。
步驟(i)較佳包含：(a)將燒結膜施加於晶粒以形成具有晶粒側和燒結膜側的組件；以及(b)使該組件的膜側與基材接觸。
這樣的步驟可以使製程的自動化更簡單，而且可以例如藉由使用壓印機來進行。
步驟(a)較佳是在15至400℃的溫度和0.1至5MPa的壓力下進行0.1至60秒。這樣的條件可以產生特別有效施加的燒結膜，同時避免損壞晶粒。
步驟(b)較佳是在15至400℃的溫度和0.1至40MPa的壓力下進行0.1至60分鐘。這樣的條件可以產生特別有效的、晶粒對基材的接觸，同時避免損壞晶粒或基材。
在進一步的態樣中，本發明提供一種晶粒黏附方法，包含以下步驟：(i)將本文所述的燒結膜放在晶粒與待接合基材之間；以及(ii)燒結該燒結膜，其中該燒結係在施加從0.1至40MPa的壓力時進行。
在進一步的態樣中，本發明提供一種晶圓黏著方法，包含以下步驟：(i)將本文所述的燒結膜放在兩個或更多個待接合晶圓之間；以及(ii)燒結該燒結膜，其中該燒結之進行未施加壓力。
在進一步的態樣中，本發明提供一種轉移燒結膜至元件的方法，包含以下步驟：將本文所述的燒結膜施加於基材以形成組件，該組件具有燒結膜側及基材側；使該組件之該燒結膜側與元件接觸；將該組件加熱至從50至200℃的溫度；對該組件施加從1至5MPa的壓力持續0.1秒至60分鐘；以及從該燒結膜分離該基材。
該基材可以是聚合物。該燒結膜的尺寸大致上可與該元件相同。該元件可以是LED。
在進一步的態樣中，本發明提供一種晶粒黏附方法，包含以下步驟：將本文所述的燒結膜施加於基材；在該膜上貼裝晶粒以形成組件；對該組件施加小於2MPa的壓力；以及在100至400℃的溫度下燒結該組件持續0.1秒至5分 鐘、施加低於3MPa的壓力。同一組件可以使用各種製程及提供適當熱度的設備進一步在175至400℃的溫度下以無壓力的方式進行燒結，以起始並完成燒結。
在進一步的態樣中，本發明提供一種晶粒黏附方法，包含以下步驟：將本文所述的燒結膜施加於基材；在該膜上貼裝晶粒以形成組件；對該組件施加小於5MPa的壓力；以及在100至400℃的溫度下燒結該組件持續0.1秒至60分鐘、施加低於40MPa的壓力。同一組件可以使用各種製程及提供適當熱度的設備進一步在175至400℃的溫度下以無壓力的方式進行燒結，以起始並完成燒結。
在進一步的態樣中，本發明提供一種晶粒黏附方法，包含以下步驟：將本文所述的燒結膜施加在晶圓的背側上；切割該晶圓以形成複數個晶粒；將至少一個晶粒放在基材上以形成組件；對該組件施加超過1MPa的壓力；以及在100至400℃的溫度下燒結該組件持續0.1秒至60分鐘。同一組件可以使用各種製程及提供適當熱度的設備進一步在175至400℃的溫度下以無壓力的方式進行燒結，以起始並完成燒結。
在進一步的態樣中，本發明提供一種晶圓黏著方法，包含以下步驟：將本文所述的燒結膜施加在晶圓的背側上；貼裝多一個相同或不同類型的晶圓在含有晶圓的可燒結Ag膜上，以形成組件；對該組件施加>0.1MPa的壓力；以及在100至400℃的溫度下燒結該組件持續0.25秒至120分鐘。同一組件可以使用各種製程及提供適當熱度的設備進一步在175至400℃的溫度下以無壓力的方式進行燒結，以起始並完成燒結。
在進一步的態樣中，本發明提供一種晶圓黏著方法，包含以下步驟：將燒結膜施加在晶圓的背側上；貼裝多一個相同或不同類型的晶圓在含有晶圓的燒結膜上，以形成組件；對該組件施加小於40MPa的壓力；以及在100至400℃的溫度下燒結該組件持續0.25秒至120分鐘。同一組件可以使用各種製程及提供 適當熱度的設備進一步在175至400℃的溫度下以無壓力的方式進行燒結，以起始並完成燒結。
在進一步的態樣中，本發明提供本文所述的燒結粉末或本文所述的燒結漿料或膜在選自以下的方法中的用途：晶粒黏附(例如晶片對板、晶片對基材、晶片對散熱片、晶片對夾具)、晶圓對晶圓黏著(例如晶片對散熱器)、反射層印刷、密閉及近密閉的密封(例如用於封裝和周邊密封)、互連線的生產(例如電路、襯墊)、半導體元件和基材中的通孔填充、及覆晶和晶圓凸塊。
在進一步的態樣中，本發明提供一種製造燒結接點的方法，包含以下步驟：在兩個或更多個待接合工件附近提供本文所述的燒結粉末或本文所述的燒結漿料或膜；以及加熱該燒結粉末或燒結漿料或膜以至少部分燒結金屬。
有利的是，加熱步驟可以在大氣壓力下進行。可以在低壓下將燒結粉末或燒結漿料或膜放在工件的附近(通常在1至5MPa、在約175至250℃的溫度下持續0.1至60秒)。
加熱步驟較佳是在至少140℃、更佳從150至350℃、甚至更佳從160至300℃的溫度下進行。低於140℃的溫度可能不會導致燒結粉末中的顆粒充分燒結及/或可能不會導致有機物藉由蒸發及/或燒掉充分去除。高於350℃的溫度可能導致工件損壞。
在進一步的態樣中，本發明提供一種製造本文所述燒結粉末的方法，包含以下步驟：提供金屬鹽溶液；使該金屬鹽溶液與包覆劑接觸；以及沉澱出至少部分塗覆有該包覆劑的金屬顆粒。
沉澱出的金屬顆粒可以從溶劑中回收，例如藉由過濾。金屬鹽溶液的實例為金屬硝酸鹽溶液。
沉澱步驟可以使用還原劑來進行。還原劑在使金屬顆粒沉澱上特別有效。特別合適的還原劑包括例如肼(例如水合肼)和硼氫化鈉。
過量的包覆劑可以使用極性溶劑洗掉，該極性溶劑例如甲醇或丙酮。
將理解的是，本文揭示的方法、粉末、漿料及膜與許多優於現有技術的益處相關聯。特別是，當使用該漿料印刷時沒有坍落現象、沒有橋接、在印刷沉積物中沒有氣泡、沒有滲出且沒有孔阻塞。此外，提供80至90微米的漿料高度、沒有摺角且沒有起伏的平坦沉積物是可能的。因此，包括黏結劑(例如樹脂)的漿料之益處包括：無壓燒結
標準SMT生產線的處理能力
平坦均勻的表面形貌
晶粒切變強度平均>20MPa
無界面失效模式
室溫穩定性=最少1個月
熱循環：可接受的接點強度高達1500個週期(-40℃至+125℃，停留10分鐘)。
針和噴嘴可分配的
膜成形因子
除了上面提及的益處之外，含有機銀化合物的漿料具有以下所列的一些進一步的益處：高的晶粒切變強度(25至45MPa)
高的導熱性(>200W/mK)
針可轉移的
良好的高熱性能
現在將參照以下非限制性圖式來描述本發明，其中：第1圖圖示(a)使用帶材澆鑄機製備的大面積Ag膜(實例1)，並且插圖圖示PET上的矩形膜片，(b)厚度18-20μm的獨立乾膜之光學顯微鏡影像，(c-e)實例2的獨立乾膜在PET(30-40μm厚)上的光學顯微鏡影像，以及(f-g)實例5的獨立乾膜在PET上的光學顯微鏡影像。
第2圖圖示用於本發明燒結膜之晶粒黏附應用的晶粒黏附製程「加壓燒結(PS)」Vs.「加壓貼裝和減壓燒結(PPPS)」製程步驟之示意性表示。
第3圖圖示用於本發明燒結膜之晶粒黏附應用的「加壓貼裝和減壓燒結」製程步驟及其典型製程參數及其相依性之示意性表示。
第4圖圖示使用「加壓貼裝和減壓燒結晶粒黏附製程」時黏附在塗覆Ni/Ag的DBC(使用實例2的膜)上、塗覆Ni/Au的3mmx3mm Si晶粒之晶粒切變為a)貼裝時間及b)工具溫度之函數的曲線圖。
第5圖圖示使用「加壓貼裝和減壓燒結晶粒黏附製程」時黏附在塗覆Ni/Ag的DBC(使用實例2的膜)上、塗覆Ni/Au的3mmx3mm Si晶粒在貼裝時間1s的橫截面區域之SEM影像。
第6圖圖示在塗覆Ni/Au的Si晶圓上的轉移Ag膜和轉移之後在PET上的殘留膜。
第7圖圖示來自熱壓黏合的(a)塗覆Ni/Au的4□Si晶圓對及(b)塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au、使用18-20μm實例2的膜的4□CuW晶圓並藉由市售切割機製備的切割(3mmx3mm)樣品之影像。沒有觀察到碎屑。
第8圖圖示熱壓黏合的、塗覆Ni/Au且使用實例1的18-20μm膜的4□Si晶圓對之C-SAM影像。
第9圖圖示顯示BLT和微結構的切割樣品之橫截面區域的SEM影像。這些樣品是從熱壓黏合的、塗覆Ni/Au且使用實例1的18-20μm膜的Si晶圓對在不同施加壓力下製備的：0.5MPa(上左)、1MPa(上中)、2MPa(上右)、5MPa(下左)及10MPa(下中)。
第10圖圖示熱壓黏合的、塗覆Ni/Au、使用實例1的18-20μm膜且無後加熱步驟(步驟4)的4□Si晶圓對之C-SAM影像。
第11圖圖示熱壓黏合的塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au且使用實例1的18-20μm膜的4□CuW晶圓之代表性CSAM影像。
第12圖圖示從熱壓黏合的、塗覆Ni/Au且使用實例2的30-40μm膜的4□Si晶圓製備的離子拋光晶粒之橫截面區域的SEM影像。
第13圖圖示熱壓黏合的塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au且使用實例2的膜的4□CuW晶圓之C-SAM影像。該C-SAM影像證實有良好的黏合而且黏合的晶圓中沒有脫層或空隙。
第14圖圖示從熱壓黏合的4□Si晶圓與塗覆Ni/Au且使用實例2的30-40μm膜的4□CuW晶圓製備的離子拋光晶粒之橫截面區域的SEM影像。
第15圖圖示從熱壓黏合的塗覆Ni/Au的4□Si晶圓對及塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au且使用實例1的膜和實例2的膜的4□CuW製備的、尺寸3mm x 3mm的晶粒之晶粒切變曲線圖。
現在將參照以下非限制性實例來說明本發明。
實例1
將0至8%的樹脂或聚合物、0至2%的膜成形劑及5%至30%的溶劑混合物混合以獲得均勻的溶液。對該混合物添加0至2%的潤濕劑、0至2%的有機過氧化物，接著加入65至85%的前述銀奈米粉末(即具有5至75nm的平均最長尺寸)，並使用軌道混合器以1000rpm混合。混合後，將混合物在三輥研磨機中研磨幾分鐘以獲得均勻的漿料。
實例2
將0至2%的膜成形劑、0至5%的銀金屬有機化合物(Ag MOC)、5至30%的溶劑混合物在罐中混合。對該混合物添加0至2%的潤濕劑、0至2%的有機過氧化物，接著加入65至85%的前述銀奈米粉末(即具有5至75nm的平均最長尺寸)。使用軌道混合器以1000rpm混合該混合物。混合後，將該混合物在三輥研磨機中研磨幾分鐘以得到均勻的漿料。
實例3
將0至2%的膜成形劑、0至8%的樹脂或聚合物、0至5%的銀金屬有機化合物(Ag MOC)及5至30%的溶劑混合物在罐中混合。對該混合物添加0至2%的潤濕劑、0至2%的有機過氧化物，接著加入65至85%的前述銀奈米粉末(即具有5至75nm的平均最長尺寸)。使用軌道混合器以1000rpm混合該混合物。混合後，將該混合物在三輥研磨機中研磨幾分鐘以得到均勻的漿料。
實例4
將0至2%的膜成形劑、0至8%的樹脂或聚合物、0至7%的銀金屬有機化合物(Ag MOC)及5至30%的溶劑混合物在罐中混合。對該混合物添加0至2%的潤濕劑、0至2%的有機過氧化物，接著加入65至95%的銀微米顆粒(即具有100nm至50μm的平均最長尺寸)。使用軌道混合器以1000rpm混合該混合物。混合後，將該混合物在三輥研磨機中研磨幾分鐘。
實例5
將0至2%的膜成形劑、0至8%的樹脂或聚合物、0至7%的銀金屬有機化合物(Ag MOC)及5至30%的溶劑混合物在罐中混合。對該混合物添加0至2%的潤濕劑、0至2%的有機過氧化物，接著加入65至95%的銀奈米(即具有5至75nm的平均最長尺寸)與微米顆粒(即具有100nm至50μm的平均最長尺寸)之混合物。使用軌道混合器以1000rpm混合該混合物。混合後，將該混合物在三輥研磨機中研磨幾分鐘。
發現實例1-5的燒結銀樣品之導熱率是在100-250W.m-1.K-1的範圍中。燒結銀樣品的導熱率是藉由在250℃下將實例1-5的漿料加熱60分鐘且沒有施加壓力而製備的，並使用Netzsch LFA 447 Nanoflash量測。導熱率k(W.m-1.K-1)是使用下列公式計算：K=α ρ c p ，其中α是熱擴散率(m2.s-1)，ρ是材料的密度(Kg.m-3)，cp是比熱容量(J.kg-1.K-1)。
膜製備製程：
膜是藉由使用市售的帶材澆鑄機以輥對輥的方式、使用設置有帶材澆鑄機的微量儀表控制刮刀組件或藉由使用刮刀的手動模板印刷印刷在塗覆矽的聚酯片上而製備的。
市售的帶材澆鑄機：
使用市售的帶材澆鑄機將實例1的漿料印刷在塗覆矽的聚酯片上，並在130℃下以輥對輥的方式乾燥其加熱表面。為了完全乾燥，膜花費10至15分鐘。使用設置有帶材澆鑄機的刮刀組件之間隙設定控制膜的厚度。藉由改變微量儀表控制的刮刀組件之間隙設定來製備18-20μm和33-35μm的膜厚度。第1(a)圖圖示使用帶材澆鑄機製備的大面積膜並且插圖圖示在PET上的矩形膜片。第1(b)圖圖示厚度18-20μm的獨立乾膜之光學顯微鏡影像。也可以藉由簡單改變刮刀組件的間隙設定來輕易地獲得厚度>5μm的膜。
手動模板印刷：
使用刮刀在塗覆矽的聚酯上手動模板印刷實例2的漿料。將這些初製備的膜在60至90℃的烘箱中乾燥30至90分鐘。發現這種手動印刷的實例2膜之厚度為20至60μm。將在PET(30至40μm的厚度)上實例2和實例5的獨立乾燥膜之光學顯微鏡影像分別圖示於第1(c-e)圖和第1(f-g)圖。或者，也可以使用市售的帶材澆鑄機以輥對輥的方式將膜印刷在塗覆矽的聚酯片上，而且可以使用設置有帶材澆鑄機的微量儀表控制刮刀組件之間隙設定來控制膜的厚度。
Ag膜用於晶粒黏附的應用：
本發明的燒結膜可被使用於使用各種基於銀燒結的現有晶粒黏附製程(加壓燒結(PS)製程)的電子元件接合，包括專利申請US 13/287820(公開號：US 2012-0114927 A1)中描述的那些，將該專利申請之揭示內容以引用方式併入本文中。此外，本發明的燒結膜可被用於晶粒黏附「加壓貼裝和減壓燒結(PPPS)製程」。第2圖圖示使用本發明之燒結膜的「加壓燒結(PS)」Vs.「加壓貼裝和減壓燒結(PPPS)」製程步驟之一般製程步驟的示意性表示。這種新的PPPS製程與PS製程相比有幾個額外的優點，即晶粒貼裝所需時間較短(高UPH)、貼裝的低壓要求(對於處理薄晶圓非常有利)、與商用晶粒黏合機的相容性及在外部加熱設備中燒結(批次處理以改良UPH)。此外，在基於燒結的晶粒黏附製程期間，這些可燒結Ag膜也可被用於需要明顯較高壓力(>5MPa)的PS製程。
加壓貼裝和減壓燒結(PPPS)製程
本發明的燒結膜可被使用於使用新的銀燒結低溫低壓晶粒黏附製程「加壓貼裝和減壓燒結(PPPS)製程」的電子元件接合。第3圖圖示用於奈米Ag膜之晶粒黏附應用的「加壓貼裝和減壓燒結製程」步驟、其典型製程參數及其相依性之示意性表示。使用此加壓貼裝和減壓燒結製程(使用此可燒結Ag膜) 的電子元件接合非常靈活，而且時間、溫度及壓力的確切組合可以根據應用的本質與熱機械、電及熱性能要求來最佳化。
PPPS晶粒黏附製程步驟：
整體黏合製程通常可以包括例如：1)膜轉移，2)壓力輔助晶粒貼裝及3)無壓燒結，除非他處另有個別的說明。
(1)膜轉移：藉由使用工具和板材之時間、壓力及溫度的最佳化組合的壓印製程將可燒結Ag膜轉移到晶粒上。典型的製程參數是：工具溫度：室溫至400℃
板材溫度：室溫至400℃
壓力：0.1至5MPa
時間：0.1至60秒
(2)壓力輔助晶粒貼裝：使用工具和板材之時間、壓力及溫度的最佳化組合在DBC(直接貼合銅)基材上貼裝含可燒結Ag的晶粒。典型的製程參數是：工具溫度：室溫至400℃
板材溫度：室溫至400℃
壓力：0.1至40MPa
時間：0.1至60分鐘
額外加熱時間：可以在貼裝(不施加任何外部壓力)之後立即包括額外的0-60分鐘
(3)無壓燒結：無壓燒結是在外部烘箱中或熱板上進行。製程參數總結如下：燒結溫度：150-400℃
燒結時間：0至120分鐘
壓力輔助燒結(PS)製程：
本文所述的燒結膜可被用於使用壓力輔助燒結晶粒黏附製程的電子元件接合。使用此壓力輔助燒結製程(使用該可燒結Ag膜)的電子元件接合非常靈活，而且時間、溫度及壓力的確切組合可以根據應用的本質與熱機械、電及熱性能要求來最佳化。
PS晶粒黏附製程步驟：
整體黏合製程通常可以包括例如：1)膜轉移，2)壓力輔助晶粒貼裝及燒結，除非他處另有個別的說明。
(1)膜轉移：藉由使用工具和板材之時間、壓力及溫度的最佳化組合的壓印製程將可燒結Ag膜轉移到晶粒上。典型的製程參數是：工具溫度：室溫至400℃
板材溫度：室溫至400℃
壓力：0.1至5MPa
時間：0.1至60秒
(2)壓力輔助晶粒貼裝及燒結：使用工具和板材之時間、壓力及溫度的最佳化組合在DBC基材上貼裝含可燒結Ag的晶粒。典型的製程參數是：工具溫度：室溫至400℃
板材溫度：室溫至400℃
壓力：0.1至40MPa
時間：0.1秒至60分鐘
額外加熱時間：可以在貼裝(不施加任何外部壓力)之後立即包括額外的0-60分鐘
黏合晶粒的一般特徵化製程：
使用晶粒切變、熱衝擊和循環、黏合層厚度量測及在離子拋光之後使用SEM進行微結構分析來特徵化黏合的晶粒。
晶粒黏附應用1(PPPS)：
已經示範將由實例2形成的燒結膜應用於使用加壓燒結製程的電子元件接合(製程示意性圖示於第3圖)。這種應用的實例已經示範使用實驗室手動晶粒黏合機將塗覆Ni/Au的3mm x 3mm Si晶粒黏附在使用可燒結Ag膜、塗覆Au或Ag的DBC基材上。第4圖圖示使用「加壓貼裝和減壓燒結晶粒黏附製程」時黏附在塗覆Ni/Ag的DBC(使用實例22形成的燒結膜)上、塗覆Ni/Au的3mm x 3mm Si晶粒之晶粒切變為a)貼裝時間及b)工具溫度之函數的結果。將以下的製程參數用於晶粒黏附：
(1)膜轉移：
工具溫度：100-200℃
板材溫度：室溫
壓力：1.5MPa
時間：1秒
(2)壓力輔助晶粒貼裝：
工具溫度：100-200℃
板材溫度：200℃
壓力：2
時間：0.25至1.5秒
額外加熱時間：無
(3)無壓燒結
燒結溫度：225℃
燒結時間：60分鐘
第5圖圖示由黏附在塗覆Ni/Ag的DBC(使用由實例2形成的燒結膜)上、塗覆Ni/Au的3mm x 3mm Si晶粒製備的離子拋光晶粒在1s貼裝時間的橫截面區域之SEM影像。黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。
晶粒黏附應用2(PS)
已經示範將由實例5形成的燒結膜應用於使用壓力輔助燒結製程的 電子元件接合。這種應用的實例已經示範使用實驗室手動晶粒黏合機藉由在250℃下施加5至20MPa的燒結壓力持續30至90秒的燒結時間來將塗覆Ni/Au的3mm x 3mm Si晶粒黏附在塗覆Au或Ag的DBC或塗覆Ag的Cu引線框架基材上，燒結膜由實例5形成。晶粒切變結果顯示強的黏接(>40MPa)，而且黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。
Ag膜在晶圓黏合的應用
使用實驗室壓印機在250℃下使用1MPa的壓力使用實例1形成的膜和實例2形成的膜示範一對塗覆Ni/Au的4" Si晶圓(Si燒結的Ag-Si)及塗覆Ni/Au的4" Si晶圓與塗覆Ni/Au的4" CuW晶圓(Si燒結的Ag-CuW)之熱壓黏合應用。對於使用這些膜的所有晶圓黏合的示範(應用1-4)，除非他處另有說明，否則遵循以下的黏合製程。
晶圓黏合製程步驟：
整體黏合製程通常可以包括例如：1)膜轉移，2)晶圓堆疊形成，3)晶圓黏合及4)後加熱，除非他處另有個別的說明。
1)膜轉移：
在80-150℃和1MPa的壓力下將Ag膜從PET表面轉移到塗覆Ni/Au的Si或塗覆Ni/Au的CuW持續5分鐘。去除剩餘的Ag膜和PET，並將轉移Ag的、塗覆Ni/Au的Si或塗覆Ni/Au的CuW晶圓用於堆疊形成。第6圖圖示轉移之後在塗覆Ni/Au的Si晶圓上的轉移Ag膜及在PET上的剩餘膜之影像。
2)晶圓堆疊形成：
堆疊是藉由步驟1將塗覆Ni/Au的Si晶圓貼裝在轉移Ag膜的、塗覆Ni/Au的Si或塗覆Ni/Au的CuW上而製備的。然後在100-150℃和1MPa的壓力下將堆疊加熱5-15分鐘。
3)晶圓黏合
將藉由步驟2處理的晶圓堆疊使用於在250℃和1MPa的壓力下進行15分鐘的黏合。
4)後加熱
將藉由步驟3在250℃處理的晶圓堆疊使用於250℃的後加熱且不施加任何的壓力持續45分鐘。在這些處理之後，將黏合晶圓冷卻到室溫，並用於進一步特徵化。
黏合晶圓的一般特徵化製程：
使用C-SAM檢查所有黏合晶圓的脫層和空隙。然後切割這些黏合晶圓以得到不同晶粒尺寸，像是3mm x 3mm和10mm x 10mm，以用於在離子拋光之後使用SEM進行各種特徵化，例如晶粒切變、熱衝擊和循環、黏合層厚度量測及微結構分析。例如，第7圖圖示使用市售的切割機從熱壓黏合的(a)塗覆Ni/Au的4□Si晶圓對和(b)塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au、使用實例1的18-20μm膜的4□CuW晶圓製備的切割(3mm x 3mm)樣品之影像。在所有這些黏合的晶圓上沒有觀察到脫黏和碎裂，這表示良好的黏合。
晶圓黏合應用1(Si-AF1-Si) 不同施加壓力的黏合：
使用實驗室壓印機在250℃下使用0.5、1、2及5MPa的壓力使用實例1的18-20μm膜示範一對塗覆Ni/Au的4" Si晶圓之熱壓黏合。對於10MPa的壓力，使用一對塗覆Ni/Au的2" Si晶圓。使用C-SAM檢查所有黏合晶圓的脫層和空隙， 並確認沒有脫層和空隙。第8圖圖示熱壓黏合的、塗覆Ni/Au且使用實例1的18-20μm膜的4□Si晶圓對之C-SAM影像。C-SAM影像確認黏合良好且黏合晶圓中沒有脫層和空隙。然後切割這些黏合晶圓以得到不同的晶粒尺寸，像是3mm x 3mm、10mm x 10mm，並用於在離子拋光之後使用SEM進行晶粒切變測定、黏合層厚度量測及微結構分析。為了觀察壓力對燒結銀層之微結構和黏合線厚度(BLT)的影響，切割這些晶圓並使用SEM檢察。第9圖圖示在不同施加壓力：a)0.5MPa、b)1MPa、c)2MPa、d)5MPa及e)10MPa下從使用實例1的18-20μm膜、塗覆Ni/Au的Si晶圓熱壓黏合對製備的離子拋光晶粒之橫截面區域的SEM影像。黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。發現在低壓區(0.5至2MPa)BLT是高度壓力相關的，之後壓力對BLT的影響變得較不明顯。相對地，這些燒結銀的微結構在整個實驗施加的壓力範圍間都是高度壓力相關的，如從結晶大小、互連相鄰者及密度所證實。如可以看到的，在5和10MPa的壓力下產生了高度緻密和互連的結構。黏合晶粒的晶粒切變顯示塊體或界面破壞，因此可以得到的結論是：與黏合的矽晶圓材料相比，燒結銀黏合的材料非常強固。
無後加熱的黏合：
為了確認後加熱步驟的必要性，我們使用實驗室壓印機在250℃下使用1MPa的壓力黏合了兩對塗覆Ni/Au且使用實例1形成的18-20μm膜的4" Si晶圓，且不進行後加熱步驟(步驟4)。如第10圖可以清楚看到的，這些晶圓中有幾個脫層區域存在。
晶圓黏合應用2(Si-AF1-CuW)：
使用實驗室壓印機在250℃下使用1MPa的壓力使用實例1形成的18-20μm膜示範塗覆Ni/Au的4" Si晶圓與塗覆Ni/Au的4" CuW晶圓之熱壓黏合。第11圖圖示熱壓黏合的、塗覆Ni/Au的4" Si晶圓與塗覆Ni/Au且使用實例1的18-20 μm膜的4" CuW晶圓之C-SAM影像。C-SAM影像確認黏合良好且黏合晶圓中沒有脫層和空隙。然後切割這些黏合晶圓以得到不同的晶粒尺寸，像是3mm x 3mm和10mm x 10mm，並用於在離子拋光之後使用SEM進行晶粒切變測定、黏合層厚度量測及微結構分析。為了觀察膜厚度對燒結銀層之黏合線厚度(BLT)的影響，我們選擇了由實例1形成的18-20和32-35μm膜、使用實驗室壓印機在250℃下使用1MPa的壓力來將4" Si晶圓與塗覆Ni/Au的4" CuW晶圓黏合。黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。發現BLT隨著膜厚度減小而減小。黏合晶粒的晶粒切變顯示塊體或界面破壞，因此可以得到的結論是：與黏合的矽晶圓材料相比，燒結銀黏合的材料非常強固。
晶圓黏合應用3(Si-AF2-Si)：
使用實驗室壓印機在250℃下使用1MPa的壓力使用實例2的30-40μm膜示範一對塗覆Ni/Au的4" Si晶圓之熱壓黏合。使用C-SAM檢查所有黏合晶圓的脫層和空隙，並確認沒有脫層和空隙。熱壓黏合的、使用實例2的30-40μm膜、塗覆Ni/Au的4" Si晶圓對之C-SAM影像確認黏合良好且黏合晶圓中沒有脫層和空隙。然後切割這些黏合晶圓以得到不同的晶粒尺寸，像是3mm x 3mm、10mm x 10mm，並用於在離子拋光之後使用SEM進行晶粒切變、黏合層厚度量測及微結構分析。第12圖圖示在1MPa的施加壓力下從使用實例2的30-40μm膜、熱壓黏合的、塗覆Ni/Au的4□Si晶圓對製備的離子拋光晶粒之橫截面區域的SEM影像。黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。黏合晶粒的晶粒切變顯示塊體或界面破壞，因此可以得到的結論是：與黏合的矽晶圓材料相比，燒結銀黏合的材料非常強固。
晶圓黏合應用4(Si-AF2-CuW)：
使用實驗室壓印機在250℃下使用1MPa的壓力使用實例2的30-40μm膜示範塗覆Ni/Au的4" Si晶圓與塗覆Ni/Au的4" CuW晶圓之熱壓黏合。第13圖 圖示熱壓黏合的、塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au且使用實例2的30-40μm膜的4" CuW晶圓之SEM影像。C-SAM影像確認黏合良好且黏合晶圓中沒有脫層和空隙。然後切割這些黏合晶圓以得到不同的晶粒尺寸，像是3mm x 3mm和10mm x 10mm，並用於在離子拋光之後使用SEM進行晶粒切變和黏合層厚度量測及微結構分析。第14圖圖示在250℃下使用1MPa的壓力從熱壓黏合的4□Si晶圓與塗覆Ni/Au且使用實例2的30-40μm膜的4□CuW晶圓製備的離子拋光晶粒之橫截面區域的SEM影像。黏合層的SEM顯示燒結銀顆粒的頸縮具有良好的裝填分率。黏合晶粒的晶粒切變顯示塊體或界面破壞，因此可以得到的結論是：與黏合的矽晶圓材料相比，燒結銀黏合的材料非常強固。
黏合晶圓的機械和熱機械特性 晶粒切變結果：
為了研究黏合燒結Ag層的機械黏合強度，將熱壓黏合的晶圓切割成3mm x 3mm大小的晶粒，並進行晶粒切變測試。黏合晶粒的晶粒切變顯示塊體或界面破壞，因此可以得到的結論是：與黏合的矽晶圓材料相比，燒結銀黏合的材料非常強固。第15圖圖示在250℃下使用1MPa的壓力從熱壓黏合的、塗覆Ni/Au的4□Si晶圓對及塗覆Ni/Au的4□Si晶圓與塗覆Ni/Au且使用實例1形成的膜和實例2形成的膜的4□CuW晶圓製備的、尺寸3mm x 3mm的晶粒之晶粒切變值比較。
熱衝擊結果：
為了研究熱應力對使用燒結奈米銀膜的黏合晶圓和晶粒的影響，使熱壓黏合的4" Si晶圓與塗覆Ni/Au、使用在250℃和1MPa的壓力下由實例1形成的膜和由實例2形成的膜的4" CuW晶圓及10mm x 10mm的晶粒依據JESD22-A104-B測試條件B、浸泡模式2(-55至+125℃，5分鐘停留時間，1000 次循環)進行熱衝擊實驗。在1000次循環後，黏合晶圓和晶粒的C-SAM影像都沒有在黏合晶圓中顯露任何脫層、空隙和裂縫。
熱循環結果：
為了研究熱應力對使用燒結奈米銀膜的黏合晶粒的影響，使來自熱壓黏合的4" Si晶圓與塗覆Ni/Au、使用在250℃和1MPa的壓力下由實例1形成的膜和由實例2形成的膜的4" CuW晶圓的10mm x 10mm切割樣品依據IPC 9701-A標準TC3/NTC-C曲線(-40至+125℃，15分鐘停留時間，1000次循環)進行熱循環實驗。在1000次循環後，這些晶粒的C-SAM影像沒有在黏合晶圓中顯露任何脫層、空隙和裂縫。
本發明的燒結粉末、燒結膜及燒結漿料之其他應用如下：
1.用於垂直LED設計、薄膜覆晶設計及紅色LED設計且基於可印刷漿料和膜兩者的晶圓對晶圓黏合層。對於其中黏合層在黏合後表現出極高溫特性的低溫(在250℃以下而且也在200℃以下)晶圓對晶圓黏合存在顯著的需求。在LED晶圓黏合的情況下，這可以例如在薄膜覆晶或垂直薄膜或截斷倒金字塔LED任一情境下完成，其中CTE不匹配及因此產生的應變和缺陷可以被最少化，同時允許使用各種先進材料進行高溫後處理，以增強裝置的光輸出和電效率。另外，除了其他優點之外，黏合層的高溫傳導性和高熱傳導性和電傳導性允許優異的熱輸送、裝置的高溫操作及優異的電流擴展。這種晶圓黏合可以藉由將該材料的膜層壓在晶圓的背側上、接著在標準的晶圓黏合機或壓印機中藉由溫度和壓力處理來完成。進行該處理的另一種工具包括在晶圓的背側上印刷保形的漿料層，然後在標準的晶圓黏合機或壓印機中、在溫度和壓力條件下進行乾燥和黏合。這種晶圓黏合的其他應用包括功率半導體晶圓、穿矽通孔(TSV)的應用、堆疊晶粒的應用、微機電系統、聚光光伏及其他應用。低溫燒結能夠得到高CTE不匹配的堆疊以及溫度敏感材料堆疊、熱電材料及壓電材料的組件。
2.將半導體晶粒(無論是覆晶或引線黏合的)黏附於多種基材上，例如DBC(直接貼合銅)、DPC(直接鍍銅)、MCPCB(金屬芯印刷電路板)、FR4、銅引線框架、撓性印刷電路板和基材、銅和鋁散熱片、夾具等。應用包括從各種化合物半導體材料製成的LED晶粒(發光二極體，例如橫向、垂直薄膜或覆晶等種類)、由矽製成的功率晶粒、聚光光伏化合物半導體電池(例如多接面電池)用於功率模組的碳化矽和氮化鎵、及離散元件、所有類型的MEMS(微機電感測器)裝置、半導體和堆疊晶粒及其他應用，例如熱電材料和壓電材料。
(a)這種半導體或其他晶粒元件的黏附可以藉由印刷到基材上、隨後經由晶粒黏合機或拾取和貼裝機器進行晶粒貼裝、及在回流爐帶或箱式爐任一者中進行燒結來完成。這種半導體和晶粒元件的黏附也可以經由分配漿料、隨後進行如上概述的晶粒貼裝和燒結來完成，或進行膜轉移並層壓在從該材料製成的膜之晶粒背側上、隨後進行晶粒貼裝並定位於基材上、然後進行燒結來完成。覆晶晶粒可以藉由將凸塊印刷在基材上、貼裝晶粒、然後進行燒結來組裝。低溫燒結能夠產生高CTE不匹配堆疊以及溫度敏感材料堆疊的組件。
3.黏附各種類型的半導體封裝(例如底部終止元件，諸如LGA、QFN、QFP等)到各種基材上，該基材例如DBC(直接貼合銅)、DPC(直接鍍銅)、MCPCB(金屬芯印刷電路板)、FR4、撓性印刷電路板和基材、銅和鋁散熱片、夾具等。應用包括各種類型的LED封裝(例如陶瓷次黏著LED、具有引線框架結構的SMD LED等)、功率模組、及離散元件、所有類型的MEMS(微機電感測器)封裝、半導體和堆疊晶粒封裝及其他應用。
(a)這種半導體的黏附或其他封裝可以藉由印刷到基材上、隨後經由具有Z高度調整及/或壓力能力的標準拾取和貼裝機器進行封裝貼裝、及在回流帶 爐或箱式爐任一者中進行燒結來完成。低溫燒結能夠產生高CTE不匹配堆疊以及溫度敏感材料堆疊的組件。
4.個別地及與覆晶互連一起生產互連線(電路、襯墊等)。例如，用於互連線的應用包括LED板和燈具，其中互連線可以藉由各種印刷(例如模板印刷)或分配或噴射技術施加。在LED應用的情況下，這種互連可以作為電和熱的導體，以攜帶電子往返裝置，並將熱攜離裝置。此外，這種互連線可以在與用於黏附覆晶或引線黏合裝置的互連同一步驟中直接施加。這種互連的另一個實例是太陽能電池(無論基於矽或基於薄膜)，其中在網格圖案中的互連可被用來收集產生的電子，而且還將一個電池連接到另一個電池。
5.用於LED和光學應用的反射層印刷。該材料可被用於印刷反射層到基材上，該基材例如DBC(直接貼合銅)、DPC(直接鍍銅)、MCPCB(金屬芯印刷電路板)、FR4、撓性印刷電路板和基材、銅和鋁散熱片、夾具等，以提供增強的光輸出，並因此提供發光效率增強的LED及其他光學系統。這種反射層可以經由模板或網版印刷、噴射或分配或膜層壓該材料來形成。
6.密閉和近密閉的密封，用於封裝、周邊密封等，用於LED、MEMS、OLED及PV應用和一般的半導體封裝。對於LED、OLED、MEMS及薄膜PV封裝的密閉密封存在顯著的需求，以保護裝置免受濕氣侵入。使用適當的施加和燒結，該材料可以表現出密閉或近密閉的密封行為。該材料可以在製造製程的各個階段中被施加於上述裝置：無論是在晶圓黏結的晶圓層次、或在經由膜層壓和黏合的封裝製程中、或漿料噴射/分配之後為蓋或玻璃或積層蓋黏附和燒結。低溫燒結能夠產生高CTE不匹配堆疊以及溫度敏感材料堆疊的組件。
7. ACF替換。該材料的凸塊陣列可以經由模板印刷、凸塊轉移、或高速噴射分配被遞送到基材。這樣的陣列可用以作為組裝裝置的電觸點，無需明確的高度對準。

Claims (45)

  1. 一種燒結粉末，包含：一第一類型金屬顆粒，具有一100nm至50μm的平均最長尺寸。
  2. 如請求項1所述之燒結粉末，其中至少一部分的該第一類型金屬顆粒被至少部分塗覆一包覆劑，較佳為一包含一羧酸酯及/或胺官能基的包覆劑。
  3. 如請求項1或2所述之燒結粉末，其中該第一類型金屬顆粒的該包覆劑包含一直鏈或支鏈脂族酸，較佳為油酸。
  4. 如請求項1或請求項2所述之燒結粉末，包含多達5wt%的包覆劑，較佳從0.1至3wt%的包覆劑，更佳約0.5wt%的包覆劑。
  5. 如請求項1或請求項2所述之燒結粉末，其中該第一類型金屬顆粒具有一從100nm至20μm的平均最長直徑。
  6. 如請求項1或請求項2所述之燒結粉末，其中該第一類型金屬顆粒具有一從1至3μm的D50。
  7. 如請求項1或請求項2所述之燒結粉末，其中該第一類型金屬顆粒具有一從3.5至5.5g/cc的振實密度。
  8. 如請求項1或請求項2所述之燒結粉末，進一步包含一第二類型金屬顆粒，該第二類型金屬顆粒具有一小於100nm的平均最長尺寸，其中該第二類型金屬顆粒被至少部分塗覆一包覆劑。
  9. 如請求項8所述之燒結粉末，其中該第二類型金屬顆粒具有一從5至75nm的平均最長尺寸。
  10. 如請求項8所述之燒結粉末，包含從1至19wt%的該第一類型金屬 顆粒及從81至99wt%的該第二類型金屬顆粒，較佳從5至15wt%的該第一類型金屬顆粒及從85至95wt%的該第二類型金屬顆粒。
  11. 如請求項8所述之燒結粉末，其中該第一類型金屬顆粒及/或第二類型金屬顆粒包含銀或一合金或塗覆銀的顆粒之核殼結構。
  12. 如請求項8所述之燒結粉末，其中該第二類型金屬顆粒的該包覆劑包含一胺及/或一羧酸酯官能基。
  13. 如請求項8所述之燒結粉末，其中該第二類型金屬顆粒的該包覆劑包含一直鏈或支鏈脂族胺，較佳為辛胺。
  14. 如請求項8所述之燒結粉末，包含：從1至10wt%的一第一類型金屬顆粒，該第一類型金屬顆粒具有一從100nm至20μm的平均最長尺寸，該金屬顆粒至少部分塗覆有一油酸包覆劑；以及從90至99wt%的一第二類型金屬顆粒，該第二類型金屬顆粒具有一從5至75nm的平均最長尺寸，其中該第二類型金屬顆粒係至少部分塗覆有一辛胺包覆劑。
  15. 一種燒結粉末，包含：具有一小於100nm的平均最長尺寸的金屬顆粒，其中至少一些該金屬顆粒係至少部分塗覆有一包覆劑。
  16. 如請求項15所述之燒結粉末，其中該金屬顆粒具有一從5至75nm的平均最長尺寸。
  17. 如請求項15所述之燒結粉末，其中該金屬顆粒具有一從500nm至5μm的平均最長尺寸。
  18. 如請求項15至17中任一項所述之燒結粉末，其中該包覆劑包含一 胺及/或羧酸酯官能基。
  19. 如請求項15至17中任一項所述之燒結粉末，其中該包覆劑包含一直鏈或支鏈脂族胺，較佳為辛胺。
  20. 一種使用任何前述請求項的燒結粉末形成的燒結接點。
  21. 一種包含如請求項20所述之燒結接點的發光二極體(LED)、微機電系統(MEMS)、有機發光二極體(OLED)或光伏電池。
  22. 一種燒結漿料，包含：如請求項1至19中任一項所述之燒結粉末；一黏結劑；一溶劑；以及可選的一流變改質劑及/或一有機銀化合物及/或一活化劑及/或一界面活性劑及/或潤濕劑及/或過氧化氫或有機過氧化物。
  23. 如請求項22所述之燒結漿料，其中該黏結劑包含一環氧基樹脂。
  24. 如請求項22或請求項23所述之燒結漿料，其中該溶劑包含一單萜醇及/或一二醇及/或二醇醚，較佳為一萜品醇及/或二乙二醇單正丁基醚。
  25. 如請求項22或請求項23所述之燒結漿料，包含：從1至15wt%的黏結劑；及/或從1至30wt%的溶劑；及/或多達5wt%的流變改質劑；及/或多達10wt%的一有機銀化合物；及/或多達2wt%的活化劑；及/或多達6wt%的界面活性劑；及/或 多達2wt%的過氧化氫或有機過氧化物。
  26. 一種燒結漿料，包含：如請求項1至19中任一項所述之燒結粉末；一有機銀化合物；一溶劑；以及可選的一活化劑及/或流變改質劑及/或界面活性劑。
  27. 如請求項26所述之燒結漿料，包含：從1至30wt%的溶劑；及/或多達50wt%的有機銀化合物，較佳從0.1至25wt%，更佳從0.1至10wt%，甚至更佳從0.1至9wt%；及/或多達5wt%的流變改質劑；及/或多達2wt%的活化劑；及/或多達6wt%的界面活性劑；及/或多達2wt%的過氧化氫或有機過氧化物。
  28. 如請求項22、23、26及27中任一項所述之燒結漿料，其中該有機銀化合物包含草酸銀、乳酸銀、琥珀酸銀、新癸酸銀、檸檬酸銀及硬脂酸銀中之一者或更多者。
  29. 如請求項22、23、26及27中任一項所述之燒結漿料，進一步包含一脂肪酸及或潤濕劑，較佳為以下中之一者或更多者：短或長鏈(C=2至30)羧酸或二羧酸或羥基羧酸，更佳為月桂酸、硬脂酸、新癸酸、硬脂酸、油酸、草酸、丙二酸、琥珀酸、己二酸、馬來酸、檸檬酸或乳酸；或 短或長鏈(C=2至30)胺，更佳為丁胺、己胺、辛胺、十二烷胺或十六烷胺；或界面活性劑，更佳為triton X100、IGEPAL CA-630或月桂基葡糖苷。
  30. 如請求項22、23、26及27中任一項所述之燒結漿料，進一步包含一過氧化物，較佳為過氧化氫或一有機過氧化物。
  31. 如請求項22、23、26及27中任一項所述之燒結漿料，其中該漿料實質上不含樹脂。
  32. 如請求項22、23、26及27中任一項所述之燒結漿料，其中該漿料係可印刷及/或可分配及/或可噴射及/或針可轉移及/或表現出大於200W/mK的導熱率及/或能夠提供從25至45MPa的晶粒切變強度。
  33. 如請求項22、23、26及27中任一項所述之燒結漿料，進一步包含一膜成形劑。
  34. 一種燒結膜，包含如請求項1至19中任一項所述之燒結粉末及一黏結劑。
  35. 一種晶粒黏附方法，包含以下步驟：(i)將如請求項34所述之燒結膜放在一晶粒與一待接合基材之間；以及(ii)燒結該燒結膜，其中該燒結之進行未施加壓力。
  36. 如請求項35所述之方法，其中該燒結係於一從150至400℃的溫度下進行長達120分鐘。
  37. 如請求項35或36所述之方法，其中步驟(i)包含以下步驟：(a)將該燒結膜施加於該晶粒以形成一組件，該組件具有一晶粒側及一燒結膜 側；以及(b)使該組件之該燒結膜側與該基材接觸。
  38. 如請求項37所述之方法，其中步驟(a)係於一從15至400℃的溫度及一從0.1至5MPa的壓力下進行0.1至60秒。
  39. 如請求項37所述之方法，其中步驟(b)係於一從15至400℃的溫度及一從0.1至40MPa的壓力下進行0.1至60分鐘。
  40. 一種晶粒黏附方法，包含以下步驟：(i)將如請求項34所述之燒結膜放在一晶粒與一待接合基材之間；以及(ii)燒結該燒結膜，其中該燒結係在施加一從0.1至40MPa的壓力時進行。
  41. 一種晶圓黏著方法，包含以下步驟：(i)將如請求項34所述之燒結膜放在兩個或更多個待接合晶圓之間；以及(ii)燒結該燒結膜，其中該燒結之進行未施加壓力。
  42. 一種轉移一燒結膜至一元件的方法，包含以下步驟：將如請求項34所述之燒結膜施加於一基材以形成一組件，該組件具有一燒結膜側及一基材側；使該組件之該燒結膜側與一元件接觸；將該組件加熱至一從50至200℃的溫度；對該組件施加一從1至5MPa的壓力持續0.1秒至60分鐘；以及從該燒結膜分離該基材。
  43. 如請求項1至19中任一項所述之燒結粉末或如請求項22至33中任 一項所述之燒結漿料或如請求項34所述之燒結膜在一方法中的用途，該方法係選自：晶粒黏附、晶圓對晶圓黏著、反射層印刷、密閉及近密閉的密封、燒結包含形成於一背層上的一膜中的一燒結粉末及一黏結劑的膜、互連線的分配及生產。
  44. 一種製造一燒結接點的方法，包含以下步驟：在兩個或更多個待接合工件附近提供如請求項1至19中任一項所述之燒結粉末或如請求項22至33中任一項所述之燒結漿料或如請求項34所述之燒結膜；以及加熱該燒結粉末或燒結漿料或燒結膜以至少部分燒結該金屬。
  45. 如請求項44所述之方法，其中該加熱係於一至少140℃、較佳從150℃至300℃的溫度下進行。
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