TW201609993A - 製造金屬粉末的方法 - Google Patents

製造金屬粉末的方法 Download PDF

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Publication number
TW201609993A
TW201609993A TW104111974A TW104111974A TW201609993A TW 201609993 A TW201609993 A TW 201609993A TW 104111974 A TW104111974 A TW 104111974A TW 104111974 A TW104111974 A TW 104111974A TW 201609993 A TW201609993 A TW 201609993A
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Taiwan
Prior art keywords
powder
silver
acid
sintered
metal powder
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TW104111974A
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English (en)
Inventor
恰奇尼馬雅庫瑪
羅伊寶拉米希谷帕塔
沙卡蘇利
木克吉蘇塔巴
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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 TW201609993A publication Critical patent/TW201609993A/zh

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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • 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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    • 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
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract

一種用於製造金屬粉末之方法，該方法包括：提供鹼性金屬鹽溶液；將鹼性金屬鹽溶液與還原劑接觸以從該鹼性金屬鹽溶液中沉澱金屬粉末；及從溶劑中回收沉澱的金屬粉末。

Description

製造金屬粉末的方法
本發明係關於用於製造金屬粉末之方法及根據該方法製造之金屬粉末。
燒結接頭提供焊接接頭之替代物。形成燒結接頭之典型方法涉及在兩個待接合工件之間放置金屬粉末(常常是粉末壓胚形式)，然後燒結金屬粉末。所得的金屬原子之原子擴散在兩個工件之間形成鍵結。
金屬奈米粉末已在電子工業中用以形成燒結接頭，且被視為無鉛焊料之實用替代物。奈米材料與對應之塊體材料之間的不同特性被認為歸因於具有更高表面積與體積比之奈米材料。
已知含銀奈米粒子之燒結粉末。藉由銀奈米粒子之原子擴散而形成之燒結接頭可在顯著低於塊體材料熔化溫度之一溫度下處理，且亦可用於高溫應用。諸如高溫穩定性、高電導率及熱傳導率以及優良機械特性之潛在優勢使該種燒結粉末成為用於晶粒附著應用之有希望候選者。然而，該種燒結粉末之燒結溫度對大多數電子應用中的有效使用而言仍然過高。
可藉由在燒結期間施加外部壓力而降低燒結溫度。作為晶粒附著方法，銀膏之壓力輔助低溫燒結已經證明是焊料回流之可行替代方法。高壓之施加已經證明顯著降低燒結溫度，且可以相對更快速率獲得用於晶粒附著之所需特性，從而使得燒結接頭在數分鐘之內形成。然 而，較大外部壓力使得製程之自動化較為困難。此外，較大外部壓力之施加可導致工件損壞。
已知施配焊錫膏以用於多種應用，但主要在不可能進行波焊或網印之情況下用作替代物。可在多種表面安裝應用中將焊錫膏施配在印刷電路板、積體電路封裝及電力組件連接器上。焊錫膏之典型問題包括：滴液、跳點，及施配不一致。軟焊料及硬焊料通常在電子工業用於晶粒附著及施配。軟焊料在熱循環條件下易於疲勞斷裂影響。另一方面，硬焊料及玻璃基質複合物用以賦能裝置在更高接面溫度下使用，但硬焊料及玻璃基質複合物之更高彈性模數及處理溫度可在裝置中產生高機械應力，且該等材料亦具有相對較低之熱傳導率及電導率。
本發明尋求解決與先前技術相關聯之至少一些問題或至少提供對先前技術的商業上可接受之替代解決方案。
在第一態樣中，本發明提供用於製造金屬粉末之方法，該方法包括以下步驟：提供鹼性金屬鹽溶液；將鹼性金屬鹽溶液與還原劑接觸以從該鹼性金屬鹽溶液中沉澱金屬粉末；及從溶劑中回收沉澱的金屬粉末。
如本文中定義之每一態樣或實施例可與任何其他態樣或實施例組合，除非本文中另有明確的相反指示。特定而言，被指示為較佳或有優勢的任何特徵可與被指示為較佳或有優勢的任何其他特徵組合。
如本文中所使用，術語「燒結粉末」可包含能夠形成燒結接頭之粉末。燒結接頭是由置於兩個待接合工件之間的金屬粒子之原子擴 散形成的。術語「燒結粉末」可包含微粒。燒結粉末可包括規則形狀粒子(例如球形)或不規則形狀粒子(例如鬚狀、板塊、條狀或片狀)。
如本文中所使用，術語「封端劑」可包含一物種，當該物種在金屬粒子表面上存在時會減少金屬粒子黏聚，在粉末產生期間賦能粒度控制，且減少粒子的表面氧化或其他污染。
發明者已令人驚訝地發現根據該方法製造之金屬粉末可展現大於2g/cm3，通常大於3g/cm3，更通常自3.5g/cm3至5.5g/cm3之敲緊密度。敲緊密度越低，可導致越強的粒子聚合。因此，由本文中所述方法製造之粉末易於操縱，且可用以形成細線。較低的敲緊密度可導致不適宜地非緊密及多孔燒結接頭。可在標準程序下藉由使用敲緊密度計測量敲緊密度。
金屬粉末的粒徑通常為微米級的，且可展現提供尤其有優勢的燒結特性之粒徑分佈。例如，粉末通常展現從500nm至10μm之D50。可藉由使用動態光散射方法或雷射散射方法，利用粒度分析器測量D50。形成粉末之粒子中之大多數有利地具有從100nm至50μm之最長尺寸，較佳為從100nm至30μm。通常，形成粉末之大體上全部粒子將已具有該等範圍中之最長尺寸。當粒子為球形時，最長尺寸將為球體之直徑。
金屬粉末所展現之粒徑、粒徑與形狀分佈及敲緊密度值之組合可使得例如在高密度、低孔隙率的燒結金屬接頭之製造中，粉末可尤為有效地用作燒結粉末。該種接頭可擴展工業及汽車應用中必需之現代功率模組之功率及熱循環能力。
發明者已令人驚訝地發現根據本發明之方法製造之粉末可在相對較低溫度下燒結，僅需施加極低壓力，通常大體上無壓力。因此， 工件之間藉由使用金屬粉末進行的燒結接頭之成型可在減少對工件之損害的情況下進行。另外，由於並非必須施加高壓，因此燒結接頭之成型得以簡化，且可更易於自動化。此外，與奈米粒徑粒子相比，利用僅少量封端劑可避免金屬粒子之黏聚。因此，與僅包括奈米粒徑粒子的燒結粉末相比，包含在所得燒結接頭中的殘餘有機物的量減少，由此改良接頭之機械特性。
鹼性金屬鹽溶液通常為含水的，且通常展現大於7，更通常大於約7.5，更佳為約8之pH。可藉由含金屬之氫氧化物的存在來提供高pH值，氫氧化物例如氫氧化鈉。替代地或另外，可藉由三級有機鹼之存在來提供高pH值，三級有機鹼例如三乙胺。
尤其適合之金屬鹽溶液是金屬硝酸鹽溶液。金屬硝酸鹽溶液之實例包括，例如，硝酸銀溶液及硝酸銅溶液。金屬硝酸鹽溶液可包括表面活化劑，例如DAXAD。
形成金屬粉末之金屬粒子可全部包括相同金屬。或者，粒子中之一些粒子可包括不同的金屬。另外，個別顆粒可包括兩種或兩種以上的不同金屬。如本文中所使用，術語「金屬」可包含合金或核殼結構。因此，粒子可包括一或更多種金屬之一或更多種合金或核殼結構。
形成所得金屬粉末之粒子的形狀是藉由球形、具有刻面、不規則形、薄片或上述各者中兩個或兩個以上之組合。
可藉由例如過濾及/或傾析及/或離心來從溶劑中回收沉澱金屬粉末。經過濾及/或傾析及/或離心之金屬粉末可隨後經受例如沖洗及/或乾燥。
還原劑較佳包括肼、甲醛及硼氫化物中之一或更多者。該種還原劑在為所得金屬粉末提供適宜的粒徑分佈及敲緊密度值方面尤其 有效。就此而言，包括肼與氫氧化物之組合之還原劑尤為較佳。此令人驚訝，因為在該項技術中，應理解，使用肼通常導致奈米粒徑粒子的成型。在不受理論約束之情況下，氫氧化物與肼組合之存在及(初始時)反應介質中沒有任何封端劑被認為藉由奧士華熟化製程而降低反應速率及增強較大粒子之生長，由此導致微米粒徑粒子的成型，該等粒子具有比奈米粒徑粒子更適宜之粒徑分佈。延遲添加封端劑(見下文)被進一步認為導致粒子黏聚之適宜的粒徑分佈。適合還原劑之實例包括例如水合肼、鹼性甲醛溶液，及硼氫化鈉。
較佳地，該方法進一步包括在使鹼性金屬鹽溶液與還原劑接觸之後，使鹼性金屬鹽溶液與封端劑接觸。換言之，較佳在已將還原劑添加至溶液中之後但在從溶劑中回收沉澱的金屬粒子之前添加封端劑。封端劑可至少部分地塗佈在形成金屬粉末之粒子的表面，且可因此有助於減少粒子之不受控制的黏聚。更高程度之不受控制的黏聚是不適宜的，因為此黏聚可能降低敲緊密度且將產生非緊密及多孔燒結接頭。使用封端劑可有助於避免金屬降級，例如由於金屬曝露於空氣所引起之損害。此外，在添加還原劑之後添加封端劑可有助於產生適宜的粒度分佈及敲緊密度值。封端劑較佳在還原劑之後與溶液接觸至少1秒鐘，更佳在還原劑之後接觸2秒鐘，甚至更佳接觸2秒鐘至600秒鐘，甚至再更佳接觸3秒鐘至120秒鐘。在一特定較佳之實施例中，封端劑在還原劑之後與溶液接觸約5秒鐘。
封端劑可包括例如脂肪酸及酯、醯胺、胺、表面活化劑及/或聚合物。封端劑較佳包括脂肪酸，更佳包括月桂酸、棕櫚酸、硬脂酸、異硬脂酸及油酸中之一或多種。該等封端劑在阻止形成金屬粉末之金屬粒子發生聚集方面尤其有效。
該方法較佳進一步包括碾磨回收之沉澱金屬粉末。該種碾磨可導致形成具有扁平的或「薄片狀」形狀的金屬粉末之粒子之比例增大。例如，粉末通常可包括至少10體積%之具有薄片狀形狀之粒子，更通常包括從20體積%至80體積%之該種粒子。增加碾磨時間可能增大薄片狀粒子之比例及深寬比。具有薄片狀粒子比例更高的該種粒度分佈之粉末可展現與包括球形粒子之粉末相比得到增強的緊實度，且可能由此展現更適宜的燒結特性。此外，包括該種粉末的漿料可能展現增大的黏度，且可能因此更易於操縱。此外，具有該種粉末之漿料顯示對基板及工件之增強潤濕行為，此歸因於與僅用敲緊密度較低之球狀粒子製成之漿料相比，該漿料中存在具有適當粒徑、深寬比、分佈及敲緊密度之薄片狀粒子。潤濕之增強對在兩個工件之間形成強鍵極為重要，此結果歸因於金屬原子在燒結期間之原子擴散。具有本文所述之敲緊密度、粒徑及深寬比分佈之薄片形狀之組合產生一金屬粉末，該金屬粉末展現尤其適宜的燒結特性。
較佳藉由使用球磨機來執行碾磨。使用球磨機在保持適宜的粒徑分佈及敲緊密度值之同時增大薄片狀粒子比例方面尤為有效。適合之球磨機實例是藉由使用氧化鋯珠之磨碎機球磨機。較佳珠粒直徑包括例如自0.05mm至2mm，較佳約為0.1mm。
較佳在存在脂肪酸之情況下執行碾磨，該脂肪酸較佳為月桂酸、棕櫚酸、硬脂酸、異硬脂酸及油酸中之一或更多者；及/或在存在聚合物之情況下執行碾磨，該聚合物較佳為PEG 400；及/或在存在多胺之情況下執行碾磨，該多胺較佳為三伸乙四胺。該等物種可在碾磨期間充當封端劑，由此用以減少粉末在碾磨期間及在使用之前聚集及/或氧化。
碾磨較佳執行達至少30分鐘，較佳為至少90分鐘。增長的碾磨時間可能增大具有薄片狀形狀之粒子之比例。
金屬較佳包括銀、銅及上述各者中一或更多者之合金中之一或更多者。該等金屬展現高電導率及熱傳導率，且因此在粉末用於諸如晶粒附著及微電子封裝之電子應用中時尤其有利。適合之銀合金包括例如AgSn、AgPd、AuAg、AgCu及AgNi。金屬粒子可包括銀塗佈粒子之核殼結構，例如銀塗佈銅、銀塗佈鎳、銀塗佈CuNi、銀塗佈CuNiZn及銀塗佈BN。
當粒子包括銀時，粉末可能有利地展現以下粒徑分佈：D90，自3μm至6μm，較佳自4μm至5.5μm；及/或D50，自0.9μm至2μm，較佳自1μm至1.8μm；及/或D10，自0.3μm至0.8μm，較佳自0.5μm至0.75μm。當粒子包括銅時，粉末可能有利地展現以下粒徑分佈：D90，自4μm至15μm，較佳自10μm至13μm；及/或D50，自2μm至10μm，較佳自4μm至6μm；及/或D10，自0.5μm至3μm，較佳自1.5μm至2.5μm。結合適宜的敲緊密度值，此情況可使粉末能夠用於高密度及低孔隙率之燒結接頭的製造中。銅粒子可為具有刻面。
在一特定較佳之實施例中，該金屬包括銀；及還原劑包括肼；該方法進一步包括以下步驟：在使鹼性金屬鹽溶液接觸還原劑之後，使鹼性金屬鹽溶液接觸油酸封端劑；及在存在油酸封端劑之情況下，藉由使用球磨機碾磨回收之沉澱金屬 粉末達至少30分鐘。
由該種方法製造之金屬粉末展現尤為適宜之粒度分佈及敲緊密度值，且可能展現上文論述之適宜的粒徑分佈。
當金屬包括銅時，該方法較佳進一步包括將鍍銀層塗覆至形成粉末之粒子上。該種銀塗佈銅粒子展現銀粒子之較高電導率及熱傳導率，成本相對低於銅粒子。銀塗佈銅粒子較佳展現以下粒徑分佈：D90，自4μm至13μm，較佳自9μm至12μm；及/或D50，自1μm至10μm，較佳自4μm至5.5μm；及/或D10，自0.5μm至3μm，較佳自2μm至2.8μm。
塗覆鍍銀層之操作較佳包括以下步驟：從銅粒子上蝕刻氧化物層；及藉由使用電鍍將銀塗層塗覆至銅粒子。
該種方法在塗佈銅粒子時尤其有效。在一個實施例中，藉由使用諸如三伸乙四胺之多胺執行蝕刻，且在存在溶於去離子水及檸檬酸中之水溶性銀鹽的情況下執行電鍍。在一替代性實施例中，藉由使用硫酸銨與氫氧化銨之組合來執行兩步驟蝕刻，然後利用諸如三伸乙四胺之多胺進行處理。
該方法較佳進一步包括將脂肪酸塗層塗覆至銀塗佈粒子上。脂肪酸塗層充當封端劑，且可能由此用以減少形成金屬粉末之金屬粒子之黏聚及/或氧化。
在又一實施例中，本發明提供製造銅粉末之方法，該方法包括以下步驟：提供銅粉末；及在存在聚合物及/或多胺之情況下，藉由使用球磨機碾磨銅粉末。
所得銅粉末可主要包括展現「薄片狀」形狀之粒子。所得粉末可展現自500nm至10μm之D50值及/或大於2g/cm3之敲緊密度。聚合物可包括例如PEG 400及/或諸如三乙烯三胺之多胺。
在又一態樣中，本發明提供根據本文所述之方法製造之金屬粉末。
在又一態樣中，本發明提供金屬粉末，該金屬粉末具有：自500nm至10μm之D50；及大於2g/cm3之敲緊密度，其中該金屬粉末包括銀、銅及上述各者中一或更多者之合金中之一或更多者。
由金屬粉末展現之粒徑分佈及敲緊密度值組合可能使得粉末可尤其有效地用作燒結粉末，例如用於高密度、低孔隙率之燒結金屬接頭之製造中之燒結粉末。
金屬粉末可有利地具有較低水平的有機物，例如小於5wt.%之有機物，較佳小於3wt.%之有機物，更佳小於1wt.%之有機物，更佳小於0.5wt.%之有機物。(在本文中使用之術語wt.%之有機物係指藉由熱或化學分析測得之碳的wt.%。)
金屬粉末可有利地展現低比表面積(specific surface area；BET)，例如比表面積小於1.5m2/g，較佳小於1m2/g，更佳小於0.8m2/g。
在又一態樣中，本發明提供藉由使用如本文所述之金屬粉末所形成之燒結接頭。該種燒結接頭可展現特別高的強度及/或特別高的電導率及熱傳導率。此外，燒結接頭在熱衝擊之後可展示極少的抗剪強度變化，抗剪強度通常大體上無變化。
在又一態樣中，本發明提供發光二極體(light-emitting diode；LED)、微機電系統(microelectromechanical system；MEMS)、有機發光二極體(organic light-emitting diode；OLED)、光伏打電池(photovoltaic cell；PV cell)、功率電子設備，或在聚合物或其他可撓性或可成形基板上之印刷電子設備，該等基板包括本文所述之燒結接頭。
在又一態樣中，本發明提供燒結漿料，該漿料包括：如本文所述之金屬粉末；黏合劑；溶劑；及視需要，流變改質劑及/或有機銀化合物及/或活化劑及/或表面活化劑及/或潤濕劑及/或過氧化氫或有機過氧化物。
漿料可為可印刷及/或可施配及/或可噴射及/或可針式轉印的。漿料可具有特別適宜於施配之黏度及流動特性，意謂著該漿料可用作焊料之一對一替代物。
與此項技術中已知的燒結漿料相比，本發明之燒結漿料在室溫下展現高穩定性。此意謂著燒結漿料無需低溫儲存。此為本發明之燒結漿料之一特別重要優勢。
通常選擇黏合劑及/或溶劑，以使得能夠在低於燒結粉末之目標燒結溫度的溫度下從漿料中移除該等黏合劑及/或溶劑(例如藉由蒸發及/或燒盡)。此可能有助於促使金屬粒子之近乎完全燒結。當有機材料在燒結期間殘留在接頭中時，金屬粒子可能發生不充分燒結。此舉可能產生脆弱的燒結接頭。
黏合劑可用以將漿料黏合在一起，以使得漿料更易於操縱及 準確地在所需之燒結接頭之位置中定位。適合黏合劑實例包括但不限定於：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，例如聚胺甲酸酯、聚三聚氰酸酯、環氧樹脂、聚醯亞胺、三聚氰胺樹脂及雙馬來醯亞胺樹脂。特別較佳之實例包括羥基丙基甲基纖維素、三乙酸甘油酯及聚乙酸乙烯酯。較佳地，該黏合劑包括環氧基樹脂。環氧基樹脂在將漿料黏合在一起方面特別有效，以便更易於操縱漿料，且可更易於在所需之燒結接頭之位置中準確定位。此外，使用環氧樹脂可能在燒結之前導致更強固接頭之形成，意謂著在燒結之前無需將待接合工件固持在一起。在封端劑包括胺官能基時，使用環氧樹脂特別有利。在該情況下，胺充當形成交聯結構之硬化劑。此情況可在燒結之前產生特別強固之接頭。
溶劑較佳包括單萜乙醇及/或乙二醇及/或乙二醇醚，較佳包括萜品醇及/或二乙二醇單正丁醚。單萜乙醇及/或乙二醇醚可特別有效地用於在漿料內散佈金屬粒子，從而產生金屬粒子在有機組分基質中之均質分佈，同時降低群集聚集及/或黏聚。使用單萜乙醇及/或乙二醇醚可用以提高燒結漿料之流動能力及列印機能力。
可添加流變改質劑以控制漿料之黏度。適合之流變改質劑之實例包括但不限於：短鏈或長鏈(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、丁二酸、己二酸、馬來酸、檸檬酸、乳酸，或短鏈或長鏈(C=2至30)胺類，例如丁胺、己胺、辛胺、十二烷胺、十六烷胺、Thixcin R及Crayvallac Super，或上述各者中兩個或兩個以上者之組合。
在燒結期間，有機銀化合物可能分解為金屬銀，從而可提高燒結接頭之熱傳導率。此外，有機銀化合物之存在提高漿料對接頭界面 之潤濕度。有機銀化合物可包括短鏈或長鏈羧酸(C=1至30)中之一或更多者，該等羧酸例如硬脂酸銀、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，可省去有機銀化合物。
可添加活化劑以從印刷表面移除可能存在之任一金屬氧化物，及/或移除可能存在於燒結粉末中之任一氧化物。芳基或烷基羧酸可用作活化劑，該等羧酸例如己二酸、丁二酸及戊二酸中之一或更多者。
可將表面活化劑添加至燒結漿料中以協助將燒結粉末散佈在燒結漿料中。適合之表面活化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括過氧化物。適合過氧化物之實例包括但不限於過氧化氫或有機過氧化物，例如第三丁基氫過氧化物及過氧-2-乙基己酸第三丁酯。過氧化物將氧引入漿料，從而在晶粒附著方法中可協助漿料在晶粒區域下方之燒結。氧亦可使金屬粒子能夠在惰性氣氛下燒結，該惰性氣氛例如氮氣氛。燒結漿料較佳包括高達3wt.%之過氧化氫或有機過氧化物，較佳包括自0.5wt.%至2wt.%之過氧化氫或有機過氧化物，更佳包括自0.7wt.%至1.8wt.%之過氧化氫或有機過氧化物。液態過氧化物較佳用於控制流變學及銀沉降。
燒結漿料較佳包括：自1wt.%至15wt.%之黏合劑；及/或自1wt.%至30wt.%之溶劑；及/或高達5wt.%之流變改質劑；及/或高達10wt.%之有機銀化合物；及/或高達2wt.%之活化劑；及/或 高達6wt.%之表面活化劑；及/或高達2wt.%之過氧化氫或有機過氧化物。
該等範圍內之黏合劑及/或溶劑含量可有助於為燒結漿料提供特別合乎需要的流動能力及列印機能力。較佳燒結漿料包括自2wt.%至8wt.%之黏合劑。在一個實施例中，燒結漿料包括約4.5wt.%之黏合劑。較佳燒結漿料包括自5wt.%至30wt.%之溶劑。在一個實施例中，燒結漿料包括約26wt.%之溶劑。燒結漿料可包括0至5wt.%之流變改質劑及/或0至2wt.%之活化劑及/或0至6wt.%之表面活化劑及/或0至2wt.%之過氧化氫或有機過氧化物。燒結漿料可包括自62wt.%至90wt.%之燒結粉末。燒結粉末可形成燒結漿料之餘量。
在又一態樣中，本發明提供燒結漿料，該燒結漿料包括：如本文所述之金屬粉末；有機銀化合物；溶劑；及視需要，活化劑及/或流變改質劑及/或表面活化劑及/或過氧化氫或有機過氧化物。
在燒結期間，有機銀化合物可能分解為金屬銀，從而可提高燒結接頭之熱傳導率。此外，有機銀化合物之存在提高漿料對接頭界面之潤濕度。有機銀化合物可包括短鏈或長鏈羧酸(C=1至30)中之一或更多者，該等羧酸例如硬脂酸銀、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，可省去有機銀化合物。
燒結漿料較佳進一步包括脂肪酸及/或潤濕劑，該脂肪酸及/或潤濕劑較佳為以下各者中之一或更多者：短鏈或長鏈(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、丁二酸、己二酸、馬來酸、檸檬酸，或乳酸；或短鏈或長鏈(C=2至30)胺類，更佳為丁胺、己胺、辛胺、十二烷胺，或十六烷胺；或表面活化劑，更佳為氚核X100、IGEPAL CA-630或月桂基葡糖苷。
脂肪酸之存在有助於將漿料黏合在一起。換言之，脂肪酸之存在避免對單獨黏合劑之需求，該單獨黏合劑如上文論述之環氧基樹脂黏合劑。因此，漿料中之有機物總量減少，從而產生更強健之最終接頭。
燒結漿料較佳進一步包括過氧化物。適合過氧化物之實例包括但不限於過氧化氫或有機過氧化物，例如第三丁基氫過氧化物及過氧-2-乙基己酸第三丁酯。過氧化物將氧引入漿料，從而在晶粒附著方法中可協助漿料在晶粒區域下方之燒結。氧亦可使金屬粒子能夠在惰性氣氛下燒結，該惰性氣氛例如氮氣氛。燒結漿料較佳包括高達3wt.%之過氧化氫或有機過氧化物，較佳包括自0.5wt.%至2wt.%之過氧化氫或有機過氧化物，更佳包括自0.7wt.%至1.8wt.%之過氧化氫或有機過氧化物。液態過氧化物較佳用於控制流學及銀沉降。
燒結漿料可包括成膜劑，例如聚醯胺、聚異丁烯、聚醯胺蠟流變改質劑及基於蓖麻油之觸變劑。
較佳地，燒結漿料大體上不含樹脂，更佳完全不含樹脂。樹脂之存在可降低銀之熱傳導及電導。溶劑較佳包括單萜乙醇及/或乙二醇及/或乙二醇醚，更佳包括萜品醇及/或二乙二醇單正丁醚。
燒結漿料較佳包括：自1wt.%至30wt.%之溶劑；及/或高達50wt.%之有機銀化合物，較佳自0.1wt.%至25wt.%，更佳 自0.1wt.%至10wt.%，甚至更佳自0.1wt.%至9wt.%；及/或高達5wt.%之流變改質劑；及/或高達2wt.%之活化劑；及/或高達6wt.%之表面活化劑；及/或高達2wt.%之過氧化氫或有機過氧化物。
燒結漿料可包括0至5wt.%之流變改質劑及/或0至2wt.%之活化劑及/或0至6wt.%之表面活化劑及/或0至2wt.%之過氧化氫或有機過氧化物。燒結粉末可形成燒結漿料之餘量。
在又一態樣中，本發明提供燒結薄膜，該薄膜包括如本文所述之金屬粉末及黏合劑。薄膜可以晶圓級、晶粒級、封裝/基板級及/或模組級塗覆。該種薄膜可藉由在聚酯板上印刷如本文所述之燒結漿料，加熱漿料以至少部分地移除溶劑及形成薄膜，然後從聚酯板上移除薄膜而獲得。本文所述之薄膜尤其有利，因為僅藉由在略高溫度下將晶粒壓至薄膜上即可轉印該薄膜。轉印薄膜是備用塗覆方法，該方法可在某些情況下以有利方式提供。薄膜可在聚合物基板、玻璃基板、金屬基板或陶瓷基板上形成，或直接在晶圓上形成。薄膜可位於包括聚酯之聚合物基板上。薄膜可在聚合物基板上形成，其中該聚合物基板包括脫模塗層。可藉由材料之印刷或鑄造來塗覆漿料組成物，從而產生薄膜。可藉由在連續層中印刷來產生薄膜。或者，可藉由印刷以形成離散形狀陣列來產生薄膜。
在又一態樣中，本發明提供晶粒附著之方法，該方法包括以下步驟：(i)將本文所述之燒結薄膜置於待接合之晶粒與基板之間；及(ii)燒結該燒結薄膜， 其中在不施加壓力之情況下執行燒結。
此「低壓」或「無壓」燒結尤其有利，因為此燒結可使製程自動化更簡易。此外，可減少對工件之損害。優於使用加壓燒結之方法的其他優勢包括：晶粒放置所需時間更短(高UPH)、用於放置之低壓要求(非常有利於處理薄晶圓)、與商售晶粒接合器之相容性，及在外部加熱設備中燒結(分批製程以改良UPH)。
較佳在自150℃至400℃之溫度下執行燒結長達120分鐘。該等條件可使得燒結薄膜進行尤為有效的燒結，同時避免對工件之損害。
步驟(i)較佳包括以下步驟：(a)將燒結薄膜塗覆至晶粒上以形成具有晶粒側面及燒結薄膜側面之組合件；及(b)使組合件之薄膜側面接觸基板。
該種步驟可使得製程自動化更為簡單，且可例如藉由使用壓印器而執行。
步驟(a)較佳在自15℃至400℃之溫度下及自0.1MPa至5MPa之壓力下執行長達自0.1秒鐘至60秒鐘之久。該等條件可使得尤為有效的塗覆燒結薄膜，同時避免對晶粒之損害。
步驟(b)較佳在自15℃至400℃之溫度下及自0.1MPa至40MPa之壓力下執行長達自0.1分鐘至60分鐘之久。該等條件可使得晶粒與基板進行尤為有效的接觸，同時避免對晶粒或基板之損害。
在又一態樣中，本發明提供晶粒附著之方法，該方法包括以下步驟：(i)將本文所述之燒結薄膜置於待接合之晶粒與基板之間；及 (ii)燒結該燒結薄膜，其中在施加自0.1MPa至40MPa之壓力的同時執行燒結。
在又一態樣中，本發明提供晶圓結合之方法，該方法包括以下步驟：(i)將本文所述之燒結薄膜置於兩個或兩個以上待接合晶圓之間；及(ii)燒結該燒結薄膜，其中在不施加壓力之情況下執行燒結。
在又一態樣中，本發明提供將燒結薄膜轉印至組件的方法，該方法包括以下步驟：將本文所述之燒結薄膜塗覆至基板上以形成具有燒結薄膜側面及基板側面之組合件；使組合件之燒結薄膜側面接觸組件；將組合件加熱至自50℃至200℃之溫度；將自1MPa至5MPa之壓力施加至組合件長達自0.1秒鐘至60分鐘之久；及將基板自燒結薄膜上分離。
基板可為聚合物基板。燒結薄膜可大體上與組件具有相同大小。組件可為LED。
在又一態樣中，本發明提供用於晶粒附著附著之方法，該方法包括以下步驟：將本文所述之燒結薄膜塗覆至基板；將晶粒置於薄膜上以形成組合件；向組合件施加小於5MPa之壓力；及在施加小於40MPa之壓力的情況下，在100℃至400℃之溫度下燒結組合件達0.1秒至60分鐘之久。同一組合件可藉由使用多種提供適度熱以開始及結束燒結的製程及設備，以無壓方式在175℃至400℃的溫度下進一步燒結。
在又一態樣中，本發明提供用於晶粒附著之方法，該方法包括以下步驟：將本文所述之燒結薄膜塗覆在晶圓背側；切割晶圓以形成複數個晶粒；將至少一個晶粒置於基板上以形成組合件；向組合件施加大於1MPa之壓力；及在施加小於40MPa之壓力的情況下，在100℃至400℃之溫度下燒結組合件達0.1秒至60分鐘之久。同一組合件可藉由使用多種提供適度熱以開始及結束燒結的製程及設備，以無壓方式在175℃至400℃的溫度下進一步燒結。
在又一態樣中，本發明提供用於晶圓結合之方法，該方法包括以下步驟：將本文所述之燒結薄膜塗覆在晶圓背側；將又一個相同或不同類型之晶圓置於含有可燒結Ag薄膜之晶圓上以形成組合件；向組合件施加大於0.1MPa之壓力；及在100℃至400℃之溫度下燒結組合件達0.25秒鐘至120分鐘之久。同一組合件可藉由使用多種提供適度熱以開始及結束燒結的製程及設備，以無壓方式在175℃至400℃的溫度下進一步燒結。
在又一態樣中，本發明提供用於晶圓結合之方法，該方法包括以下步驟：將燒結薄膜塗覆在晶圓背側；將又一個相同或不同類型之晶圓置於含有燒結薄膜之晶圓上以形成組合件；向組合件施加小於40MPa之壓力；及在100℃至400℃之溫度下燒結組合件達0.25秒至120分鐘之久。同一組合件可藉由使用多種提供適度熱以開始及結束燒結的製程及設備，以無壓方式在175℃至400℃的溫度下進一步燒結。
在又一態樣中，本發明提供如本文中所描述之金屬粉末或如本文中所描述之燒結漿料或薄膜在選自以下各者之方法中的用途：晶粒附著(例如板上晶片、基板上晶片、散熱器上晶片、夾具上晶片)、晶圓間結合(例如散熱器上晶圓)、反射層印刷、氣密及近乎氣密密封(例 如用於封裝及邊緣密封)、互連線路(例如電路系統、襯墊)之生產，半導體裝置及基板中之通孔充填，及晶片倒裝及晶圓轟擊(bumping)。
在又一態樣中，本發明提供製造燒結接頭之方法，該方法包括以下步驟：在兩個或兩個以上待結合工件的鄰近處，提供如本文中描述之金屬粉末或如本文中描述之燒結漿料或薄膜；及加熱金屬粉末或燒結漿料或薄膜以至少部分地燒結金屬。
有利地，加熱步驟可在大氣壓力下執行。金屬粉末或燒結漿料或薄膜可在低壓下置於工件鄰近處(通常為在1MPa至5MPa壓力下及約175℃至250℃之溫度下長達0.1秒鐘至60秒鐘之久)。
加熱步驟較佳在至少140℃之溫度下執行，該溫度更佳自150℃至350℃，甚至更佳自160℃至300℃。低於140℃之溫度無法導致燒結粉末中之粒子的充足燒結，及/或無法導致藉由蒸發及/或燒盡而充分移除有機物。高於350℃之溫度可能產生對於工件之損害。
在又一態樣中，本發明提供製造燒結漿料之方法，該方法包括以下步驟：根據本文中描述的方法製備金屬粉末；及將金屬粉末與黏合劑、溶劑及視需要流變改質劑及/或有機銀化合物及/或及活化劑及/或過氧化物組合。
將理解，本文中揭示之方法、粉末、漿料及薄膜與先前技術相比具有多種益處。特定而言，利用漿料印刷時，沒有塌陷現象，沒有橋接，印刷沉積物中沒有氣泡，沒有滲出及沒有孔經遮擋。此外，有可能為自80微米至90微米之漿料高度提供平坦的沉積物，沒有圖廓外延區(Dog-ear)及沒有起伏。因此，包括黏合劑(例如樹脂)之漿料的 益處包括：
無壓燒結
標準SMT線路中之處理能力
平坦及均勻的表面拓撲學
晶粒抗剪強度大於15MPa
沒有界面斷裂模式
室溫穩定性為最短1個月
熱循環：可接受的接頭強度高達1000個週期(-40℃至125℃，停 留10分鐘)。
噴針及噴口可施配
薄膜形狀因子
除上文提及之益處之外，含有機銀化合物之漿料具有一些其他益處，該等益處列於下方：
高晶粒抗剪強度(15MPa至45MPa)
高熱傳導率(大於100W/mK)
可針式轉印
優良之高熱特性
本發明現將藉由參考以下非限制性圖式進行描述，在該等圖式中：
第1圖顯示Ag1-3類型之Ag粒子的粒度分佈(particle size distribution；PSD)圖表。
第2圖顯示Ag1-3類型之Ag粒子的掃描電子顯微照片(scanning electron micrograph；SEM)。
第3圖顯示Ag1-3類型之Ag粒子的熱解重量分析(thermogravimetric analysis；TGA)圖表。
第4圖顯示Ag1-3類型之Ag粒子的差分掃描熱量測定法(differential scanning calorimetric；DSC)圖表。
第5圖顯示Cu1-5類型之Cu粒子的粒度分佈(particle size distribution；PSD)圖表。
第6圖顯示Cu1-5類型之Cu粒子掃描電子顯微照片(scanning electron micrographs；SEM)。
第7圖顯示AgCu1-5類型之Ag塗佈Cu粒子的粒度分佈(particle size distribution；PSD)圖表。
第8圖顯示AgCu1-5類型之Ag塗佈銀粒子的掃描電子顯微照片(scanning electron micrographs；SEM)。
本發明現將藉由參考以下非限制性實例進行描述。
實例1-Ag微米粒子類型1
在化學製程中，藉由攪拌將420g硝酸銀溶於2100g去離子水中。將420g二甲基甲醯胺(DMF)添加至溶液中，並連續攪拌。向此溶液中同時添加兩個單獨溶液，亦即(1)325g三乙胺與460g甲醛的混合物，及(2)30g氫氧化鈉在200g去離子水中之溶液。隨後立即添加新製備的油酸鈉溶液(將6.3g油酸添加至1.3g氫氧化鈉於200g水中之溶液中)。使攪拌混合物達1小時之久，然後過濾粉末，用水及丙酮沖洗粉末，直至濾液之pH值呈中性。然後，在烘箱中在70℃下烘乾粉末達8小時之久。
此後執行機械製程，在該製程中，在含250g甲苯與4g油 酸的溶液中攪拌200g乾燥粉末達30分鐘之久，然後藉由使用磨碎球磨機、使用粒徑為0.1mm之氧化鋯珠機械地處理該粉末達4.5小時之久。隨後用丙酮沖洗所得產物，以分離珠粒與粉末，並允許珠粒沉降。藉由傾析溶劑，收集粉末。用丙酮沖洗所得產物，移除額外有機物。然後，在烘箱中在70℃下烘乾粉末達8小時之久。
實例2及3-Ag微米粒子類型2及3
在化學製程中，藉由攪拌將420g硝酸銀溶於1500g去離子水中。向上述溶液添加89g氫氧化鈉於400g去離子水中之溶液，從而產生褐色非均質溶液。向該反應混合物中添加126g水合肼於1890g去離子水中之溶液中，隨後再添加新製備之油酸鈉溶液(將6.3g油酸添加至1.3g氫氧化鈉於210g水中之溶液中)。允許攪拌混合物達1小時之久，然後過濾粉末，用水及丙酮沖洗粉末，直至濾液之pH值呈中性。然後，在烘箱中在70℃下烘乾粉末達8小時之久。
隨後執行機械製程，該製程中，在200g甲苯與4g油酸的溶液中攪拌200g乾燥粉末達30分鐘之久，然後藉由使用磨碎球磨機、使用粒徑為0.1mm之氧化鋯珠機械地處理(a)達4.5小時之久，以產生Ag微米粒子類型2，或(b)達9小時，以產生Ag微米粒子類型3。隨後用丙酮沖洗所得產物，以分離珠粒與粉末，並允許珠粒沉降。藉由傾析溶劑，收集粉末。用丙酮沖洗以去除額外有機物。然後，在烘箱中在70℃下烘乾粉末達8小時之久。
實例4-具有刻面之銅微米粒子類型Cu 2之製備
將1140g三水合硝酸銅(II)溶於含6.9g表面活性劑(DAXAD)的1550g去離子水中，攪拌30分鐘。將該反應混合物置於具有電子溫度計之熱板上。將1380mL濃度為30%之氨溶液添加至上 述溶液中，直至pH值變為8。攪拌該溶液達10分鐘。溫度設定在70℃。在獲得所需溫度之後，以每分鐘30mL之速率添加1970mL濃度為60%之水合肼，且連續攪拌30分鐘。為減少起泡，不時地添加最少量之乙醇。溫度設定在85℃。在獲得該溫度之後，攪拌該溶液達2.5小時。允許粉末沉降，且藉由傾析上清液來收集粉末。用水及丙酮沖洗粉末，在50℃下在成型氣體(90%-95%氮；5%-10%氫)環境中烘乾達8小時。
實例5-7-薄片狀銅微米粒子類型Cu 3-5之製備
將500g細碎銅粉(Cu 1)添加至300g蒸餾水、25g PEG 400及2.25g三伸乙四胺之溶液中。充分混合，得到均質混合物，然後全部移送至具有粒徑為1.6mm之2.2Kg氧化鋯珠之磨碎球磨機中。持續碾磨達(a)45分鐘，以獲得Cu 3；(b)1小時，以獲得Cu 4；及(c)2小時，以獲得Cu 5。在機械製程之後，使混合物隨著珠粒放入燒杯，使用水分離銅薄片與珠粒。用水及丙酮混合物沖洗直至藍色上清液消失，然後用丙酮沖洗。在50℃下在成型氣體(90%-95%氮：5%-10%氫)環境中烘乾銅薄片，以避免銅薄片氧化。
實例8-球形AgCu：類型AgCu 1
Ag塗佈製程：將1Kg細碎商售銅粉(Cu 1)添加至2Kg去離子水中。向上述溶液中添加50g PEG-400，然後充分攪拌混合物達10分鐘，以獲得均質形式。將上述漿液添加至3L三伸乙四胺中，期間持續不斷地攪拌。攪拌此混合物達1.5小時。將10Kg冰水添加至反應器。然後再攪拌15分鐘。將220g硝酸銀及660g檸檬酸溶於5Kg蒸餾水中，然後將該溶液緩緩(在約20分鐘內)添加至上述反應混合物中，期間持續不斷地攪拌。在添加完成後，進一步攪拌反應混合物達1小時。 在反應完成之後，允許混合物沉降，傾析藍色上清液溶液，用水沖洗沉降之AgCu，直至上清液完全呈無色，隨後用丙酮沖洗。在烘箱中在50℃至60℃下烘乾粉末。
有機塗佈製程：塗佈溶液由140g異硬脂酸溶於2600g甲苯中組成。將乾燥的AgCu粉末添加至此溶液中，攪拌達1小時。允許該混合物沉降；傾倒出海綠色上清液溶液。用丙酮沖洗AgCu粉末，直至獲得無色溶液。在烘箱中在50℃至60℃下烘乾粉末。
實例9-具有刻面之AgCu：類型AgCu 2
Ag塗佈製程：將100g具有刻面之銅粉(Cu 2)置入350g水中，充分攪拌以達到適當散佈。向上述溶液中添加350g水、22.75g硫酸銨與20mL氫氧化銨之混合物，然後攪拌達15分鐘。傾析上清液，然後立即添加5g PEG、350g水與350g三乙基四胺六乙酸之混合物添加，攪拌達1.5小時。向上述溶液中添加1Kg水，然後逐滴添加26.4g AgNO3與22g檸檬酸於250g水中之溶液，攪拌達1小時。用丙酮沖洗粉末，直至獲得無色溶液。在烘箱中在50℃至60℃下烘乾粉末。
有機塗佈製程：使粉末進入500mL燒杯，向燒杯中添加300g濃度為5%之異硬脂酸溶液(285g甲苯與15g異硬脂酸)，然後攪拌達1小時。用丙酮沖洗塗層粉末，然後在50℃至60℃下烘乾。
實例10-12-薄片狀AgCu：類型AgCu 3-5
Ag及有機塗佈製程：薄片狀銅粒子Cu 3-5用於製備薄片狀AgCu粒子。Ag塗佈及有機塗佈製程與針對球形AgCu 1之描述相同。
藉由使用SEM、PSD、元素分析、BET、敲緊密度及熱分析(TGA及DSC)來表徵實例1-12中之銀、銅及銀塗佈銅微米粒子，及且在表1(Ag微米粒子)、表2(銅微米粒子)及表3(塗佈Ag之銅 微米粒子)中加以匯總。
本發明之金屬粉末、燒結薄膜及燒結漿料之其他應用如下所示：
1.晶圓間之結合層基於可印刷漿料及薄膜，用於垂直LED設 計、薄膜倒裝晶片設計及紅色LED設計。對於在低溫(低於250℃及亦低於200℃)下之晶圓間結合存在顯著需求，在該低溫下，結合層展示結合後之極高溫度特性。在LED晶圓結合之情況下，可例如在薄膜倒裝晶片或垂直薄膜或截頂倒置稜錐LED之情況下實現此目的，在該等情況中，CTE失配及由此產生之應變及缺陷可能降至最低，同時允許利用多種先進材料進行高溫後處理，以增強裝置之光輸出及電效率。此外，高溫及結合層之高熱傳導率及電導率允許進行優良的熱轉印、裝置之高溫操作，及優良的電流擴展，及其他優勢。該種晶圓結合可藉由以下方式完成：所述材料在晶圓背側上之薄膜積層，隨後在標準晶圓接合器或壓機中進行溫度及壓力處理。進行處理之另一手段包括在溫度及壓力條件下在晶圓背側印刷漿料保形層，隨後在標準晶圓接合器或壓機中進行乾燥及結合。該種晶圓結合之其他應用包括功率半導體晶圓、穿矽通孔(Through Silicon Via；TSV)應用、堆疊晶粒應用、MEMS、濃縮光伏打電池及其他應用。低溫燒結賦能高CTE失配堆疊及熱敏材料堆疊、熱電材料及壓電材料之組合。
2.半導體晶粒(或倒裝晶片或結合金屬絲)在多種基板上之附著，該等基板如直接結合銅(Direct Bond Copper；DBC)、直接銅板(Direct Plate Copper；DPC)、金屬核心PCB(Metal Core PCB；MCPCB)、FR4、銅引線框、撓性PCB及基板、銅及鋁散熱裝置、夾具等等。應用包括由多種化合物半導體材料製成的LED晶粒(發光二極體，例如具有橫向、垂直薄膜或倒裝晶片種類之發光二極體)、由矽製成的功率晶粒、濃縮光伏打化合物半導體電池(例如多接頭電池)、用於功率模組中之碳化矽及氮化鎵，及離散裝置、所有類型之微機電感測器(micro-electromechanical sensor；MEMS)裝置、半導體及堆疊晶 粒，及諸如熱電材料及壓電材料之其他應用。
(a)該種半導體或其他晶粒元件之附著可藉由以下方式實現：在基板上印刷，隨後經由晶粒接合器或取放機器放置晶粒，且在回流烘箱帶或烘箱中燒結。該種半導體及晶粒元件之附著亦可經由以下方式實現：施配漿料，隨後如上文所概述放置晶粒及進行燒結，或在由所述材料製成的薄膜之晶粒背側進行薄膜轉印及積層，隨後放置晶粒及釘在基板上，隨後進行燒結。倒裝晶片晶粒可藉由在基板上印刷凸塊、放置晶粒，隨後進行燒結而組裝。低溫燒結賦能高CTE失配堆疊及熱敏材料堆疊之組合。
3.多種類型之半導體封裝(例如底部端接組件，如LGA、QFN、QFP，等等)在多種基板上之附著，該等基板如直接結合銅(Direct Bond Copper；DBC)、直接銅板(Direct Plate Copper；DPC)、金屬核心PCB(Metal Core PCB；MCPCB)、FR4、撓性PCB及基板、銅及鋁散熱裝置、夾具等等。應用包括多種類型之LED封裝(例如陶瓷子座架LED、具有引線框構造之SMD LED，等等)功率模組，及離散裝置、所有類型之微機電感測器(micro-electromechanical sensor；MEMS)封裝、半導體及堆疊晶粒封裝，及其他應用。
(a)該種半導體或其他封裝之附著可藉由以下方式實現：在基板上印刷，隨後經由具有Z軸高度調整及/或壓力能力的標準取放機器放置封裝，且在回流帶式烘箱或箱式烘箱中燒結。低溫燒結賦能高CTE失配堆疊及熱敏材料堆疊之組合。
4.與倒裝晶片互連分別或同時進行之互連線路(電路系統、襯墊，等等)的生產。例如，互連線路之應用包括LED板及光源，其中互連線路可藉由多種印刷(例如模版印刷)或施配或噴射技術而得以應用。在LED應用之情況下，該等互連裝置可充當電導體及熱導體以 承載電子往返於裝置，且將熱載離裝置。此外，該等互連線路可直接以與互連裝置相同的步驟應用，以用於附著倒裝晶片或金屬絲結合裝置。該等互連裝置之另一實例是太陽能電池(基於矽或基於薄膜)，其中處於柵格模式中之互連裝置可用以收集所產生之電子，且亦將一個電池連接至另一個電池。
5.用於LED及光學應用之反射層印刷。所述材料可用以將反射層印刷至基板上，該等基板如直接結合銅(Direct Bond Copper；DBC)、直接銅板(Direct Plate Copper；DPC)、金屬核心PCB(Metal Core PCB；MCPCB)、FR4、撓性PCB及基板、銅及鋁散熱裝置等等，以便為LED及其他光學系統提供光輸出增強，且因此而導致的發光效能增強。該等反射層可經由對所述材料進行模版或絲網印刷、噴射或施配或薄膜積層而形成。
6.在LED、MEMS、OLED及PV應用及一般半導體封裝中用於封裝、邊緣密封等的氣密及近乎氣密密封。對於LED、OLED、MEMS及薄膜PV封裝之氣密密封存在顯著需求，以保護裝置免於濕氣侵入。所述材料在適當應用及燒結時可展現氣密或近乎氣密密封的特性。所述材料可應用於上述裝置製造製程之多個階段中：在晶圓結合時之晶圓級，或在經由薄膜積層及結合進行之封裝製程中，或漿料噴射/施配，隨後進行蓋或玻璃或層狀封蓋之附著及燒結。低溫燒結賦能高CTE失配堆疊及熱敏材料堆疊之組合。
7.ACF替代物。所述材料之凸塊陣列可經由模版印刷、凸塊轉印或高速噴嘴施配而傳遞至基板。該等陣列可用以充當電觸點以在並未明確高度校準之情況下組裝裝置。

Claims (18)

  1. 一種用於製造金屬粉末之方法，該方法包括以下步驟：提供一鹼性金屬鹽溶液；將該鹼性金屬鹽溶液與一還原劑接觸以從該鹼性金屬鹽溶液中沉澱金屬粉末；及從該溶劑中回收該沉澱的金屬粉末。
  2. 如請求項1所述之方法，其中該還原劑包括肼、甲醛及硼氫化物中之一或更多者。
  3. 如請求項1或請求項2所述之方法，進一步包括以下步驟：在使該鹼性金屬鹽溶液與該還原劑接觸之步驟之後，使該鹼性金屬鹽溶液與一封端劑接觸。
  4. 如請求項3所述之方法，其中該封端劑包括一脂肪酸，該脂肪酸較佳為月桂酸、棕櫚酸、硬脂酸、異硬脂酸及油酸中之一或更多者。
  5. 如請求項1所述之方法，進一步包括以下步驟：碾磨該回收之沉澱金屬粉末。
  6. 如請求項5所述之方法，其中藉由使用一球磨機執行該碾磨之步驟。
  7. 如請求項5或請求項6所述之方法，其中在存在一脂肪酸之情況下執行該碾磨之步驟，該脂肪酸較佳為月桂酸、棕櫚酸、硬脂酸、異硬脂酸及油酸中之一或更多者；及/或在存在一聚合物之情況下執行該碾磨，該聚合物較佳為PEG 400；及/或在存在一多胺之情況下執行該碾磨，該多胺較佳為三伸乙四胺。
  8. 如請求項5或請求項6所述之方法，其中執行該碾磨之步驟達至少30分鐘，較佳達至少90分鐘。
  9. 如請求項1所述之方法，其中該金屬包括銀、銅及上述各者中之一或更多者之合金中之一或更多者。
  10. 如請求項1所述之方法，其中：該金屬包括銀；及該還原劑包括肼，該方法進一步包括以下步驟：在使該鹼性金屬鹽溶液與該還原劑接觸之步驟之後，使該鹼性金屬鹽溶液與一油酸封端劑接觸；及在存在一油酸封端劑之情況下，藉由使用一球磨機碾磨該回收之沉澱金屬粉末達至少30分鐘。
  11. 如請求項1所述之方法，其中該金屬包括銅，且該方法進一步包括以下步驟：向形成該粉末之該等粒子上塗覆一銀塗層。
  12. 如請求項11所述之方法，其中塗覆該銀塗層之步驟包括以下步驟：從該等銅粒子上蝕刻一氧化層；及藉由使用電鍍而向該等銅粒子塗覆一銀塗層。
  13. 如請求項11或請求項12所述之方法，進一步包括以下步驟：向該等銀塗佈粒子塗覆一脂肪酸塗層。
  14. 一種製造一銅粉之方法，該方法包括以下步驟：提供一銅粉；及在存在一聚合物之情況下藉由使用一球磨機碾磨該銅粉，該聚合物較佳為PEG 400；及/或在存在一多胺之情況下碾磨該銅粉，該多胺較佳為三伸乙四胺。
  15. 一種金屬粉末，根據任一前述請求項所述之方法製造而 成。
  16. 一種金屬粉末，具有：自500nm至10μm之一D50；及大於2g/cm3之一敲緊密度，其中該金屬粉末包括銀、銅及上述各者中之一或更多者之合金中之一或更多者。
  17. 一種燒結漿料，包括：如請求項15或請求項16所述之該金屬粉末；一黏合劑；一溶劑；及視需要，一流變改質劑及/或一有機銀化合物及/或一活化劑及/或一表面活性劑及/或一潤濕劑及/或一過氧化氫或有機過氧化物。
  18. 一種製造一燒結漿料之方法，該方法包括以下步驟：根據請求項1至14中任一項所述之方法製備一金屬粉末；及將該金屬粉末與一黏合劑、一溶劑及視需要，一流變改質劑及/或一有機銀化合物及/或及一活化劑及/或一過氧化物組合。
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