TW202012070A - 用於燒結黏晶及類似應用之奈米銅糊及膜 - Google Patents

用於燒結黏晶及類似應用之奈米銅糊及膜 Download PDF

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TW202012070A
TW202012070A TW108122399A TW108122399A TW202012070A TW 202012070 A TW202012070 A TW 202012070A TW 108122399 A TW108122399 A TW 108122399A TW 108122399 A TW108122399 A TW 108122399A TW 202012070 A TW202012070 A TW 202012070A
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sintered
paste
powder
film
sintered powder
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TW108122399A
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TWI808208B (zh
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夏密克 戈夏爾
雷瑪 恰德蘭
文朵 馬諾哈蘭
秀麗 薩卡
寶瓦 西恩
拉胡 勞特
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美商阿爾發裝配對策公司
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Abstract

一種包含銅粒子的燒結粉末，其中該等粒子至少部分塗佈一覆蓋劑，及該等粒子具有D10大於或等於100奈米及D90小於或等於500奈米。

Description

用於燒結黏晶及類似應用之奈米銅糊及膜
本發明係關於一種燒結粉末、燒結糊及燒結膜。
燒結接點對焊接接點提供一替換。形成燒結接點的典型方法包括將一經常呈粉餅形式的金屬粉放置在二個欲連接的工件間，然後燒結該金屬粉。該金屬原子所產生的原子擴散會於該二個工件間形成黏合。
在電子工業中，已經使用金屬奈米粉來形成燒結接點，且其視為無鉛焊料的有用代用品。在奈米材料與相應塊材間之行為差異已認為係由於奈米材料具有較高的表面積對體積比率。就機械、電及熱的信賴度來說，當與傳統的焊料糊比較時，使用奈米金屬粒子在二種材料間形成導電接點具有許多益處。
包括銀奈米粒子的燒結粉末係已知。藉由銀奈米粒子之原子擴散所形成的燒結接點可在溫度明顯低於塊材的熔化溫度下進行加工，且其亦可使用於高溫應用。但是，對有效使用於大部分電子應用來說，此燒結粉末的燒結溫度仍然太高。
該燒結溫度可藉由在燒結期間施加外部壓力而降低。已經顯示出銀糊之壓力輔助式低溫燒結係作為黏晶方法的 回焊之可實行選擇。已經顯示出施加高壓能明顯降低燒結溫度，且可以相對較快的速率在數分鐘內造成燒結接點形成並達成黏晶想要的性質。但是，大外部壓力使得該方法之自動化困難。再者，施加大外部壓力可對該工件造成損傷。
銀金屬由於其優良的導電及導熱度已長期使用在電子工業中用於黏晶應用。但是，銀的高成本限制了銀廣泛應用在許多領域中。再者，銀亦面對在相當高溫度及濕度下會離子漂移的問題，此係所關心的其它主要原因。
與銀比較，銅係更便宜的材料且亦擁有非常高的導電度(僅少於Ag有6%)。除了其較低成本外，銅亦不存在有離子漂移的問題，此提供了銅超過銀的優勢。但是，奈米銅粒子氧化的固有趨勢仍然係主要問題。
已經有一些報導提出多種方法，此些闡明奈米銅粒子若被塗佈上適合的保護層時可在周圍條件下抵擋氧化。將這些奈米銅粒子使用在用於黏晶應用之導電黏晶糊中的用途仍然未被非常大量地開發。因此，在電子市場中，對可提供與奈米銀幾乎相同的利益但是成本更低之銅黏晶糊有龐大需求。
WO 2014/068299係關於一種包含具有平均最長直徑少於10微米的微粒之燒結粉末，及針對一種具有雙峰粒子尺寸分佈之銀奈米粒子。WO 2015/155542係關於一種低壓燒結粉末及亦針對一種具有雙峰粒子尺寸分佈之銀奈米粒子。因為二者文件皆利用銀，其會發生離子漂移的問題。
本發明試圖處理與先述技藝相關的至少某些問題或至少向那裏提供一種商業可接受的替代解決方案。
在第一態樣中，本發明提供一種包含銅粒子的燒結粉末，其中：該等粒子至少部分塗佈一覆蓋劑；及該等粒子具有D10大於或等於100奈米及D90小於或等於2000奈米。
除非有明確相反地指示出，否則如於本文中所定義的每個態樣或具體實例可與任何其它態樣或具體實例結合。特別是，任何指示出為較佳或優良的特徵可與任何其它指示出為較佳或優良的特徵結合。
本案發明人已驚人地發現該燒結粉末具有優良的燒結性質，同時亦比習知的含銅燒結粉末不易於氧化。
有利的是，就燒結能力、導熱度、導電性及最後接點的適宜機械性質而論，該燒結粉末提供等於或類似於奈米銀的利益，但是成本更低。此外，已克服與奈米銀相關的離子漂移問題。
該燒結粉末典型係空氣安定及不黏聚。
再者，該燒結粉末能夠萬用(versatile)連接表面及特別是，萬用連接二或更多個不同飾面的表面，諸如銅對銅、銅對鋁、鋁對銅、鋁對鋁及銅對鎳。該燒結粉末特別合適於黏晶。
如於本文中所使用，用語「燒結粉末」可包括能形成燒結接點的粉末。該燒結接點係藉由放置在二個欲連接的工件間之金屬粒子的原子擴散而形成。用語「燒結粉末」可包括微粒。
該燒結粉末包含銅粒子。該等粒子可包含規則形狀的粒子(諸如例如，球形)及/或不規則形狀的粒子(諸如例如，鬚、板、棒或薄片)。
該銅粒子可呈例如銅金屬或銅合金形式，較佳為銅金屬。
該燒結粉末可包含除了銅粒子外之粒子。但是，在該燒結粉末中的多數粒子係銅粒子，典型來說，該等粒子實質上全部係銅粒子。
該等粒子至少部分塗佈一覆蓋劑。如於本文中所使用，用語「覆蓋劑」可包括一物種，當其存在於該金屬粒子的表面上時會減低該等金屬粒子之黏聚、能夠在該粉末製造期間控制粒子尺寸及減低粒子表面氧化或其它污染。有利的是，使用覆蓋劑可幫助減低該等粒子黏聚。此黏聚係不利，因為其可增加該燒結粉末的燒結溫度。此外，使用覆蓋劑能夠在較低溫度下於工件間形成燒結接點，因此，可幫助減低由曝露至高燒結溫度對工件所造成的損傷。此外，使用覆蓋劑可幫助避免金屬劣化，諸如例如，因金屬曝露至空氣所造成的損傷。
該等粒子典型實質上塗佈該覆蓋劑，更典型為完全塗佈該覆蓋劑。
該等粒子具有D10大於或等於100奈米及D90小於或等於2000奈米。D90描述出該直徑的分佈為90%具有較小的粒子尺寸及10%具有較大的粒子尺寸。D10直徑具有10%較小及90%較大。如在技藝中習知，該直徑與等效球直徑相應，及該分佈與體積分佈相應。該D10及D90可藉由在技藝中已知的合適技術測量，諸如例如，雷射繞射、動態光散射及SEM影像分析。
粒子小於100奈米可更易於氧化。粒子大於2000奈米可能不呈現有利的燒結性質，諸如與塊體比較，好的燒結能力及減低的燒結溫度。此外，該燒結能力呈現適宜的燒結性質，同時能在非惰性大氣諸如空氣下製造、貯存、處理及使用。該D90較佳為小於或等於1000奈米，更佳為小於或等於500奈米，甚至更佳為小於或等於450奈米，仍然甚至更佳為小於或等於400奈米。較低的D90值可改良優良的燒結性質。該D10較佳為大於或等於125奈米，更佳為大於或等於150奈米。較大的D10值可改良對氧化的抗性。較佳的是，該等粒子具有D10大於或等於125奈米及D90小於或等於450奈米，更佳為該等粒子具有D10大於或等於150奈米及D90小於或等於400奈米。
該粒子尺寸分佈典型為單峰態。
較佳的是，該燒結粉末係用於黏晶。該燒結粉末可對使用在黏晶上特別有效。
該覆蓋劑可係無機及/或有機。該有機覆蓋劑的實施例包括聚合物及配位體。較佳的是，該覆蓋劑包含胺及/或羧酸鹽官能基。此覆蓋劑可與該金屬粒子形成弱鍵結。此外，可降低打斷該鍵結所需要的溫度，此可幫助降低燒結溫度。就這一點而言，包含胺官能基的覆蓋劑特別佳。較佳的是，該覆蓋劑包含三乙醇胺；及更佳的是，該覆蓋劑係三乙醇胺。三乙醇胺在減少粒子黏聚及/或氧化而沒有相反地影響該適宜的燒結性質上特別有效。
該燒結粉末較佳為包含最高1重量%的覆蓋劑，更佳為0.1至0.5重量%的覆蓋劑，甚至更佳為0.2至0.4重量% 的覆蓋劑。較低程度的覆蓋劑可造成不利的黏聚或使得該粒子更易於氧化。較高程度的覆蓋劑可造成較高程度的殘餘覆蓋劑存在於使用該覆蓋劑所形成之燒結接點中。此可能會降低該接點的機械性質，特別是晶粒剪切強度。因為該等粒子具有比習知燒結粉末大的粒子尺寸，減低黏聚及/或提供合適的抗氧化性所需要之覆蓋劑量係少於習知燒結粉末。此可改良使用該燒結粉末所形成的燒結接點之機械性質，因為存在於該燒結接點中之殘餘覆蓋劑量將較少。
該燒結粉末可有利地呈粉餅形式。此可使得該燒結粉末較易於放置在該想要的燒結接點所需要之位置。
在進一步態樣中，有提供一種包含如於本文中所描述的燒結粉末之燒結糊。
該燒結糊提供與奈米銀糊幾乎全部相同的益處，但是具有更低的成本。該燒結糊闡明優良的導熱及導電性。例如，該燒結糊典型具有導電性至少1.0×106西門子/公尺，更典型為至少1.5×106西門子/公尺，例如，約1.8×106西門子/公尺。有利的是，該糊係在周圍室條件下安定。
該糊係可印刷及/或可配給及/或可噴射及/或可針轉移(pin transferable)及/或可網版印刷。該糊可具有特別適宜於配給的黏性及流動特徵，此意謂著該糊可使用作為焊料的一對一置換。
該燒結糊可進一步包含例如黏合劑、活化劑、分散劑及有機溶劑之一或多種。這些組分典型經選擇，以便其能夠在溫度低於該燒結粉末之標的燒結溫度下自該糊移除(例如，藉由蒸發及/或燃燒掉)。此可幫助促進接近該金屬粒子之完全燒 結。當有機材料在燒結期間餘留於該接點中時，可能發生該金屬粒子的不適當燒結。此可能產生弱的燒結接點。
較佳的是，該糊包含70至90重量%的燒結粉末，更佳為70至87重量%。此可允許適宜的燒結性質與處理性質之有利的組合。
該糊較佳為包含1至5重量%的黏合劑。該黏合劑可提供將該糊黏結在一起，以便其較易於處理及準確地放置在想要的燒結接點的位置。
該黏合劑較佳為包含聚合物。合適於使用作為黏合劑的聚合物係在技藝中已知。較佳的是，該黏合劑包含環氧基基底的樹脂，更佳為環氧基甲基丙烯酸酯胺基甲酸酯。特別是，該環氧基基底的樹脂可有效將該糊黏結在一起，以便該糊較易於處理及可較易於準確地放置在想要的燒結接點的位置。再者，該環氧樹脂之使用可在燒結前造成形成較強的接點，此意謂著並不需要於燒結前將欲連結的工件合在一起。當該覆蓋劑包含胺官能基時，使用環氧樹脂特別有利。於此情況中，該胺作用為形成交聯結構的硬化劑。此可在燒結前產生特別強的接點。
該糊較佳為包含0.5至3重量%的活化劑，更佳為1至3重量%。可加入活化劑以自欲印刷的表面移除可能存在的任何金屬氧化物，及/或移除可能存在於該燒結粉末中之任何氧化物。可使用芳基或烷基羧酸作為活化劑。較佳的是，該活化劑包含二羧酸，更佳為丙二酸。
該糊較佳為包含0.5至2重量%的分散劑。該分散劑典型包含一界面活性劑。可將分散劑/界面活性劑加入至該燒 結糊以幫助該燒結粉末分散在該燒結糊中。特別合適之可商業購得的分散劑/界面活性劑之實施例有BYK 163。
該糊較佳包含10至15重量%的有機溶劑。該有機溶劑較佳包含單萜醇(例如，萜品醇)及/或二醇(例如，三甘醇)及/或二醇醚。在將該金屬粒子分散於該糊中時，單醇及/或二醇可在該有機組分的基質中產生均勻的金屬粒子分佈上特別有效且具有減低的簇團聚集及/或黏聚。使用單萜醇及/或二醇可提供增加該燒結糊之流動能力及印刷機能力。該有機溶劑較佳為包含萜品醇作為特別有效的溶劑。
該燒結糊可包含進一步物種。例如，可加入流變改質劑以控制該糊的黏性。合適的流變改質劑之實施例包括但不限於Thixcin R及Crayvallac Super。
在特別佳的具體實例中，該糊包含：70至90重量%的燒結粉末；1至3重量%的活化劑；0.5至2重量%的分散劑；10至15重量%的有機溶劑；及選擇性，1至5重量%的黏合劑。
該糊較佳為可印刷及/或可配給及/或可噴射及/或可針轉移及/或可網版印刷。
在進一步態樣中，本發明提供一種包含於本文中所描述的燒結糊之燒結膜。
在一個較佳具體實例中，該膜係預施加至晶圓。在另一個較佳具體實例中，該膜係在一聚合物基材上。在另一個較佳具體實例中，該膜係自立式(free standing)。
在進一步態樣中，本發明提供一種製造燒結粉末的方法，該方法包含：提供包含銅離子及覆蓋劑的溶液；讓該溶液與還原劑接觸以提供該燒結粉末；及回收該燒結粉末。
該方法產生包含銅粒子的燒結粉末。該方法產生包含銅粒子且具有適宜地窄的粒子尺寸分佈之燒結粉末，典型具有D10大於或等於100奈米及D90小於或等於500奈米。與習知的銅燒結粉末比較，所產生的燒結粉末可特別合適於使用作為燒結粉末，例如用於黏晶，可呈現改良的抗氧化性。所產生燒結粉末可係於本文中所描述的燒結粉末。本發明之下列態樣的方法之優點及較佳特徵係同等地施用至此態樣。
在進一步態樣中，本發明提供一種製造於本文中所描述的燒結粉末之方法，其包含：提供包含銅離子及覆蓋劑的溶液；讓該溶液與還原劑接觸以提供該燒結粉末；及回收該燒結粉末。
因為該燒結能力呈現抗氧化性，該方法可有利地在非惰性大氣諸如例如空氣中進行。
該銅離子及覆蓋劑可相繼或同時地加入至該溶劑以形成該溶液。典型地，該覆蓋劑係在強烈攪拌下逐滴加入至該銅離子溶液。此可保證該覆蓋劑係精細地分散在該溶液中，因此幫助將粒子尺寸控制在想要的範圍中。
該溶液較佳為水溶液，諸如例如，去礦質水。
該溶液及還原劑典型藉由混合及攪拌而接觸。在此步驟期間，該燒結粉末的粒子係自該溶液沉澱出。
在該溶液中的銅離子：覆蓋劑莫耳比率較佳為1：1至10：1，更佳為2：1至7：1，甚至更佳為4：1至6：1。此比率可幫助提供該粒子呈想要的尺寸。例如，較高的覆蓋劑量可造成形成不合意的小粒子，然而較低的覆蓋劑量可造成形成不合意的大粒子。
在該溶液中的銅離子較佳為以銅鹽形式提供。該銅鹽較佳包含醋酸銅。醋酸銅係特別合適的鹽及具低成本。
該覆蓋劑較佳包含三乙醇胺。
該溶液較佳為具有pH大於7。例如，可藉由將氫氧離子加入至該溶液達成pH大於7，例如，藉由加入NaOH及/或KOH。pH大於7可提供更適宜於還原的條件，因此增加產率。再者，pH大於7可避免任何銅粒子與酸的不利反應。
該還原劑對銅離子的莫耳比率較佳為大於1：1。過量的還原劑可增加產率。
該還原劑較佳為包含肼(例如，肼水合物)。肼係特別合適的還原劑，及其在製造具需要的尺寸範圍內之粒子時特別有效。
該包含銅離子及覆蓋劑的溶液較佳為與該還原劑接觸5至30小時，較佳為10至20小時。較短的時間可造成產率減低及/或形成不適宜的小粒子。較長的時間可造成形成不適宜的大粒子。
該回收典型包含下列之一或多種：自所產生溶液(「母液」)傾出燒結粉末、洗滌該燒結粉末及乾燥該燒結粉 末。該洗滌可以例如以水接著丙酮來進行。該乾燥可例如在溫度超過30℃下進行，例如，35℃。
該方法較佳為在非惰性大氣諸如空氣中進行。此係與習知的銅燒結粉末製備方法形成對比，該習知的方法易受氧化影響。在非惰性大氣下進行該方法可減少該方法的複雜性及/或成本。
在進一步態樣中，本發明提供一種製造於本文中所描述的燒結糊之方法，該方法包含：提供於本文中所描述的燒結粉末；及混合該燒結粉末與有機溶劑及選擇性的活化劑、分散劑、覆蓋劑及黏合劑之一或多種。
較佳的是，該方法進一步包含例如以三輥式軋機來碾軋該燒結糊。此可改良該糊的均勻性。在該混合步驟期間，於碾軋前加入額外的覆蓋劑可減低在碾軋期間發生黏聚。
較佳的是，該方法進一步包含將該燒結糊澆鑄成膜。合適的澆鑄方法係在技藝中已知。
在進一步態樣中，本發明提供一種在二或更多個工件間形成接點的方法，該方法包含：提供二或更多個欲連接的工件；在該二或更多個工件附近提供於本文中所描述的燒結粉末及/或於本文中所描述的燒結糊及/或於本文中所描述的燒結膜；乾燥該燒結粉末及/或燒結糊及/或燒結膜；及加熱該燒結粉末及/或燒結糊及/或燒結膜以至少部分燒結該金屬。
在較佳具體實例中，該二或更多個工件包含晶粒及基材。
該乾燥步驟係在該加熱步驟前進行。該乾燥步驟能夠讓隨後在燒結期間施加壓力而沒有位移(「擠出」)該粉末、糊或膜。該乾燥步驟亦對「無壓燒結」有利，於此其提供防止在該加熱步驟期間有任何位移。
該乾燥較佳為在溫度30至100℃下進行，更佳為40至80℃，甚至更佳為50至70℃。該乾燥較佳為進行1至60分鐘，更佳為5至40分鐘，甚至更佳為10至30分鐘。
該至少部分燒結造成接點形成。該加熱典型造成該金屬實質上燒結，更典型為該金屬完全燒結。該加熱較佳為在溫度140至300℃下進行，更佳為180至280℃。該加熱較佳為進行最長15分鐘，更佳為1至8分鐘，甚至更佳為2至6分鐘。較低的溫度及較短的加熱時間可造成不完全燒結，因此造成最後接點有不利的機械及/或熱及/或電性質。較高的溫度及較長的加熱時間可對工件造成損傷。
該加熱可在壓力或沒有壓力(所謂的「無壓燒結」)下進行。當在壓力下進行加熱時，較佳為於加熱期間施加2至18MPa的壓力，更佳為3至15MPa，甚至更佳為5至13MPa，仍然甚至更佳為8至12MPa。較高的壓力可有利地由於經改善的粒子間接觸而需要較低的加熱溫度及/或造成形成具有更適宜的機械及/或熱及/或電性質之接點。但是，若壓力太高時，則有損傷工件的風險。
在較佳具體實例中： 將該燒結糊被網版印刷到一或多個欲連接的工件上而形成網版印刷圖案；及將焊料施加至該網版印刷圖案；選擇性，在施加該焊料前藉由無電鍍鎳浸金(ENIG)技術塗佈該網版印刷圖案。
合適於網版印刷的技術係在技藝中已知。該網版印刷可使用例如網狀篩(例如，篩孔尺寸70)進行。該網版印刷係在將該燒結糊提供至該二或更多個工件附近之步驟期間進行。該焊料可使用例如標準焊料糊施加。由於該燒結糊，該焊接可具有適宜的敷開及焊接特徵。該焊接及ENIG典型在乾燥步驟及加熱步驟後進行。
選擇性在施加焊料前藉由無電鍍鎳浸金(ENIG)技術來塗佈該網版印刷圖案。合適的無電鍍鎳浸金技術係在技藝中已知。無電鍍鎳浸金(ENIG)係一種使用於印刷電路板的表面電鍍型式。其由覆蓋浸金薄層的無電鍍鎳組成，其中該薄層係保護該鎳不氧化。ENIG具有一些更超過習知(及較便宜)表面電鍍諸如HASL(焊料)的優點，包括優良的表面平面性(對具有大BGA封裝的PCBs特別有幫助)、好的抗氧化性及用於未經處理的接觸表面諸如薄膜開關及接觸點之可用性。
該二或更多個工件較佳包含半導體或其它晶粒元件與基材。該基材可包含例如DBC(直接覆銅(Direct Bond Copper))、DPC(直接鍍銅(Direct Plate Copper))、MCPCB(金屬核心PCBs(Metal Core PCBs))、FR4、銅引線架、可撓PCBs。
在典型的方法中，將該粉末及/或糊及/或膜被放置或被網版印刷在該基材上，然後乾燥。然後，接著此，典型為經由例如黏晶機或取放機來放置晶粒。然後，典型使用例如Carver加壓機進行加熱。之後，然後典型進行焊接及選擇性ENIG。
在進一步態樣中，本發明提供於本文中所描述的燒結粉末及/或於本文中所描述的燒結糊及/或於本文中所描述的膜之用途，其係使用選自於下列之方法中：黏晶、晶圓對晶圓黏合、氣密式及近氣密式密封、包含由燒結粉末與黏合劑在底層上形成膜之燒結膜、互連線之配給及製造。
在進一步態樣中，本發明提供一種使用於本文中所描述的燒結粉末、及/或於本文中所描述的燒結糊、及/或於本文中所描述的燒結膜所形成之燒結接點。
該燒結接點可具有相較於使用習知燒結粉末所形成之接點之高剪切強度。
本發明將與下列非為限制的圖式相關聯進行說明，其中：圖1顯示出根據本發明之合成的銅粉之FESEM影像(×10,000)。
圖2顯示出根據本發明之合成的銅粉之FESEM影像(×30,000)。
圖3顯示出在5及10MPa壓力下的晶粒剪切之盒狀圖及後硬化的效應。
圖4顯示出於燒結溫度250℃下，在不同壓力下的晶粒剪切之盒狀圖。
圖5顯示出在使用壓力燒結，於250℃及不同時間及壓力燒結條件下黏晶後之SEM截面影像。
圖6顯示出在使用壓力燒結，於200℃及不同時間及壓力燒結條件下黏晶後之SEM截面影像。
現在，本發明將與下列非為限制的實施例相關聯進行說明。
在下列實施例中所使用之材料係如下購買：醋酸銅(II)單水合物係自Fischer Scientific購買；三乙醇胺(85%)係自ViVochem購買；氫氧化鈉、肼(85%LR)、甲醇及丙酮係自SDFCL購買；及去礦質水係自Spectrum Chemicals購買。
在下列實施例中所使用的設備如下：晶粒剪切係在Dage4000 PXY上進行；膜係在Pro-cast薄帶鑄造器(tape caster)(TC-71LC)上澆鑄；及燒結係使用Carver加壓機(3891CEB.4NE1001)進行。
實施例1：奈米銅粒子之合成
將醋酸銅(100克)溶解在去礦物質水(1500毫升)中。對醋酸銅之水溶液，伴隨著強烈攪拌逐滴加入三乙醇胺(20克)，然後攪拌該溶液30分鐘。然後，加入氫氧化鉀/氫氧化鈉(20克氫氧化鉀在100毫升水中)以使該溶液變鹼性(pH>7)，及允許攪拌該溶液另30分鐘。經由滴入漏斗對此混合物加入過量肼水合物溶液(150毫升)。因為該反應非常放熱及放出泡騰，應該採取預防措施。因此，在水浴中進行該反應，其中該反應溫度係維持於20至25℃間。然後，攪拌所產生溶液6小時。該反應混合物的顏色自藍綠色改變至橙色，然後最後至淡棕色。然 後，允許靜置該溶液1小時，以便允許該合成的銅粒子沈澱在底部，然後傾出所產生的溶液(母液)。然後，以過量水完全清洗該合成的粉末以移除不想要的反應物。然後，以丙酮清洗該經清洗的粉末。在35℃下乾燥該粉末。
然後，藉由粉末掃描式電子顯微鏡(SEM)及粉末X射線繞射(XRD)來標出該合成的粉末之特徵。藉由影像分析，該D10係大於或等於100奈米及該D90係小於或等於500奈米。圖1及2顯示出該合成的粒子之場發射掃描式電子顯微鏡(FESEM)影像。FESEM顯示出該等粒子具有可區別的形狀及具有範圍200至400奈米的窄粒子尺寸分佈。不意欲由理論界限，已考慮到與習知燒結粉末中的奈米銅粒子比較，較大尺寸的奈米銅粒子使得其對氧化更具抗性。
該粒子尺寸亦使用粒子尺寸分析器(PSA)測定，其顯示出在150至350奈米間有非常一致及窄的尺寸分佈範圍，此與SEM符合。
實施例2：奈米銅糊之製備 實施例2.1：
使用高速混合器(1000rpm，1分鐘)，將上述的合成的奈米銅粉(24克)以環氧基甲基丙烯酸酯胺基甲酸酯(0.279克)進行分散。對該分散物加入三乙醇胺(85%，0.279克)、BYK 163(0.558克)、丙二酸(1.116克)及萜品醇(1.674克)，及使用高速混合器以1000rpm摻合1分鐘。然後，使用EXAKT三輥式軋機徹底碾軋所得的混合物。然後，將所收集的均勻可印刷糊貯存在標準溫度及壓力(STP)下。
實施例2.2：
使用高速軌道式混合器，將上述的合成的奈米銅粉(15克)以環氧基甲基丙烯酸酯胺基甲酸酯(0.70克)進行分散。對該分散物加入BYK(0.70克)。將丙二酸的甲醇溶液(1.41克丙二酸在1.41克甲醇中)加入至該分散物，接著加入萜品醇(1.5克)。然後，將該混合物放到高速軌道混合物中及以三輥式軋機碾軋數分鐘以提供均勻的糊。
實施例2.3：
使用高速軌道式混合器，將上述的合成的奈米銅粉(15克)以環氧基甲基丙烯酸酯胺基甲酸酯(0.754克)進行分散。對該分散物加入BYK(0.754克)。將丙二酸(1.51克)加入至該分散物，接著加入萜品醇(2.64克)。然後，將該混合物放到高速軌道混合物中及以三輥式軋機碾軋數分鐘而提供均勻的糊。
實施例2.4：
使用高速軌道式混合器，將上述的合成的奈米銅粉(15克)以環氧基甲基丙烯酸酯胺基甲酸酯(0.754克)進行分散。對該分散物加入BYK(0.754克)。將丙二酸(1.51克)加入至該分散物，接著加入蟻酸(1.511克)及萜品醇(2.64克)。然後，將該混合物放到高速軌道混合物中及以三輥式軋機碾軋數分鐘以提供均勻的糊。
上述的合成的銅糊之導電性係約1.8×106西門子/公尺。
實施例3：膜澆鑄方法
藉由薄帶鑄造器的幫助，將該銅糊澆鑄在聚對[酉+太]酸乙二酯(PET)膜上。該膜的厚度係設定在75微米。讓該銅 糊在100℃下通過該薄帶鑄造器。該膜的澆鑄時間係約25分鐘。該澆鑄膜的厚度係約50至60微米。
實施例4：在晶粒上的膜轉移方法
使用Datacon黏晶機執行在晶粒上膜轉移(DTF)方法。3毫米*3毫米塗金矽晶粒之戳印條件係如下列表1。
Figure 108122399-A0202-12-0018-1
該膜係完全轉移到晶粒側上而無銅膜餘留在PET基材上。然後，在下列表2之條件下，使用Tresky黏晶機將該塗佈銅的Si晶粒黏附至塗金/銅之直接覆銅(DBC)。
Figure 108122399-A0202-12-0018-2
自上述條件獲得的晶粒剪切係顯示在圖3中。在圖3中，該後硬化條件係在溫度300℃下30分鐘。該在5MPa燒結壓力下含及不含後硬化的晶粒剪切各別約14MPa及約20MPa。該在10MPa燒結壓力下含及不含後硬化的晶粒剪切各別約24MPa及約30MPa。可明確地看見，當該媒劑係在300℃下後硬化30分鐘時，接點強度有激烈增加。失效模式係整體失效而與使用條件無關。
實施例5：使用Carver加壓機之2英吋鍍金矽晶圓的晶圓積層
將Carver加壓機的二個平台保持在175℃。使用5至10MPa壓力進行矽晶圓之積層。使用矽橡膠作為該積層的緩衝效用。該積層的停留時間係約3分鐘。該膜的戳印部分顯示出 並無膜餘留在該PET薄片上。然後，將該經積層的晶圓裝配在UV膠帶上及使用切塊機進行切塊。
然後，使用Carver加壓機將經切塊的3毫米*3毫米晶粒黏附至塗Au/Cu的DBC。當該燒結壓力係5MPa時，獲致約30至32MPa的接點強度。然而，當該燒結壓力係約10MPa且在250℃下的停留時間係3分鐘時，則獲致40MPa的接點強度。
圖4顯示出在燒結溫度250℃下，於不同壓力下之晶粒剪切的盒狀圖。在圖4中，該燒結條件的第一溫度、壓力及時間各別為250℃、5MPa及3分鐘。該燒結條件的第二溫度、壓力及時間各別為250℃、10MPa及3分鐘。在5MPa及10MPa燒結壓力下的晶粒剪切各別約31MPa及約40MPa。
實施例6：用於自立膜(free standing film)之方法
使用Carver加壓機製得自立式銅膜。在200℃下，以5至10MPa之壓力將該澆鑄膜加壓在矽晶圓上。該停留時間係約2分鐘。該銅膜取得該矽晶圓之形狀及不擴散進矽中，其依次造成該膜與該聚合物基材分離而產生厚度約30至40微米的自立膜。當穿越該膜連接9伏特電池時，該奈米銅膜之導電度造成LED發光。該膜的電阻率實測係2×10-8歐姆．公尺。
實施例7：使用壓力燒結之奈米銅糊黏晶
可藉由將該奈米銅糊印刷到諸如直接覆銅(DBC)、直接鍍銅(DPC)、金屬核心印刷電路板(MCPCB)、FR4、銅引線架、可撓PCBs之基材上，接著在60℃下加熱該經印刷的基材20分鐘來乾燥該經印刷的區域以達成該半導體或其它晶粒元件之黏附。然後，該方法接著經由黏晶機或取放機來放置晶粒，及在Carver加壓機中使用壓力燒結進行燒結。
在DBC上，使用3毫米*3毫米塗金矽晶粒來評估各別使用5MPa及10MPa的燒結壓力、燒結時間3分鐘及5分鐘及燒結溫度200℃及250℃之燒結的銅接點之接點強度。在放置晶粒後，然後以鋁箔覆蓋整體組合，此將防止該銅氧化。使用厚度0.5毫米的石墨薄片，將其保持在該矽晶粒上以提供緩衝效用。已觀察到當與較高的燒結壓力及溫度比較時，在較低的燒結壓力(5MPa)及溫度(燒結時間3分鐘)下，接點強度較低。
測試不同燒結溫度及壓力在接點強度上的效應。結果總整理在下列表3中。表3顯示出不同燒結溫度及壓力在接點強度上的效應。要注意的是，在較高的燒結溫度及時間下，大部分晶粒碎裂，此顯露出該接點強度太好而無法自該基材剪切晶粒的事實。再者，其亦顯露出在二者界面上有強的銅擴散。
Figure 108122399-A0202-12-0020-3
在界面上的銅擴散亦藉由SEM截面證實，其顯示出奈米銅粒子在該燒結層中有非常好的緻密度及該奈米粒子在二者界面上的優良擴散造成整體破損。可明確地看見，奈米銅粒子在10MPa下的擴散及緻密度比5MPa燒結壓力者更好許多。 此可在圖5及6的SEM截面中看見。在圖5中，上二列的截面影像顯示出界面比較；上列係晶粒-銅層界面及中間列係銅層-基材界面。底列的截面影像顯示出該銅層之微結構比較。每行的截面影像例示出不同的時間及壓力燒結條件設定。在第一及第二行中及在第三及第四行中的燒結壓力各別係5MPa及10MPa。在第一及第三行中及在第二及第四行中的燒結時間各別係3及5分鐘。在圖6中，上二列的截面影像顯示出界面比較；上列係晶粒-銅層界面及中間列係銅層-基材界面。底列的截面影像顯示出銅層之微結構比較。每行的截面影像例示出不同的時間及壓力燒結條件設定。在第一行中及在第二及第三行中的燒結壓力各別為5MPa及10MPa。在第二行中及在第一及第三行中的燒結時間各別係3及5分鐘。
此半導體及晶粒元件亦可藉由下列達成黏附：DTF及在自該材料製得的晶粒背部上積層，接著放置該晶粒及使用壓力進行燒結。
該晶圓積層的主要優點為不用網版印刷，就機械及人力而論，此係增加的優點。然後，使用切塊機來單粒化(singulate)該經切塊的塗銅矽晶圓及使用Carver加壓機在10及5MPa壓力下3分鐘而黏附至DBC。已觀察到該晶粒剪切各別為約30至40MPa。
已觀察到在10MPa壓力下，大部分矽晶粒碎裂，此再次證明該晶粒對該基材的優良黏結強度。不由理論界限，已考慮到隨著燒結壓力增加，該等奈米粒子漸漸彼此接觸，其依次增加該等奈米粒子之接觸點，而產生較好的粒子融合以提供優良的接點強度。
實施例8：奈米銅糊在陶瓷、FR4及PET基材上之黏附力
測試該奈米銅糊在陶瓷、FR4及PET上的黏附力。使用DEK印刷機將該糊印刷在多種基材上，然後於氮氣下，在1700℃的箱式烤箱中硬化30分鐘。然後，藉由典型的刻痕-膠帶測試方法來測試該印刷。對陶瓷及FR4之黏附力係分類為5B，然而對PET的黏附力係分類為4B。
實施例9：網版印刷及焊接
該合成的奈米銅糊亦具有被網版印刷的能力。使用網狀篩對該糊進行網版印刷。使用篩孔尺寸70的篩網在DEK印刷機上製得設計圖案。
然後，對該經網版印刷的奈米銅圖案進行無電鍍鎳浸金(ENIG)塗佈，接著以標準焊料糊進行焊接。該焊接顯示出非常好的敷開，但是在某些位置處看見晶片間焊球(mid chip solder balls)。
再者，已經探索藉由將該合成的奈米銅糊印刷於裸FR4試樣上來焊接在銅印刷上之可能性。使用標準焊料糊進行該在奈米銅上的焊接。在該銅印刷上沒有ENIG塗層的焊接亦顯示出好的敷開及好的焊接特徵。
已經提供前述詳細描述作為說明及闡明，且其不意欲限制所附加的申請專利範圍之範圍。將由一般技藝人士明瞭在本文目前所闡明的較佳具體實例中之許多變化，且其係保持在所附加的申請專利範圍及其同等物之範圍內。

Claims (46)

  1. 一種包含銅粒子的燒結粉末，其中：該等粒子至少部分塗佈覆蓋劑(capping agent)；及該等粒子之D10大於或等於100奈米及D90小於或等於2000奈米。
  2. 如請求項1之燒結粉末，其係用於黏晶。
  3. 如請求項1或2之燒結粉末，其中該覆蓋劑包含三乙醇胺。
  4. 如任何前述請求項之燒結粉末，其包含最高1重量%的覆蓋劑，較佳為0.1至0.5重量%的覆蓋劑，更佳為0.2至0.4重量%的覆蓋劑。
  5. 如任何前述請求項之燒結粉末，其中該等粒子之D90小於或等於1000奈米，較佳為小於或等於500奈米，更佳為小於或等於450奈米。
  6. 如任何前述請求項之燒結粉末，其中該等粒子之D10大於或等於125奈米及D90小於或等於450奈米。
  7. 如任何前述請求項之燒結粉末，其中該等粒子之D10大於或等於150奈米及D90小於或等於400奈米。
  8. 如任何前述請求項之燒結粉末，其係呈粉餅(powder compact)形式。
  9. 一種燒結糊，其包含如任何前述請求項之燒結粉末。
  10. 如請求項9之燒結糊，其中該糊包含70至90重量%的該燒結粉末。
  11. 如請求項9或10之燒結糊，其中該糊包含1至5重量%的黏合劑。
  12. 如請求項9至11之任一項的燒結糊，其中該黏合劑包含環氧基甲基丙烯酸酯胺基甲酸酯。
  13. 如請求項9至12之任一項的燒結糊，其中該糊包含0.5至3重量%的活化劑，較佳為1至3重量%。
  14. 如請求項13之燒結糊，其中該活化劑包含二羧酸。
  15. 如請求項14之燒結糊，其中該二羧酸包含丙二酸。
  16. 如請求項9至15之任一項的燒結糊，其中該糊包含0.5至2重量%的分散劑。
  17. 如請求項16之燒結糊，其中該分散劑包含界面活性劑。
  18. 如請求項9至17之任一項的燒結糊，其中該糊包含10至15重量%的有機溶劑。
  19. 如請求項18之燒結糊，其中該有機溶劑包含萜品醇。
  20. 如請求項9至19之任一項的燒結糊，其中該糊包含：70至90重量%的該燒結粉末；1至3重量%的活化劑；0.5至2重量%的分散劑；10至15重量%的有機溶劑；及選擇性，1至5重量%的黏合劑。
  21. 如請求項9至20之任一項的燒結糊，其中該糊係可印刷及/或可配給及/或可噴射及/或可針轉移(pin transferable)及/或可網版印刷。
  22. 一種燒結膜，其包含如請求項9至21之任一項的燒結糊。
  23. 如請求項22之燒結膜，其中該膜係預施加至晶圓。
  24. 如請求項22之燒結膜，其中該膜係在一聚合物基材上。
  25. 如請求項22之燒結膜，其中該膜係自立式(free standing)。
  26. 一種製造燒結粉末的方法，該燒結粉末較佳為如請求項1至8之任一項的燒結粉末，該方法包含：提供包含銅離子及覆蓋劑的溶液；讓該溶液與一還原劑接觸以提供該燒結粉末；及回收該燒結粉末。
  27. 如請求項26之方法，其中在該溶液中之銅離子：覆蓋劑的莫耳比率係1：1至10：1，較佳為2：1至7：1，更佳為4：1至6：1。
  28. 如請求項26或27之方法，其中在該溶液中的銅離子係以銅鹽形式提供，且該銅鹽包含醋酸銅。
  29. 如請求項26至28之任一項的方法，其中該覆蓋劑包含三乙醇胺。
  30. 如請求項26至29之任一項的方法，其中該溶液之pH大於7。
  31. 如請求項26至30之任一項的方法，其中該還原劑對銅離子的莫耳比率係大於1：1。
  32. 如請求項26至31之任一項的方法，其中該還原劑包含肼。
  33. 如請求項26至32之任一項的方法，其中該包含銅離子及覆蓋劑的溶液係與該還原劑接觸5至30小時，較佳為10至20小時。
  34. 如請求項26至33之任一項的方法，其中該回收包含下列一者以上：自所產生的溶液傾析出該燒結粉末、洗滌該燒結粉末及乾燥該燒結粉末。
  35. 如請求項26至34之任一項的方法，其中該方法係在非惰性大氣中，較佳為在空氣中進行。
  36. 一種製造如請求項9至21之任一項的燒結糊之方法，該方法包含：提供如請求項1至8之任一項的燒結粉末；及混合該燒結粉末與有機溶劑及選擇性的活化劑、分散劑、覆蓋劑及黏合劑之一者以上。
  37. 如請求項36之方法，其更包含碾軋該燒結糊。
  38. 如請求項36或37之方法，其更包含將該燒結糊澆鑄(casting)成膜。
  39. 一種在二個以上工件間形成接點之方法，該方法包含：提供二個以上欲連接的工件；在該二個以上工件附近，提供如請求項1至8之任一項的燒結粉末及/或如請求項9至21之任一項的燒結糊及/或如請求項22至25之任一項的燒結膜；乾燥該燒結粉末及/或燒結糊及/或燒結膜；及加熱該燒結粉末及/或燒結糊及/或燒結膜，以至少部分燒結金屬。
  40. 如請求項39之方法，其中該二個以上工件包含晶粒及基材。
  41. 如請求項39或40之方法，其中該乾燥係在溫度30至100℃下進行，較佳為40至80℃，更佳為50至70℃。
  42. 如請求項41之方法，其中該乾燥係進行1至60分鐘，較佳為5至40分鐘，更佳為10至30分鐘。
  43. 如請求項39至42之任一項的方法，其中在該加熱步驟期間施加2至18MPa的壓力，較佳為3至15MPa，更佳為5至13MPa，甚至更佳為8至12MPa。
  44. 如請求項39至43之任一項的方法，其中：將該燒結糊網版印刷到欲連接的一個以上工件之上，以形成一網版印刷圖案；及對該網版印刷圖案施加焊料；選擇性在施加該焊料前，藉由無電鍍鎳浸金(electroless nickel immersion gold,ENIG)技術，塗佈該網版印刷圖案。
  45. 一種如請求項1至8之任一項的燒結粉末、及/或如請求項9至21之任一項的燒結糊、及/或如請求項22至25之任一項的膜之用途，其係使用在選自於下列的方法中：黏晶、晶圓對晶圓黏接、氣密式及近氣密式密封、包含由燒結粉末及黏合劑在底層上形成膜的燒結膜、互連線之配給及製造。
  46. 一種燒結接點，其係使用如請求項1至8之任一項的燒結粉末、及/或如請求項9至21之任一項的燒結糊、及/或如請求項22至25之任一項的燒結膜所形成。
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