TWI701287B - 工程聚合物系電子材料 - Google Patents

工程聚合物系電子材料 Download PDF

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Publication number
TWI701287B
TWI701287B TW105110592A TW105110592A TWI701287B TW I701287 B TWI701287 B TW I701287B TW 105110592 A TW105110592 A TW 105110592A TW 105110592 A TW105110592 A TW 105110592A TW I701287 B TWI701287 B TW I701287B
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Taiwan
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weight
composition
graphene
filler
composition according
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TW105110592A
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TW201700597A (zh
Inventor
凡卡塔吉瑞雅帕瑞馬克里斯納郝許
瑞貝斯摩根娜迪艾薇拉
達斯巴倫
悉達帕哈瑞許漢青納
木克吉蘇塔巴
沙卡蘇利
西恩寶瓦
勞特拉赫爾
潘德賀蘭吉特
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美商阿爾發裝配解決方案公司
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    • H01L24/10—Bump connectors ; Manufacturing methods related thereto
    • H01L24/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
    • H01L24/13—Structure, shape, material or disposition of the bump connectors prior to the connecting process of an individual bump connector
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
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    • B23K35/3613—Polymers, e.g. resins
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    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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    • B23K35/025—Pastes, creams, slurries
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Abstract

一種用於電子組裝製程的組成，組成包含分散於有機介質的填料，其中：有機介質包含聚合物；填料包含一或更多的石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、二維材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子，及組成按組成總重量計包含0.001-40重量%的填料。

Description

工程聚合物系電子材料
本發明係關於聚合物組成，用於製造電子部件和裝置，及用於電子組裝與包裝。
表面安裝技術(SMT)係用於製造電子電路的方法，其中部件裝設或直接放在印刷電路板(PCB)的表面。依此製作的電子裝置稱為表面安裝裝置(SMD)。在電子產業中，SMT大半已取代使用導線將部件裝入電路板孔的穿孔技術建構方法。這兩種技術均可用於同一基板上不適合表面安裝的部件，例如大型變壓器和散熱功率半導體。SMT部件通常比部件穿孔對應物小，因為SMT部件具有較小引線或根本沒有引線。SMT部件可在部件主體上設有短銷或各種類型引線、平面觸點、焊球矩陣(BGA)或終端。
在部件待放處，印刷電路板通常具有平面、通常為錫-鉛、銀或鍍金的無孔銅墊，此稱作焊墊。焊錫膏(黏性熔接劑與焊錫微粒混合物)先利用網印製程施用於具不銹鋼或鎳模板的所有焊墊。亦可利用類似噴墨印刷的噴印機制施用。黏貼後，再將板放到拾放機，其 中板置於傳送帶上。待放在板上的部件通常將輸送到捲繞於捲軸或塑膠管的任一紙/膠帶生產線。一些大型積體電路輸送到無靜電托盤。數值控制拾放機從帶、管或托盤移出零件並放到PCB。板接著輸送到回流焊爐。板先進入預熱區，其中板和所有部件的溫度逐漸均勻上升。板接著進入溫度高到足使焊錫膏的焊錫粒子熔化的區域，以接合部件引線與電路板上墊。熔融焊錫的表面張力有助於讓部件保持原位，若焊墊幾何形狀經恰當設計，則表面張力可自動對準墊上部件。有一些用於回流焊接的技術。其一使用紅外燈；此稱作紅外回流。另一使用熱氣對流。再一越來越熱門的技術係具高沸點的特殊氟碳液體，此採用所謂氣相回流方法。
電子裝置的焊錫接點易遭受熱機械疲勞。此係因為由焊錫接點接合的工件通常具有不同的熱膨脹係數(CTE)。此外，期電子裝置的焊錫接點具有高機械強度和高落下耐震性。故接點通常被稱為「底膠」的材料包覆。底膠通常係有機聚合物與無機填料(例如矽石)複合物。底膠固化前和固化後性質落在材料光譜最極端。期固化前的底膠像水般在最小間隙內(通常小於25微米)自由流動。期固化底膠具有堅硬、類無機性質，同時牢牢接合至無機矽和有機基板。增加填料量可改善底膠機械性質。然此亦會提高組成黏度。故底膠材料(或底膠材料替代物)需在未固化狀態時具低黏度且在固化狀態時增進機械性質。另外，習知底膠材料無法利用標 準SMT回流製程和型材固化。因此，當使用底膠時，需要個別不同處理步驟，以致增加製程複雜度。
在LED晶片結構中，覆晶係成長最快的晶片結構，並漸漸佔有側向結構與垂直結構LED的市場。覆晶LED市佔率可望從2014年的<5%成長到2020年的>20%。另外，在覆晶CSP方面(即2階組裝)也有顯著成長，其中CSP包裝具有本質上和覆晶LED晶粒一樣的底面積，故就相同或增強功率與流明輸出而言，可減少包裝成本和底面積。
至於包裝方面的覆晶LED組裝，越來越傾向使用SAC系焊錫膏來建造覆晶LED晶粒與包裝基板間的覆晶內連線。銀環氧樹脂或燒結金屬材料亦可用於建造覆晶LED晶粒與包裝基板間的覆晶內連線。
組裝包裝基板上的覆晶LED(1階附接)及組裝CSP LED(2階)將面臨重大問題。回流後，若使用免洗焊錫膏，熔接劑通常會殘留在基板上的陽極與陰極焊墊周圍和之間。若未適當完成回流，則可能造成陽極與陰極焊接內連線於操作時短路，特別係在存有濕氣情況下，因高電流通過內連線並施加電壓偏壓至陽極與陰極間所致。若使用銀環氧樹脂或燒結金屬材料來建造覆晶LED晶粒與包裝基板或CSP LED包裝與板間的覆晶內連線也可能出現相同問題。若LED包裝或組裝擬使用常用底膠材料，則需有個別固化步驟使底膠固化(不同於焊接回流步驟)，以致降低產量及提高成本。另外， 使用焊錫膏組裝覆晶LED或CSP LED會造成晶粒或包裝浮動和傾斜。
本發明試圖解決至少一些先前技術相關問題，或為此至少提供商業上可接受的替代解決方案。
本發明提供用於電子組裝製程的組成，組成包含分散於有機介質的填料，其中：有機介質包含聚合物；填料包含一或更多的石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、二維(2D)材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子，及組成按組成總重量計包含0.001-40重量%的填料。
除非另行指明，否則所述實施例的每一態樣可結合任何其他態樣或實施例。特別地，任何稱為較佳或有利的特徵可結合任何其他較佳或有利的特徵。
在此所用「石墨烯」一詞包含單原子面石墨(稱作單層石墨烯)或數層石墨烯或多層石墨烯或石墨烯薄板。
在此所用「2D材料」一詞包含二個維度比例上遠大於第三維度的材料。材料實例為氮化硼、二硫化鉬、二硒化鎢、二硫族化過渡金屬、鎳HITP(2,3,6,7,10,11-六亞胺基聯伸三苯)、單鍺、石墨 烷、磷烯、錫烯、液態矽膠、硼烯、石墨炔、氟化石墨烯和2D合成金屬，例如鈀與銠。
在此所用「氧化石墨烯」一詞包含將氧化石墨分散於鹼性介質所得的分子片。氧化石墨烯包含表面具含氧官能基的石墨烯片。
在此所用「官能化石墨烯」一詞包含表面具一或更多官能基的石墨烯。
在此所用「多面體寡聚半矽氧烷(POSS)」一詞包含具實驗式RSiO1.5的奈米結構，其中R可為氫原子或有機官能基，例如烷基、伸烷基、壓克力基、羥基或環氧化物。POSS可稱作矽石奈米粒子，此由矽石籠核心和附接至籠角的其他有機官能基組成。POSS由有機與無機物質組成，並具有無機矽與氧內部核心和有機成分外層，此可為極性或非極性。半矽氧烷結構可無規則、階梯狀、籠狀或局部籠狀。POSS奈米結構的直徑為1-3奈米(nm)，故可視為現存最小矽石粒子。多面體寡聚半矽氧烷的分子結構如下。
Figure 105110592-A0202-12-0005-1
在此所用「表面安裝技術(SMT)」一詞包含製造電子電路的方法，其中部件裝設或直接置於印刷電路板(PCB)的表面。
在此所用「表面安裝製程」一詞係指利用SMT的製程。
在此所用「可固化」一詞意指所稱物種(即組成或聚合物)能由如電子束、雷射、紫外光(UV)、熱或化學添加劑引起聚合物鏈交聯。
在此所用「電子組裝製程」一詞係指用於製造電子裝置或部件的製程，此亦包括統稱SMT的製程。
在此所用「聚合物」一詞通常係指熱塑性或熱固性聚合物。
本發明人發現，相較於不含填料的組成，本發明組成具有改善機械強度及/或耐熱疲勞性及/或阻障特性。特別地，該組成可展現一或更多的改善機械與熱性質，例如落下耐震性、抗撓曲性、耐熱陡震性、CTE、屈服強度、斷裂韌度、彈性模數、耐熱循環性等。
當組成用於製造電子裝置的方法時，此類特性特別有利，因為該等特性可轉移到裝置。例如，組成可用於取代習知底膠材料，以強化(透過包覆)形成在覆晶與有機電路板間的焊錫接點，此將遭受覆晶與有機印刷電路板的熱膨脹不同所引起的熱機械應變。
組成可用於焊錫膏做為焊錫熔接劑。加熱二工件間的焊錫膏後，可形成焊錫接點，組成可固化及包 覆焊錫接點，藉以強化焊錫接點。或者，組成可用於如導電黏著劑，其中期最終黏著接合具高機械強度及/或耐熱疲勞性。
組成在100%的根領(collar)或填角高度或低於100%的根領或填角高度處可展現有利的機械及/或熱疲勞性。
流動動力及/或聚合物固化動力有利於防止未回流焊錫膏變位及可能傳送，且有利於達成更高Tg和良好熱機械性質。
聚合物可為可固化聚合物。組成可利用標準SMT生產線處理，及利用SMT回流製程和型材固化或硬化。由於不像習知底膠材料，此在電子組裝製程期間不需要個別不同處理步驟，因而特別有利。故相較於使用習知底膠材料的電子組裝製程，使用本發明組成的電子組裝製程更簡化。組成可利用如熱、雷射或UV固化。例如，組成通常利用熱與焊錫膏，在回流爐內固化。採用溫度通常為200℃至300℃，例如尖峰溫度為約245℃。
組成在室溫下呈穩定、容易加工處理且與焊錫膏殘餘物相容。組成通常展現膏狀或凝膠狀稠度。
組成可用於低壓與高壓成型、雙射出成型、灌注和包覆。組成可和印刷及/或沉積焊錫膏一起使用。
組成的應用例如有用於製造系統的標準電子組件，例如手機、電腦、相機、平板電腦和顯示器；半導體包裝；及類似系統組件，例如PV模組和電池。
電子組裝製程實例例如包括晶粒附接、覆晶封裝、包裝載板接合、焊球陣列(BGA)、表面安裝技術(SMT)和LED製造製程。電子組裝製程較佳為表面安裝技術(SMT)製程。
填料分散於有機介質。換言之，有機介質形成連續相，填料包含不連續相。
填料例如為球體、棒、薄板及/或薄片形式。填料可具1nm至25微米(μm)的最大尺寸(或者，填料為球體形式時具最大直徑)，例如1至100nm或1至10nm或0.1至25μm或1至5μm。
組成可為膜形式，例如B-階段膜(即組成部分固化的膜)。膜可預先施用於工件，及利用沖壓形成在工件周圍，例如熱沖壓。
組成特別有益用於覆晶LED附接方法或覆晶CSP(晶片級包裝)LED附接方法。
在覆晶組裝期間施用於基板上時(1階)，組成可強化晶粒附接內連線(焊錫、燒結金屬或甚至AuSn)，進而改善包裝可靠度。強化可改善組裝後的記錄晶粒剪切值。組成亦可在覆晶或CSP包裝載板組裝期間施用(2階)。組成可強化包裝載板接合焊錫內連線，從而提高部件剪切值。
在習知覆晶附接方法中，底膠材料用於強化覆晶組件，以免遭受基板與晶粒間熱膨脹係數(CTE)失配引起的應力。然此方式有許多缺點。首先，組件冷 卻後，焊錫接點便回流，而在焊錫接點中產生應力(出自晶粒與基板間的CTE失配)。回流後，施用底膠材料僅能強化接點，以免在可靠度測試與使用壽命期間遭受出自回流應力與溫度偏離額定值時組裝遭遇的附加應力。此方式無法避免在回流步驟期間形成CTE失配應力。其次，在晶粒附接(或包裝附接)後，施用底膠。底膠通常分配到晶粒-基板組件邊緣周圍。底膠接著利用毛細力環繞焊錫接點，以填入晶粒(或包裝)與基板間的空間。不幸的是，當距外高度(晶粒與基板間的高度)為約50微米或以下時，來自毛細作用的驅動力不足以填入晶粒與基板間的間隙。最後，一旦填入底膠，便把組件放到爐內，使底膠固化，以達成預定焊錫接點強化性質。此額外底膠固化步驟另需佔1-2小時。
使用本發明組成可克服傳統底膠處理缺點。因組成通常係在製作焊錫內連線前施用，故晶粒(或包裝)與基板間的距外高度並無限制。距外高度25微米(或以下)的組件很容易強化。其次，由於組成係在焊接回流步驟時固化(通常在回流爐內)，因此不需額外固化步驟。此可提高組裝產量及降低製程成本。最後，因在組裝冷卻前，組成已固化並鎖定在凸塊之間或周圍的組件，故回流後，將抵消首先在焊錫接點周圍產生的CTE失配應力。
形成焊錫接點後，本發明組成將在焊錫接點之間或周圍固化成低應力熱固性塑膠。後續回流期間， 可保持晶粒向下及有效鎖定焊錫形狀。此能使具焊錫接點的組件歷經多次回流，而不會改變接合線厚度或包裝傾斜或浮動。組成能使用傳統SAC系合金用於晶粒附接應用，此需多次回流，又無焊錫接點重熔相關的產率損失。
隨著覆晶與CSP LED變得越來越小，P/N墊間的間隙亦縮減至70-100微米。在習知製程中，回流後，若未適當清潔焊錫膏殘餘物，則會在高溫、高濕度和反向偏壓下進行可靠度測試期間造成漏電。有時清潔小於50微米的距外高度並不實際。回流前，在焊墊間施用本發明組成可消除反向偏壓測試期間的漏電。因此，可替LED製造商帶來顯著的可靠度改善，又不需任何附外清潔步驟。
隨著覆晶與CSP LED變得越來越小，因回流期間晶粒(包裝)傾斜、浮動及旋轉，導致利用正規焊錫膏變得越來越具挑戰性。當焊錫於回流期間熔化時，表面張力將抬起(及搬移)晶粒(或包裝)，該等輕量部件不足以讓晶粒保持原位。回流前施用於焊墊時，本發明組成可提供黏性，以抵消熔融焊錫的側向表面張力。組成可確保此抵消力剛好可保證部件錨接至板，又不危及焊錫潤濕晶粒及製作接點的能力。
組成按組成總重量計包含0.001-40重量%的填料。較佳地，組成按組成總重量計包含0.01-10重量%的填料，更佳按組成總重量計為0.02-5重量%的填 料，再佳按組成總重量計為0.03-4重量%的填料，又更佳按組成總重量計為0.04-1重量%的填料，另再佳按組成總重量計為0.04-0.8重量%的填料，又再佳按組成總重量計為0.05-0.4重量%的填料。在一替代較佳實施例中，組成按組成總重量計包含30-40重量%的填料，較佳為33-37重量%的填料。此組成展現極佳流變性質。在另一替代較佳實施例中，組成按組成總重量計包含0.1-4重量%的填料。組成按組成總重量計可包含至少0.01重量%的填料，較佳為至少0.02重量%的填料，更佳為至少0.03重量%的填料，再佳為至少0.04重量%的填料，又再佳為至少0.05重量%的填料。組成按組成總重量計可包含20重量%或以下的填料，較佳為10重量%或以下的填料，更佳為5重量%或以下的填料，再佳為4重量%或以下的填料，又更佳為1重量%或以下的填料，另再佳為0.8重量%或以下的填料，又再佳為0.4重量%或以下的填料。存有填料可提供改善機械及/或熱疲勞性。大量填料可提高固化前組成的黏度。低黏度組成更容易施用於具小尺寸特徵結構的電子裝置和部件。此對表面安裝技術製造方法而言尤其重要。高黏度組成對諸如印刷、銷轉移等應用和用於電子組裝應用的無流動黏著組成較為有利。
組成在固化前的黏度在室溫下通常為12至20帕．秒，更常為約16帕．秒。利用平行板幾何形狀，在10/秒的恆定剪切率下以流變儀測量黏度。未固化組成 的黏度乃夠低，使組成得以噴塗或噴射或分配。如此組成可用於共形塗層及強化整個板或組件。
組成較佳為可固化組成，及/或聚合物較佳為可固化聚合物。
填料較佳包含一或更多的石墨烯、氧化石墨烯、官能化石墨烯、多面體寡聚半矽氧烷和2D材料。聚合物組成一旦固化，此類物種便提供具特別加強機械及/或耐熱疲勞性的組成。特別地，相較於不含填料或含有習知填料的組成，此類物種可提供具提升落下耐震性與衝擊抗彎強度的固化組成。含有此類物種的組成可用作低熱膨脹係數(CTE)黏著劑，用以接合CTE失配的工件。固化組成亦具有高硬度，以用於耐刮應用。
提供此性質只需很少量的填料，例如石墨烯和官能化石墨烯。含有少量此類物種的組成可兼具有利的機械及/或熱疲勞性，同時未固化組成可具極低黏度。使用諸如石墨烯及/或官能化石墨烯等填料可改善所得組成的熱穩定性，還可提高組成的玻璃轉換溫度(Tg)，進而提升組成的工作限度。
使用氧化石墨烯可減少能滲透組成的水分，藉以改善密封包裝/組件的氣密性。使用石墨烯及/或官能化石墨烯可用來移除/牽制組成中的自由離子，進而改善最終產品的電性。
石墨烯可為單層、數層或多層石墨烯(MLG)使用石墨烯可加強組成的電及/或熱導率。
多面體寡聚半矽氧烷(POSS)當作建構模塊，此係因為POSS巨單體具獨特結構，且為界限分明的分子聚集體，其中無機似矽石核心被八個有機角落基團圍繞。此視為最小矽酸鹽前驅物，其氧化後將形成矽石。在本發明中，POSS有利地併入組成，以克服傳統複合材料不能分子級分散於材料的缺點。當填料包含POSS時，固化組成具有提升落下耐震性與衝擊抗彎強度。使用POSS可提高材料的熱導率。
填料較佳包含：多面體寡聚半矽氧烷；及一或更多的石墨烯和官能化石墨烯(例如氧化石墨烯)。此可提供具極低黏度的組成和具極佳機械性質的組成。相較於使用僅有等量POSS或石墨烯/官能化石墨烯的組成，黏度通常較低，機械性質通常更好。換言之，結合POSS與石墨烯及/或官能化石墨烯(例如氧化石墨烯)驚人地提供協同作用。使用POSS可減少達成預定性質所需的石墨烯/官能化石墨烯量。
官能化石墨烯有助於控制石墨烯的表面性質，及長時間穩定固體與溶液形式的剝落石墨烯層。比起習知石墨烯，使用官能化石墨烯的優點例如包括改善混合及分散並與聚合物基質相互作用、防止石墨烯層在聚合物基質中重新堆疊，及改善水分與氣體不透性。
填料較佳包含官能化石墨烯，其中官能化石墨烯包含氧化石墨烯。使用氧化石墨烯可提供具極佳機械性質的組成。
當填料包含官能化石墨烯時，官能化石墨烯可由有機及/或無機基官能化，較佳為一或更多的胺基、矽烷及/或鈦酸酯基、環氧基、酯基和多面體寡聚半矽氧烷。使用官能化石墨烯可提供具極佳機械性質的組成。有利地，官能化石墨烯可由橡膠分子及/或熔接官能基官能化。官能化石墨烯可由金屬奈米粒子(最長尺寸為1至500nm的粒子)官能化，例如包含一或更多的銀、銅、金和合金(例如AgCu或AgAu)奈米粒子。使用金屬奈米粒子可加強組成的電及/或熱導率。官能化石墨烯可由金屬氧化物或準金屬氧化物的奈米粒子官能化。金屬氧化物例如為鹼土金屬、過渡金屬或貧金屬的氧化物。使用此類氧化物可加強組成的水分與氣體不透性，及/或加強組成的熱導率。
有利地，石墨烯可由氟官能化，例如氟化石墨、氟化氧化石墨烯或具氟化有機分子附接至sp2基面的氧化石墨烯。此類填料可使組成實質不透水分與氣體。
填料較佳包含官能化石墨烯，官能化石墨烯包含由多面體寡聚半矽氧烷官能化的石墨烯(及/或氧化石墨烯)。使用此類填料可提供具極低黏度的組成和具極佳機械性質的固化組成。
填料可包含氮化硼。不像石墨烯和其他石墨材料，使用氮化硼不會改變組成的顏色。
聚合物較佳包含環氧樹脂，更佳地，環氧樹脂包含不同官能度環氧樹脂及/或固態雙官能基(例如三 或四)環氧樹脂且通常具高分子量。此類樹脂具有高交聯度，因而可使固化組成具有極佳機械性質。使用固態環氧樹脂可提高組成的固含量。適用本發明的聚合物例如包括雙酚A二縮水甘油醚、雙酚F二縮水甘油醚、對胺基苯酚三縮水甘油醚、二胺基二苯基碸四縮水甘油醚、二胺基二苯基甲烷四縮水甘油醚、二胺基二苯基醚四縮水甘油醚和三(2,3-環氧丙基)異氰尿酸酯。聚合物可為熱塑性塑膠，例如聚烯烴熱塑性塑膠或丙烯酸熱塑性塑膠。當組成為膜形式時，使用熱塑性塑膠係有利的。
在一較佳實施例中，填料包含氧化石墨烯，及組成包含0.1-4重量%的氧化石墨烯。
此組成可提供具極佳機械性值的組成。
在此較佳實施例中，有機介質較佳包含：30-40重量%的有機溶劑，有機溶劑的沸點為至少280℃；5-10重量%的不同官能度環氧樹脂；15-30重量%的固態雙官能基環氧樹脂，較佳具高分子量；3-10重量%的活化劑，包含二羧酸；2-8重量%的催化劑，包含取代芳胺；1-5重量%的催化劑，包含膦(phosphine)系鹽；1-5重量%的液態酸酐型硬化劑；0.1-4重量%的液型應力調節劑；及 0.1-3重量%的黏著促進劑。
較佳地，有機介質進一步包含有機溶劑，且沸點較佳為至少280℃。使用溶劑有助於維持低組成黏度，並有助於提供最終產品穩定性。適用本發明、沸點至少280℃的有機溶劑例如包括丁基卡必醇、二甘醇單己醚和乙二醇醚。
較佳地，有機介質進一步包含活化劑，更佳地，活化劑包含二羧酸。活化劑可自施用組成的表面(例如電路板墊)移除任何氧化層，及提升具組成的焊錫膠的潤濕性能。
較佳地，有機介質進一步包含催化劑。使用催化劑有助於使可固化組成經交聯處理。催化劑較佳包含取代芳胺及/或膦系鹽。此類催化劑具低反應性。由於組成通常只經高溫交聯，故有助於提高組成的室溫穩定性。
較佳地，有機介質進一步包含硬化劑，更佳地，硬化劑包含液態酸酐型硬化劑。存有硬化劑有助於只在高溫下與環氧樹脂交聯反應，藉以提高組成的室溫穩定性。
較佳地，有機介質進一步包含應力調節劑，較佳為液型應力調節劑。使用應力調節劑可用來減低環氧樹脂的脆性。
有機介質較佳進一步包含黏著促進劑。此可用來增加組成與焊錫接點間的接合。
在一較佳實施例中，有機介質包含：30-40重量%的有機溶劑，有機溶劑的沸點為至少280℃；及/或5-10重量%的不同官能度環氧樹脂；及/或15-30重量%的固態雙官能基環氧樹脂，較佳具高分子量；及/或3-10重量%的活化劑，包含二羧酸；及/或2-8重量%的催化劑，包含取代芳胺；及/或1-5重量%的催化劑，包含膦系鹽；及/或1-5重量%的液態酸酐型硬化劑；及/或0.1-4重量%的液型應力調節劑；及/或0.1-3重量%的黏著促進劑。
在一特佳實施例中，有機介質包含：約39重量%的有機溶劑，有機溶劑的沸點為至少280℃；約8重量%的不同官能度環氧樹脂；約29重量%的固態雙官能基環氧樹脂，較佳具高分子量；約9重量%的活化劑，包含二羧酸；約3重量%的催化劑，包含取代芳胺；約4重量%的催化劑，包含膦系鹽；約2重量%的液態酸酐型硬化劑；約4重量%的液型應力調節劑；及約2重量%的黏著促進劑。
組成可利用下列一或更多者施用於裝置：膜轉印、銷轉移、組分浸漬、膏分配、印刷、噴塗、澆鑄 及刮塗。浸漬高度和浸漬時間可改變以達成高達100%的不同根領高度。
利用毛細添加劑，組成可在高溫下流動(例如170℃至280℃)。
藉由改變浸漬高度及/或浸漬時間，可使組成的根領高度變化達100%。例如，根領高度變化可為約30%至高達100%。適於達成不同根領高度的浸漬高度和浸漬時間實例列於下表1：
Figure 105110592-A0202-12-0018-2
在一較佳實施例中，填料包含石墨烯、氧化石墨烯、石墨薄片、石墨烯薄板、還原氧化石墨烯、2D材料或上述二或更多組合物。此可提供具高機械強度及/或高耐熱疲勞性的組成。
組成可包含著色顏料。此可賦予固化組成預定顏色。
在另一態樣中，本發明提供底膠，包含所述可固化組成。
底膠例如為邊緣填膠、角落填膠或邊緣膠合。在一較佳態樣中，底膠可以一或更多步驟施用，其中一或更多步驟較佳包含浸漬及/或分配。
在又一態樣中，本發明提供焊錫熔接劑，包含所述組成。
在再一態樣中，本發明提供單側或兩側強化(DSR)材料，包含所述可固化組成。
在另一態樣中，本發明提供封裝膠，包含所述組成。
在又一態樣中，本發明提供阻障材料，包含所述組成。
在再一態樣中，本發明提供電子材料，包含：焊錫合金；及所述組成。
焊錫合金可以如焊球、粉末、棒或線形式提供。可固化組成至少部分塗覆焊球、棒、線或粉粒。合金例如為無鉛合金，例如SAC合金。
在另一態樣中，本發明提供導電黏著劑，包含：導電粒子；及所述組成。
導電粒子通常包含金屬(例如一或更多的銀、銅和金)、合金(例如無鉛合金，例如SAC合金)及/或塗覆金屬及/或合金的粒子。導電粒子可為膏、棒 及/或球體形式。導電粒子通常具有1nm至40μm的最長尺寸(若為球體，則為直徑)，例如1至500nm。導電粒子分散於聚合物組成。
在又一態樣中，本發明提供非導電黏著劑，包含：非導電粒子；及所述組成。
非導電粒子通常包含金屬或準金屬氧化物、碳化物、氮化物(例如氧化鋁、氮化硼、碳化矽、氮化鋁)。金屬例如為鹼土金屬、過渡金屬或貧金屬。
非導電粒子可為膏、棒及/或球體形式。非導電粒子通常具有1nm至40μm的最長尺寸(若為球體，則為直徑)，例如1至500nm。非導電粒子分散於聚合物組成。
在再一態樣中，本發明提供焊錫膏，包含：焊錫粒子；及所述組成。
焊錫粒子通常包含金屬(例如一或更多的銀、銅和金)、合金(例如無鉛合金，例如SAC合金)及/或塗覆金屬及/或合金的粒子。焊錫粒子可為膏、棒及/或球體形式。焊錫粒子通常具有1nm至40μm的最長尺寸(若為球體，則為直徑)，例如1至500nm。焊錫粒子分散於聚合物組成。
本發明的組成、焊錫熔接劑、電子材料、導電黏著劑、焊錫膏、底膠、(DSR)材料、封裝膠及/或阻障材料可包含無鉛、零鹵素、免洗焊錫膏，例如LUMETTM P39(ALPHA®)。
在另一態樣中，本發明提供被組成至少部分包覆的焊錫接點，組成為所述可固化聚合物組成。焊錫接點通常被可固化聚合物組成實質包覆，更常為被可固化聚合物組成完全包覆。
在又一態樣中，本發明提供形成焊錫接點的方法，方法包含：在二或更多待接合工件間提供所述焊錫膏；及加熱焊錫膏，以形成焊錫接點。
焊錫膏通常加熱達170℃至280℃。
在再一態樣中，本發明提供製造所述組成的方法，方法包含：提供包含聚合物的有機介質；及使填料分散於有機介質，其中：填料包含一或更多的石墨烯、2D材料、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子；及組成按組成總重量計包含0.001-40重量%的填料。
在使填料分散於內前，通常在至多150℃下混合有機介質的組分，更常為50℃至120℃，再常為約90℃，以形成均質混合物。接著一般使用如三軋輥研磨機來研磨有機介質。確認FOG<10微米後，通常即停止研磨製程。使填料分散於有機介質可包含機械摻和。
在另一態樣中，本發明提供所述組成的用途，用於選自下列一方法：電子組裝方法、表面安裝技術(SMT)方法、晶粒附接方法、回流焊接方法、電路板製造方法和太陽能電池製造方法。
在又一態樣中，本發明提供所述組成的用途，用於電子包裝、覆晶封裝、LED組裝及氣密密封。
在再一態樣中，本發明提供石墨烯及/或官能化石墨烯的用途，用於提高組成的流動性。
在另一態樣中，本發明提供組成，包含分散於有機介質的填料，有機介質包含可固化聚合物，其中：填料包含一或更多的石墨烯、2D材料、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子，及組成按組成總重量計包含0.001-40重量%的填料。
組成例如可用作焊錫熔接劑、或用於導電黏著劑、或用作底膠材料、或用於製造電子裝置、或用於強化焊錫接點、或用作單側或兩側強化(DSR)材料、 或用作封裝膠、或用作黏著劑、或用作阻障材料(例如防止進入如焊錫接點的材料)。
在又一態樣中，本發明提供組成，用於表面安裝製程，組成包含分散於有機介質的填料，其中：有機介質包含聚合物；填料包含一或更多的石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、2D材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子；及組成按聚合物組成總重量計包含0.001-40重量%的填料。
在再一態樣中，本發明提供填料的用途，用於提供組成且組成具有12至20帕．秒的黏度和下列一或更多者：改善機械強度、改善耐熱疲勞性和改善阻障特性，填料包含一或更多的石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、2D材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子。
在另一態樣中，本發明提供所述組成的用途，用於電子組裝應用，例如印刷、銷轉移，且無流動黏著組成，組成的黏度為大於20帕．秒。如上所述，此類應用受惠於高黏度。較高黏度例如可藉由增加填料量提供。
在又一態樣中，本發明提供填料的用途，用於控制組成的熱膨脹係數(CTE)，填料包含一或更多的石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、2D材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子。控制CTE可加強組成的熱疲勞壽命。
本發明現將參照以下非限定圖式敘述，其中：第1圖係根據本發明，一些組成的衝擊抗彎測試結果作圖。
第2圖係根據本發明，一些組成的落下耐震測試結果作圖。
本發明現將描述以下相關非限定實例。
實例1
利用修改的Hummers方法，從天然片狀石墨製備氧化石墨。邊攪拌，邊將市售石墨粉末和10克硝酸鈉加至500毫升濃(98%)硫酸，然後保持在冰浴中。15分鐘後，接著慢慢加入10克石墨粉末(300目)並攪拌10分鐘，以得均質混合物。非常緩慢小心地加入67克過錳酸鉀，同時在冰浴中攪拌整個反應混合物。約30分鐘後，把整個反應混合物轉移到設為約40℃的熱板上。接著攪拌約2.5小時，直到反應混合物顏色變成淡 紅色。然後在室溫下使之冷卻，計約30分鐘。隨後，非常緩慢地加入500毫升去離子水，同時攪拌。攪拌10-15分鐘後，將1公升溫去離子水、然後為100毫升、30體積%的過氧化氫加入反應混合物，並攪拌約5分鐘。以4000rpm離心分離最終產物，計8分鐘，接著在相同離心條件下，用去離子水徹底慎密洗滌。重複此步驟近20次，以清除所有未反應化學品、副產品，及使pH接近約7。然後用丙酮洗滌3-4次，及存放在設為65℃的烘箱內，以完全乾燥。如此可得固體形式且備好供進一步使用的氧化石墨粉末。
接著製備有機介質，包含：a)高沸點有機溶劑39重量%，b)不同官能度環氧樹脂8重量%，c)具高分子量與雙官能基的固態環氧樹脂29重量%，d)做為活化劑的二羧酸9重量%，e)做為催化劑的取代芳胺3重量%，f)做為催化劑的膦系鹽4重量%，g)液態酸酐型硬化劑/催化劑2重量%，h)液型應力調節劑4重量%，i)黏著促進劑2重量%。
依所需比率混合上述所有物種(a)-(i)，及加熱達90℃，直到獲得均質混合物。接著使用三輥軋研磨機處理混合物。確認FOG<10微米後，停止研磨製程。 接著利用機械摻和，使氧化石墨粉墨分散於有機介質，以提供包含0.1-4重量%的氧化石墨烯的可固化組成。
熱循環測試：
將組成與焊錫粒子混合，以形成焊錫膏。亦使用上述組成、但無填料情況下製備焊錫膏(比較實例)。利用SMT方法，焊錫膏用於在印刷電路板上形成焊錫接點。
依下列程序進行熱循環測試。
裝備：
●Espec熱循環腔室(空氣-空氣)TSA-101S。
●Agilent 34980A資料記錄器。
測試條件：
●根據IPC 9701-A標準測試。
●-40℃(10分鐘)至+125℃(10分鐘)，計1000次循環。
失效定義：
●按照IPC 9701-A：輕微阻抗增加20%(在最多5次連續讀取掃描內)。
失效分析：
●經240、500、750、1000次循環後的截面和顯微分析。
結果列於下表2。
Figure 105110592-A0202-12-0027-3
由此可知，相較於不含填料的組成，本發明組成具有改善的耐熱循環特性。
衝擊抗彎測試：
依下列程序進行衝擊抗彎測試。
測試條件：
●連接測試載具至資料記錄器。
●使用固定板撓曲為1.2毫米(mm)。
●進行測試直至第一次失效
●部件上的衝擊撞擊點：部件角落。
●衝擊撞擊銷形狀：圓形(10mmØ)。
測試載具：
●表面光度：EniG。
●50×50mm，0.8mm厚。
●部件：BGA84。
失效定義：
●電阻增加200歐姆(Ω)。
結果繪於第1圖。由圖可知，相較於比較實例(左邊與中間)，其中組成不含任何填料，實例1的組成(右邊)具有較大衝擊抗彎性。
落下耐震測試：
依下列程序進行落下耐震測試。
裝備：
●Lansmont HC18陡震測試器。
●Lansmont TP4。
●AnaTech Event偵測器。
測試條件：
●依循JEDEC標準：JESD22-B111“Board Level Drop Test Method of Components for Handheld Electronic Products”。
●使用操作條件B(1500Gs，0.5毫秒脈衝，半正弦曲線)。
實例1的落下耐震性優於不含填料的比較實例或習知填料。落下耐震測試結果繪於第2圖(菱形：本發明；方形/圓形：參考實例)。
以上詳細敘述僅為舉例說明，而無意限定後附申請專利範圍的範圍。一般技術人士當可從本發明明白所述較佳實施例的許多變化，且仍落在後附申請專利範圍的範圍和均等物內。

Claims (15)

  1. 一種用於電子組裝製程的組成，該組成包含分散於有機介質中的填料，其中：該有機介質包含：30-40重量%之沸點為至少280℃的有機溶劑；5-10重量%的不同官能度環氧樹脂；15-30重量%的固態雙官能基環氧樹脂；3-10重量%之包含二羧酸的的活化劑；2-8重量%之包含經取代的芳胺的催化劑；1-5重量%之包含膦系鹽(phosphine-based salt)的催化劑；1-5重量%的液態酸酐型硬化劑；0.1-4重量%的液型應力調節劑；及0.1-3重量%的黏著促進劑；該填料包含下列之一或更多者：石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷(polyhedral oligomeric silsesquioxane)、石墨、2D材料、氧化鋁、氧化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子；其中該2D材料包含二硫化鉬、二硒化鎢、二硫族化過渡金屬、鎳HITP(2,3,6,7,10,11-六亞胺基聯伸三苯)、單鍺(germanane)、磷烯、錫烯(stanene)、液態矽膠(silicine)、硼烯、石墨炔、或包含鈀或銠的2D合成金屬；及該組成按該組成總重量計包含0.03-4.0重量%的該填料。
  2. 如請求項1所述之組成，按該組成總重量計包含0.04-1重量%的該填料。
  3. 如請求項1所述之組成，按該組成總重量計包含0.05-0.4重量%的該填料。
  4. 如請求項1所述之組成，其中該填料包含下列之一或更多者：石墨烯、氧化石墨烯、官能化石墨烯和多面體寡聚半矽氧烷。
  5. 如請求項4所述之組成，其中該填料包含：多面體寡聚半矽氧烷；及下列之一或更多者：石墨烯和官能化石墨烯。
  6. 如請求項4所述之組成，其中該填料包含官能化石墨烯，且該官能化石墨烯包含下列一或更多者：胺基、矽烷及/或鈦酸酯基、環氧基、酯基和多面體寡聚半矽氧烷。
  7. 如請求項1所述之組成，其中該聚合物包含一環氧樹脂，該環氧樹脂包含不同官能度環氧樹脂及/或具高分子量的固態雙官能基環氧樹脂。
  8. 如請求項1所述之組成，其中該有機介質包含：約39重量%之沸點為至少280℃的有機溶劑；約8重量%的不同官能度環氧樹脂；約29重量%的高分子量固態雙官能基環氧樹脂；約9重量%之包含二羧酸的活化劑；約3重量%之包含經取代的芳胺的催化劑；約4重量%之包含膦系鹽的催化劑；約2重量%的液態酸酐型硬化劑；約4重量%的液型應力調節劑；及約2重量%的黏著促進劑。
  9. 如請求項1所述之組成，其中利用毛細添加劑，該組成能在高溫下流動。
  10. 如請求項1所述之組成，其中藉由改變浸漬高度及/或浸漬時間，可使該組成的根領高度(collar height)變化最高達100%。
  11. 如請求項1所述之組成，其中該組成更包含著色顏料。
  12. 如請求項1所述之組成，其中該組成具有12至20帕．秒的黏度。
  13. 如請求項1所述之組成，其中該填料控制該組成的熱膨脹係數(CTE)。
  14. 一種底膠組成物，包含分散於有機介質中的填料，其中：該有機介質包含：30-40重量%之沸點為至少280℃的有機溶劑；5-10重量%的不同官能度環氧樹脂；15-30重量%的固態雙官能基環氧樹脂；3-10重量%之包含二羧酸的的活化劑；2-8重量%之包含經取代的芳胺的催化劑；1-5重量%之包含膦系鹽的催化劑；1-5重量%的液態酸酐型硬化劑；0.1-4重量%的液型應力調節劑；及0.1-3重量%的黏著促進劑；該填料包含下列之一或更多者：石墨烯、官能化石墨烯、氧化石墨烯、多面體寡聚半矽氧烷、石墨、2D材料、氧化鋁、氧 化鋅、氮化鋁、氮化硼、銀、奈米纖維、碳纖維、鑽石、奈米碳管、二氧化矽和金屬塗覆粒子；其中該2D材料包含二硫化鉬、二硒化鎢、二硫族化過渡金屬、鎳HITP(2,3,6,7,10,11-六亞胺基聯伸三苯)、單鍺、磷烯、錫烯、液態矽膠、硼烯、石墨炔、或包含鈀或銠的2D合成金屬；及該組成按該組成總重量計包含0.03-4.0重量%的該填料。
  15. 如請求項14所述之底膠組成物，其中該底膠組成物可以一或更多步驟施用，其中該一或更多步驟包含浸漬及/或分配。
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