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研究生： 饒建中
Chien-Chung Jao
論文名稱： Sn-Cu、Sn-Zn系無鉛銲料應用於微電子構裝技術之研究
Investigations of Lead free Solders of Sn-Cu and Sn-Zn series in Microelectronic Packaging
指導教授： 李嘉平
Chiapyng Lee
顏怡文
Yee-Wen Yen
口試委員: 陳信文
Sinn-wen Chen
高振宏
C.Robert Kao
薛人愷
Ren-Kai Shiue
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2006
畢業學年度： 95
語文別： 中文
論文頁數： 113
中文關鍵詞： 無鉛銲料 、錫銅金相平衡 、銀錫銅金相平衡 、錫鋅銀相平衡 、界面反應
外文關鍵詞： lead-free solder, Sn-Cu-Au phase equilibria, Ag-Sn-Cu-Au phase equilibria, Sn-Zn-Ag phase equilibria, interfacial reaction
相關次數： 點閱：291  下載：7 
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    • 本研究針對Sn-Cu及Sn-Zn系無鉛銲料，以實驗方法探討相平衡及界面反應，以提供電子構裝產業在無鉛銲接時的參考。 Sn-Cu-Au三元系統在200℃相平衡實驗顯示，存在兩連續固溶相，χ ( Au5xCu6(1-x)Sn5)及(Au、Cu)相。Cu於AuSn2及AuSn4的溶解度甚微，但Au在Cu3Sn相中有大的溶解度，近15 at.%。另ㄧ方面，Cu在ζ-Au5Sn相中更有高達28 at.%的溶解度。同時該相圖中具有三個三元化合物。而Sn-Ag-Cu-Au四元系統在200℃固定85 at.% Sn的相平衡中，並未發現四元化合物生成。而有一很大區域的四相區，三個三相區及三個兩相區。在Sn-Ag-Cu合金分別添加Cu、Au或Ni，在240℃，與Cu基材進行液/固反應的實驗結果顯示：合金中添加Cu或Au的反應，於界面皆生Cu6Sn5及Cu3Sn兩介金屬相。總厚度隨反應時間增加與Cu濃度增加而變厚。但金的加入降低了介金屬相的成長速率。合金中添加Ni時，反應偶的界面形態則明顯不同，是微島嶼狀的(Cu,Ni)6Sn5散佈在富錫區內。且厚度明顯較添加Cu、Au所形成層狀之介金屬層為厚。
    在Sn-Zn系銲料方面，Sn-Zn-Ag三元系統在260℃相平衡實驗顯示並未發現三元化合物。Sn在Zn及AgZn3的溶解度非常小，然而Zn在Ag3Sn之溶解度達7 at.%；在Ag4Sn之溶解度高達32 at.%；在Ag之溶解度更高達45 at.%。這些數據對Sn-Zn/Ag相關界面反應，在所生成之介金屬相的鑑別上，提供了必要的資訊。接著，改變Zn濃度，以Sn-Zn/Ag反應偶進行實驗。發現，共晶組成的Sn-9Zn合金與銀基材於260℃反應時，在界面生成ζ-AgZn、γ-Ag5Zn8及ε-AgZn3三Ag-Zn介金屬化合物，而不生成Ag-Sn化合物。若增加合金中鋅含量，反應生成同樣的三層介金屬相，但經相同反應時間，各層厚度皆增加。又若減低合金中鋅的含量：當鋅含量降至3wt%時，銀表面生成相發生改變，生成ζ-AgZn及α-Ag兩介金屬相；若再降低合金中鋅含量至2wt%時，則界面形態產生重大變化，銀基材表面生成Ag-Sn化合物，而AgZn相則隨著反應時間逐漸遠離界面，而可在銲料中發現。進一步探討Sn-9Zn合金中添加Cu對界面反應的影響。實驗發現，Cu的少量加入使得原本十分平整的三層介金屬層ζ-AgZn、γ-Ag5Zn8及ε-AgZn3，變的較鬆散不規則。導致許多的Sn擴散進入Ag-Zn介金屬層。當Cu的添加量達3wt%時，更多的Sn擴散進入Ag-Zn介金屬層，銀基材表面開始生成Ag-Sn化合物，這新生成的化合物，造成了表面能的改變。並使得原緊附於銀表面的Ag-Zn介金屬層，產生整體剝離現象。此一新發現對Sn-Zn/Ag銲接有其重要意義。

    The isothermal section of the Sn-Cu-Au ternary and the isoplethal section of the Sn-Ag-Cu-Au quaternary system at 200℃were experimentally established. In the Sn-Cu-Au ternary system, there existed two continuous solid solution phases. One was the Au5xCu6(1-x)Sn5 phase that had a complete solid solubility between AuSn and Cu6Sn5 phases and was marked as χ phase, and the other was the (Au,Cu) phase. Three ternary IMCs A, B, and C were found at 200℃. Cu atoms could dissolve in the ζ phase in considerable quantities. In the Sn-Ag-Cu-Au quaternary system, no quaternary compound was found. In addition, the isothermal section of the Sn-Zn-Ag ternary system at 260℃was experimentally established. The solubility of Sn in Zn or in AgZn3 phases were small. On the other hand, the maximum solubility of Zn in the α-Ag phase was approximately 45 at.% and that of Zn in the Ag4Sn phase was 32 at.%.
    Three interfacial reaction were investigated in this study. The effect of Cu, Au, and Ag additions on the interfacial reaction between Sn-3ag-0.5Cu Solder and Cu substrate were studied at 240℃. When Cu was added to the Sn-Ag-Cu alloy, two kind of intermetallic compounds (IMCs), Cu6Sn5 and Cu3Sn phases were formed. If Au was added to the Sn-Ag-Cu alloy, the same Cu-Sn IMCs, Cu6Sn5 and Cu3Sn, were formed. However, the thickness of IMC between Sn-Ag-Cu + Au / Cu was thinner than that of IMC between Sn-Ag-Cu / Cu. The addition of Au into Sn-Ag-Cu alloy caused the growth rate of IMC to decrease. If Ni was added to the Sn-Ag-Cu alloy, the morphology changed and took the shape of micro-islands on the interface.
    Three Ag-Zn intermetallic compounds (IMCs), ε-AgZn3, γ-Ag5Zn8, and ζ-AgZn, were formed on the Sn-9Zn/Ag interface at 260℃. While Zn content was decreased in Sn-Zn alloy, microstructures of IMCs changed. If the Zn content was less than 2 wt % in the Sn-Zn alloy, Ag-Sn IMCs were formed on the Ag surface and massive spalling of Ag-Zn IMC layers from the Ag surface. Furthermore, the Effect of Cu added eutectic Sn-9Zn solder reacting with the Ag substrate has been investigated. While Cu was gradually added to the Sn-9Zn alloy, the IMC microstructures became loose and Sn and Cu atoms in the Ag-Zn IMCs increased. If more than 3 wt % of Cu was added to the Sn-9Zn alloy, Ag-Sn IMCs were formed on the Ag surface and massive spalling of Ag-Zn IMC layers from the Ag surface occurred in a short reaction time.

    一、 前言 二、文獻回顧 2-1 相平衡 2-1-1 三元及四元系統相圖 2-1-2 Sn-Cu-Au 三元系統相平衡 2-1-3 Sn-Ag-Cu-Au 四元系統相平衡 2-1-4 Sn-Zn-Ag 三元系統相平衡 2-2 界面反應 2-2-1 銲料合金與基材間之界面反應 2-2-2 Sn-Ag-Cu銲料添加Cu、Au及Ni與Cu基材之界面反應 2-2-3 Sn-9Zn銲料與Ag基材之界面反應 三、實驗方法 3-1相平衡 3-1-1 合金製備 3-1-2 熱處理及分析 3-2界面反應 3-2-1 Sn-Ag-Cu添加Cu、Au、Ni與Cu基材反應 3-2-2 Sn-Zn合金與Ag基材反應 3-2-2 Sn-9Zn合金添加Cu與Ag基材反應 四、結果與討論 4-1 Sn-Cu及Sn-Ag-Cu無鉛銲料 4-1-1 Sn-Cu-Au 三元系統相平衡 4-1-2 Sn-Ag-Cu-Au四元系統相平衡 4-1-3 Sn-3Ag-0.5Cu合金添加Cu、Au、Ni與Cu基材反應 4-2 Sn-Zn系無鉛銲料 4-2-1 Sn-Zn-Ag三元系統相平衡 4-2-2 Sn-Zn合金與Ag基材反應 4-2-3 Sn-9Zn合金添加Cu與Ag基材反應 五、結論 表目錄 Table 4-1 Sn-Cu-Au 四元系統相平衡之合金配製及分析結果 Table 4-2 Sn-Ag-Cu-Au 四元系統相平衡之合金配製及分析結果 Table 4-3 Sn-3Ag-0.5Cu + Au / Cu，240℃，經3小時反應，合金中不同Au添加，IMC及析出物經EPMA組成分析。 Table 4-4 Sn-3Ag-0.5Cu + Ni / Cu，240℃反應，IMC及析出物EPMA分析。 Table 4-5 Sn-Zn-Ag合金配製與平衡相 Table 4-6 不同組成的Sn-Zn合金與Ag反應之生成相 圖目錄 Fig.1-1 封裝技術的變革。 Fig.1-2 半導體封裝技術的演進。 Fig.1-3電子構裝依製造程序幾種不同的層級。 Fig.1-4電子構裝中(a) FC-BGA構造，(b)FC的銲料凸塊結構。 Fig.1-5銲點Cu於表面生成之Sn-Cu介金屬層厚度與Shearing force之關係。 Fig.2-1 A-B-C三元合金系統溫度對組成的相圖示意圖。 Fig.2-2 A-B-C三元合金系統於溫度T1下之等溫橫截面示意圖。 Fig.2-3 XYZ平面為固定組成元素A所得的等值相圖。 Fig.2-4 錫-銅二元平衡相圖。 Fig.2-5 Au-Sn二元平衡相圖。 Fig.2-6 Au-Cu二元平衡相圖。 Fig.2-7 Sn-Au-Cu三元系統於360℃的等溫橫截面圖。 Fig.2-8 Sn-Au-Cu三元系統於190℃的等溫橫截面圖(重新繪製)。 Fig.2-9 Sn-Au-Cu三元系統於170℃的等溫橫截面圖 Fig.2-10 Sn-Ag-Cu三元系統在240℃的等溫橫截面圖。 Fig.2-11 銀-錫-金三元系統在206℃下的等溫橫截面圖。 Fig.2-12 200℃以Pandat計算出的銀-錫-金三元系統等溫相圖。 Fig.2-13 Sn-Ag二元平衡相圖。 Fig.2-14 Sn-Zn二元平衡相圖。 Fig.2-15 Ag-Zn二元平衡相圖。 Fig.2-16 Sn-Zn-Ag三元系統，於380℃之等溫橫截面圖。 Fig.4-1 Sn-Cu-Au三元合金配製圖。 Fig.4-2 Alloy #1(Sn-10at.%Cu-10at.%Au)的(a)BEI微結構圖(b)XRD繞射圖。 Fig.4-3 Alloy #6(Sn-10at.%Cu-35at.%Au)的(a)BEI微結構圖(b)XRD繞射圖。 Fig.4-4 Alloy #21(Sn-40at.%Cu-27at.%Au)的(a)BEI微結構圖(b)XRD繞射圖。 Fig.4-5 Alloy #28(Sn-25at.%Cu-55at.%Au)的(a)BEI微結構圖(b)XRD繞射圖。 Fig.4-6 Alloy #43(Sn-25at.%Cu-26at.% Au)的(a)BEI微結構圖(b)XRD繞射圖。 Fig.4-7 晶格常數a、c對nCu/nCu+nAu作圖。 Fig.4-8 Sn-Cu-Au三元系統在200℃的等溫橫截面圖。 Fig.4-9 Sn-Ag-Cu-Au 四元合金配製組成 Fig.4-10 Alloy #1(Sn-1.00 at.% Cu-11.00 at.% Ag-3.00 at.% Au)的(a)BEI微結構圖，(b) X-ray繞射圖。 Fig.4-11 Alloy #18(Sn-0.75at.%Cu-13.50at.%Ag-0.75at.% Au)的BEI微結構圖。 Fig.4-12 Alloy #22(Sn-10.50at.%Cu-1.00 at.%Ag-3.50at.%Au)的BEI微結構圖。 Fig.4-13 Alloy #23(Sn-1.00at.%Cu-3.00at.%Ag-1.00at.% Au)的BEI微結構圖。 Fig.4-14 Alloy #10(Sn-6.75at.%Cu-0.75at.%Ag-7.50at.%Au)的BEI微結構圖及 X-ray繞射圖。 Fig.4-15 Alloy #15(Sn-0.75 at.% Cu-5.25 at.% Ag-9.00 at.% Au)的BEI微結構圖及 X-ray繞射圖。 Fig.4-16 利用Alloy #16(Sn-6.00 at.% Ag-9.00 at.% Au)標定Sn-15%Ag與Sn-15%Au邊界相區之示意圖。 Fig.4-17 利用Alloy #17(Sn-7.50 at.% Cu-7.50 at.% Ag)標定之示意圖。 Fig.4-18 Sn-Ag-Cu-Au四元系統固定85 at.% Sn在200℃的等質橫截面圖。 Fig.4-19 Sn-3Ag-0.5Cu銲料(a)經3h (b)添加1wt% Cu，經3h (c) 添加5wt% Cu，經 30min (d)添加5wt% Cu，經3h 於240℃反應之OM微結構圖。 Fig.4-20 Sn-3Ag-0.5Cu+Cu / Cu反應偶對反應時間的平方根作圖。 Fig. 4-21 Sn-3Ag-0.5Cu+0.1Au / Cu，240℃反應3小時之 BEI微結構圖。 Fig.4-22 Sn-3Ag-0.5Cu+Au / Cu反應偶，240℃反應。IMC厚度對反 Fig.4-23 Sn-3Ag-0.5Cu與Sn-3Ag-0.5Cu+1wt% Au與Cu，240℃反應之比較。 Fig.4-24 Sn-3Ag-0.5Cu+1wt% Ni / Cu，240℃反應3小時的BEI微結構圖。 Fig.4-25 Sn-3Ag-0.5Cu+5wt% Ni / Cu反應偶240℃，30min反應的微結構圖。 Fig.4-26 Sn-3Ag-0.5Cu+5wt% Ni / Cu反應偶240℃，3小時的微結構圖。 Fig.4-27 Sn-Zn-Ag三元合金配製組成 70 Fig.4-28 合金1 (Sn-75.0at.%Zn-5.0at.%Ag)之BEI微結構圖及XRD圖。 Fig.4-29 合金4 (Sn-52.0at.%Zn-28.0at%Ag)之BEI微結構圖及XRD圖。 Fig.4-30 合金10 (Sn-20.0 at.% Zn-60.0 at.%Ag)之BEI微結構圖。 Fig.4-31 合金11 (Sn-10.0 at.% Zn-70.0 at.%Ag)之BEI微結構圖及XRD圖。 Fig.4-32 合金24 (Sn-25.0 at.% Zn-66.0 at.%Ag) 之BEI微結構圖。 Fig.4-33合金15 (Sn-43.0 at.% Zn-54.6 at.%Ag) 之BEI微結構圖。 Fig.4-34 Sn-Zn-Ag三元系統於260℃等溫橫截面圖。 Fig.4-35 Sn-9wt%Zn/Ag反應偶，260℃，30min反應之BEI微結構圖。 Fig.4-36 Sn-14wt%Zn/Ag，260℃，30min反應之BEI微結構圖。 Fig.4-37 Sn-3wt%Zn/Ag，260℃，經(a)1min、(b)30 min反應之BEI圖。 Fig.4-38 Sn-2.0wt% Zn/Ag，260℃，經(a) 1min，(b) 10min，(c) 30min於界面及經(d) 30min於合金中之BEI微結構圖。 Fig.4-39 Sn-1wt﹪Zn/Ag反應偶260℃反應30min之BEI微結構圖。 Fig.4-40 Sn-9Zn合金與Ag基材在260℃反應(a)30，(b)900，(c)5760 minutes之BEI微結構圖。 Fig.4-41 Sn-9Zn合金添加 (a) 0.5，(b) 1.0，(c) 3.0 wt%Cu與Ag基材於260℃反應10 min之BEI微結構圖。 Fig.4-42 Sn-9Zn+3.0wt%Cu合金與Ag基材在260℃反應(a) 1，(b) 2，(c) 4 min之BEI微結構圖。 Fig.4-43 (a) 不同材質間的附著功(work of adhesion)及(b) 相同材質間 Fig.4-44 Sn-9Zn+3.0wt%Cu與Ag基材於260℃反應，其IMC隨反應

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