TW201823512A - 無電鍍法 - Google Patents
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Abstract
使用陽離子聚合物或其類似者提供一種發泡特性比習知調節劑小但黏附性比習知調節劑高的調節劑,及使用所述調節劑的無電鍍法。本發明的進行無電鍍的方法包含以下步驟: (a)使基板與含有由以下通式(1)表示之化合物的組合物接觸:其中R1
及R2
各自獨立地為具有3至10個碳原子的伸烷基; (b)使基板與催化劑組合物接觸;以及(c)使基板與無電鍍組合物接觸。
Description
本發明係關於一種在樹脂基板、特別是印刷線路板上進行無電金屬鍍覆的方法,且更特定言之,關於一種用含有特定化合物之預處理溶液在樹脂基板之表面上形成具有高黏附性的金屬膜的方法。
印刷線路板的各層之間的電連接通常藉由稱為通孔的極小的孔進行。關於在印刷線路板之表面上及在這些通孔之內壁表面中形成導電膜的方法,通常使用以下方法:用含有陽離子聚合物及界面活性劑的預處理溶液(亦稱作調節劑)處理,施加含有鈀及其類似者的催化劑,隨後藉由無電鍍法形成金屬膜。
為了改善樹脂基板與導電膜之間的黏附性,通常在調節劑處理之前,使用主要含有溶劑之處理溶液進行樹脂溶脹製程,隨後使用主要含有過錳酸鹽之處理溶液進行粗糙化製程,隨後進行一系列去污/粗糙化製程,藉由中和製程去除錳。去污/粗糙化製程使得在樹脂表面上形成了細微的不均勻度,從而藉由錨定效應改善了樹脂基板與導電膜之間的黏附性。
然而,在主要藉由錨定效應提供黏附性的方法的情況下,若樹脂基板表面之粗糙度減小,則基板與金屬膜之間的黏附性將降低,且獲得具有高黏附性之鍍膜將變得困難。因此,需要一種即使在具有低粗糙度的樹脂基板之表面上仍具有高黏附性的調節劑來代替習知調節劑,並需要一種使用這種調節劑的無電鍍法。此外,視添加至調節劑中之化合物而定,可能在液體表面上生成氣泡;因此,需要沒有這種發泡特性的調節劑。
日本特許公開專利公開案第2006-77289號揭示一種用於無電鍍的預處理溶液,所述預處理溶液含有在一個分子中具有至少兩個胺基的化合物(特別是乙烯胺(共)聚合物或烯丙胺(共)聚合物)。此外,日本特許公開專利公開案第2010-106337號揭示藉由向含有陽離子聚合物及非離子界面活性劑之調節劑中進一步添加二氟化氫銨來形成具有高黏附性的金屬膜的方法。
因此,本發明之一個目的為使用陽離子聚合物或其類似者提供一種發泡特性比習知調節劑小但黏附性比習知調節劑高的調節劑,及使用所述調節劑的無電鍍法。
本發明人進行了大量研究且發現,向調節劑中添加具有特定伸烷基鏈長的三胺化合物來代替陽離子聚合物能夠產生黏附性比陽離子聚合物高但發泡特性比陽離子聚合物小的調節劑。已基於這些發現完成了本發明。
換言之,本發明係關於一種在基板上進行無電鍍的方法,包括以下步驟: (a)使基板與含有由以下通式(1)表示之化合物的組合物接觸: 化學式1:其中R1
及R2
各自獨立地為具有3至10個碳原子的伸烷基; (b)使基板與催化劑組合物接觸;以及 (c)使基板與無電鍍組合物接觸。
除非另外指明,否則本說明書通篇中所用的縮寫具有以下含義。
g=公克;mg=毫克;℃=攝氏度;min=分鐘;m=公尺;cm=公分;L=公升;mL=毫升;且N=牛頓。所有值之範圍均包含邊界值,且可以任何順序組合。此外,在本說明書中,除非另外說明,否則百分比(%)意指重量%。
在本發明方法中,使用含有由以下通式(1)表示之化合物的組合物:。
組合物亦可以稱為調節劑。在通式(1)中,R1
及R2
各自獨立地為具有3至10個碳原子的伸烷基。伸烷基可以為直鏈或分支鏈,但在本發明中直鏈伸烷基為較佳的。伸烷基鏈較佳地具有3至8個碳原子,更佳3至6個碳原子。特定的通式(1)化合物包含二伸丙基三胺、雙(伸丁基)三胺、雙(伸己基)三胺及其類似者。
本發明人已發現,藉由使用具有含3至10個碳原子之伸烷基鏈的三胺化合物,黏附性特徵性地改善了。雖然這不受理論限制,但是咸信,具有含3至10個碳原子之伸烷基鏈的三胺具有極佳的親水親油平衡,容易吸附在樹脂基板上且同時,容易在後續催化劑施加步驟中與催化劑結合。因此,有可能形成具有高黏附性的金屬膜。此外,雖然常用的陽離子聚合物對樹脂具有高黏附性,但是因為其分子量大,所以認為其容易吸附過度。因此,在樹脂表面與金屬膜之間留下相對較大量的陽離子聚合物,從而降低了黏附性。
調節劑中由通式(1)表示之化合物的含量較佳為0.1至10 g/L,更佳為1至8 g/L,且最佳為2至5 g/L。
本發明中所用的調節劑的特徵之一為能夠形成具有高黏附性的金屬膜,即便其不含界面活性劑。含有陽離子聚合物的調節劑通常含有界面活性劑來提高調節劑成分進入通孔及盲孔的滲透性,且賦予玻璃及樹脂均一的調節作用。然而,視使用條件而定,含有界面活性劑之調節劑可能在液體表面上產生氣泡,從而降低了可加工性。藉由使用由通式(1)表示之化合物,本發明之調節劑即使不含界面活性劑,仍展現比習知調節劑高的黏附性。
除了由通式(1)表示之化合物之外,本發明中所用的調節劑可含有任何組分。舉例而言,其可含有螯合劑作為視情況選用的組分。螯合劑藉由在金屬離子溶解至調節劑中時與金屬離子形成螯合化合物來發揮延長調節劑的使用壽命的作用。較佳螯合劑的實例包含乙醇胺、三乙醇胺、乙二胺四乙酸(ethylenediaminetetraacetic acid,EDTA)、乙二胺n,n'二琥珀酸(ethylenediamine n, n' disuccinic acid,EDDS)以及亞胺基二乙酸(iminodiacetic acid,IDA)。相對於調節劑,所添加的螯合劑的量較佳為0.1至0.2 mol/L。
必要時,本發明中所用的調節劑亦可以含有添加劑作為額外視情況選用的組分,諸如pH調節劑及其類似者。本發明中所用的調節劑較佳含有水作為溶劑。可以使用任何水,諸如去離子水,自來水及其類似者。此外,可以將溶劑與水混合並加以使用,溶劑諸如醇。
樹脂基板可為印刷線路板,且印刷線路板可具有玻璃布/樹脂。樹脂基板可具有稱為通孔的小孔或稱為盲孔的小非通孔。此外,在以高效能半導體封裝板為代表的高密度印刷線路板的情況下,使用功能性絕熱樹脂材料板作為樹脂基板。藉由本發明方法,若基板中存在孔,諸如通孔或其類似者,則鍍層不僅能夠均一地沈積在印刷線路板之表面上,而且能夠均一地沈積在孔之內壁表面上。
樹脂基板的實例包含由以下製成的基板:環氧樹脂、氰酸酯樹脂、雙馬來醯亞胺三嗪樹脂、聚醯胺、ABS、聚苯醚、聚碸、含氟樹脂、聚碳酸酯、聚縮醛、聚苯醚、聚丙烯以及液晶聚合物及其類似者。
使用任何能使調節劑與樹脂基板接觸的方法。舉例而言,可藉由以下進行處理:在基板在必要時經歷所謂的去污或粗糙化製程之後,將其浸沒於調節劑中;或將調節劑噴塗在基板上。在浸沒時,基板可在30至60℃、較佳40至50℃之溫度下,在調節劑中浸沒1至10分鐘,較佳2至6分鐘。
在調節劑與樹脂基板接觸之後,進行催化劑施加步驟以使樹脂基板與催化劑組合物接觸,從而將催化劑吸附至樹脂基板之表面上。然而,在樹脂基板與催化劑組合物接觸之前,亦可視情況進行將樹脂基板浸沒在諸如過硫酸鈉、過硫酸銨、硫酸以及過氧化氫混合溶液之水溶液中的步驟(亦稱作微蝕刻)及用諸如硫酸之酸洗滌樹脂基板之表面的步驟。即使在進行這些步驟之後,本發明中所用的調節劑仍能保持在樹脂基板之表面上及孔之內壁表面上,且在後續催化劑施加步驟中,足夠量的催化劑可被吸附在樹脂基板之表面及孔之內壁表面上。微蝕刻步驟通常可以使用水溶液在20至35℃之溫度下進行0.5至10分鐘,較佳1至3分鐘,且酸洗步驟通常可以在20至35℃,較佳25至30℃之溫度下進行0.5至5分鐘,較佳1至3分鐘。
可使用通常已知的催化劑組合物。催化劑組合物之實例包含鈀-錫膠體溶液、含有金屬離子之組合物及其類似者,金屬離子例如鈀、鉑、銀或銅。舉例而言,可使用CIRCUPOSIT™ ADV 8530催化劑及CIRCUPOSIT™ 6530催化劑(均由羅門哈斯電子材料公司(Rohm and Haas Electronic Materials Co., Ltd.)製造)。在使用CIRCUPOSIT™ ADV 8530催化劑作為催化劑組合物的情況下,舉例而言,將樹脂基板在35至60℃,較佳40至50℃之溫度下在催化劑組合物中浸沒1至10分鐘,較佳3至5分鐘,隨後可以用CIRCUPOSIT™ 6540還原劑進行鈀離子的扣除處理。
可使用通常已知的無電鍍組合物。舉例而言,可使用含有金屬或其混合物的無電鍍組合物,金屬例如銅、鎳、鈷、鐵等。在使用印刷線路板作為樹脂基板時,無電鍍銅通常為較佳的。舉例而言,可使用CIRCUPOSIT™ 6550無電銅、CIRCUPOSIT™ ADV 8550無電銅及CIRCUPOSIT™ 328銅混合濃縮物(全由羅門哈斯電子材料公司製造)。
在下文中,將參考實例更詳細地描述本發明,但本發明不限於這些實例。
在以下實例及比較實例中,藉由SEM觀察來評估鍍層在通孔內壁表面上的沈積。亦根據以下程序評估黏附強度:將經歷了無電鍍的基板之表面在室溫下用去離子水洗滌3分鐘,加熱並乾燥(120℃,30分鐘)。隨後,將待鍍覆材料之表面浸沒在含有硫酸的酸清潔劑中(液體溫度35℃,2分鐘)。之後進行酸洗,並用電解鍍銅MICRO FILL™ EVF進行電解鍍銅處理。所得已鍍覆材料之表面在室溫下用去離子水洗滌3分鐘,隨後加熱並乾燥(180℃,60分鐘)。所得鍍銅膜的膜厚度為20至25 μm,並將此鍍膜切成1 cm的寬度。使用INSTRON™ 5564測試儀,以50毫米/分鐘之拉伸速度及90°之角度,根據JIS C5012印刷線路板測試方法量測基板樹脂與鍍膜之間的黏附強度(剝離強度)。 實例1至6及比較實例1至5
使用以下樹脂基板1至3作為待處理材料的樹脂基板。 樹脂基板 樹脂基板1:Ra:100(nm) 樹脂基板2:Ra:250(nm) 環氧樹脂基板3:Ra:80(nm)
注意:Ra表示算術平均粗糙度。
將表1或表2中所示的各化合物按表1或表2中所示的量添加至去離子水中來製備調節劑。使用過錳酸鹽,使樹脂基板1至3經歷去污/粗糙化製程,隨後在45℃之溫度下在調節劑中浸沒5分鐘。接著使用過硫酸鈉進行軟蝕刻。在用酸洗滌之後,使用鹼性鈀催化劑(CIRCUPOSIT™ ADV 8530催化劑)進行催化劑給予處理並使用CIRCUPOSIT™ 6540還原劑進行還原處理。隨後,藉由在32℃之溫度下在無電鍍銅溶液(CIRCUPOSIT™ ADV 8550無電銅)中浸沒20分鐘進行無電鍍銅。在各處理之間,在室溫下用去離子水洗滌2分鐘。用SEM觀察無電鍍銅之後微導通孔中之鍍層沈積的狀態。接著進行電解鍍銅處理,隨後進行黏附性測試。評估結果亦顯示在表1或表2中。
在實例1及2中,分別添加二伸丙基三胺及雙(伸己基)三胺作為調節劑的化合物(調節劑組分)。在比較實例1及2中,使用二乙烯三胺及單乙醇胺代替實例的化合物,且在比較實例3中,不添加任何調節組分,僅用去離子水實施試驗。在比較實例4及5中,分別使用商業調節劑231及3328(均由羅門哈斯電子材料公司製造,含有陽離子聚合物、螯合劑、非離子界面活性劑及水,pH:約10及1)。 表1
表2
表3
無
圖1為SEM照片(放大倍數:2000倍),顯示經歷了實例1中之鍍銅的微導通孔之內壁表面。 圖2為SEM照片(放大倍數:2000倍),顯示經歷了實例2中之鍍銅的微導通孔之內壁表面。 圖3為SEM照片(放大倍數:2000倍),顯示經歷了比較實例1中之鍍銅的微導通孔之內壁表面。 圖4為SEM照片(放大倍數:2000倍),顯示經歷了比較實例2中之鍍銅的微導通孔之內壁表面。 圖5為SEM照片(放大倍數:2000倍),顯示經歷了比較實例3中之鍍銅的微導通孔之內壁表面。 圖6為SEM照片(放大倍數:2000倍),顯示經歷了比較實例4中之鍍銅的微導通孔之內壁表面。 圖7為SEM照片(放大倍數:2000倍),顯示經歷了比較實例5中之鍍銅的微導通孔之內壁表面。
Claims (4)
- 一種在基板上進行無電鍍的方法,包括以下步驟: (a)使所述基板與含有由以下通式(1)表示之化合物的組合物接觸:其中R1 及R2 各自獨立地為具有3至10個碳原子的伸烷基; (b)使所述基板與催化劑組合物接觸;以及 (c)使所述基板與無電鍍組合物接觸。
- 如申請專利範圍第1項所述的方法,其中所述組合物中所述由通式(1)表示之化合物的含量為0.1至10 g/L。
- 如申請專利範圍第1項或第2項所述的方法,其中所述無電鍍為無電鍍銅。
- 一種基板,其表面的至少一部分上具有藉由如申請專利範圍第1項所述的方法獲得的金屬膜。
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