TW202330998A - 與還原處理同時使用之無電解鍍敷用前處理液 - Google Patents
與還原處理同時使用之無電解鍍敷用前處理液 Download PDFInfo
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- TW202330998A TW202330998A TW112111384A TW112111384A TW202330998A TW 202330998 A TW202330998 A TW 202330998A TW 112111384 A TW112111384 A TW 112111384A TW 112111384 A TW112111384 A TW 112111384A TW 202330998 A TW202330998 A TW 202330998A
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- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- BFXAWOHHDUIALU-UHFFFAOYSA-M sodium;hydron;difluoride Chemical compound F.[F-].[Na+] BFXAWOHHDUIALU-UHFFFAOYSA-M 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract
本發明提供於含有填充劑之絕緣樹脂基板之粗化處理後與還原處理同時使用之新穎無電解鍍敷用前處理液。
本發明之無電解鍍敷用前處理液係於使含有填充劑之絕緣樹脂基板進行粗化處理，使前述絕緣樹脂基板上生成之殘渣進行還原處理時，與還原處理同時使用之無電解鍍敷用前處理液，且其包含還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種。
Description
本發明有關於絕緣樹脂中含有填充劑之印刷配線基板之製造中，與還原處理同時使用之無電解鍍敷用前處理液及印刷配線基板之製造方法。
於電子機器類等之領域中廣泛使用之印刷配線基板多數係於絕緣樹脂基板上賦予觸媒，進行無電解銅鍍敷等之無電解鍍敷處理，並根據需要進行電鍍銅鍍敷等之電鍍敷處理液而製造。由於絕緣樹脂基板與銅之間未形成化學鍵，故無法期待絕緣樹脂基板與銅鍍敷皮膜之間之高密著性。因此，迄今係進行於對絕緣樹脂基板進行膨潤處理後，藉由浸漬於含有過錳酸鹽、鉻酸鹽等之氧化劑之粗化液中使前述絕緣樹脂基板表面粗化(蝕刻)並形成錨定形狀，而提高絕緣樹脂基板與銅鍍敷皮膜之密著性之方法。上述粗化液亦稱為去膠渣液，係用以去除伴隨設於印刷配線基板之多數孔部(例如用以連接複數導體間之盲孔或通孔，或用於電路形成之溝槽等)之形成，而於孔部或基板表面發生之樹脂渣(膠渣)者。包含下述一連串步驟之處理方法，稱為去膠渣處理方法，該一連串步驟係上述
之膨潤處理、粗化處理(利用氧化劑之蝕刻)、進而用以溶解去除因粗化處理而於樹脂基板表面產生之殘渣(例如源自過錳酸鈉之錳氧化物等)之還原處理(亦稱為中和處理)、藉由調節劑之清淨化處理等。
上述絕緣樹脂中大多含有氧化矽系填充劑等之填充劑，因此，改善絕緣樹脂基板之機械特性、電特性之同時，藉由前述粗化處理時之錨定效果而提高絕緣樹脂基板與鍍敷皮膜之密著性。
近幾年來，伴隨印刷配線基板之高機能化、高積體化，隨著絕緣樹脂基板表面之粗糙度(成為錨定之凹凸，以Ra表示)變小，產生與鍍敷皮膜之密著性降低之問題。且，伴隨樹脂材料之熱膨脹係數減低化等，有樹脂材料中所含之填充劑含量增加，藉以往之去膠渣處理無法確保與鍍敷皮膜之充分密著力之問題。
因此，本申請人於專利文獻1中揭示於絕緣樹脂中含有填充劑之印刷配線基板之形成所用之無電解鍍敷用前處理液，其使藉由粗化處理所產生之氧化物等之殘渣進行還原處理，同時作為去除上述填充劑之還原及去除步驟所用之處理液，係含有還原劑及氟化合物之還原及去除處理液。此等還原處理時，若具有去除填充劑之效果之氟化合物作為填充劑去除處理劑使用時，即使為表面粗糙度小的基板，經實證亦可獲得與鍍敷皮膜之高的密著性。
[先前技術文獻]
[專利文獻]
專利文獻1：日本特開2013-153223號公報
本發明之目的在於提供於含有填充劑之絕緣樹脂基板之粗化處理後與還原處理同時使用之新穎無電解鍍敷用前處理液。
可解決上述課題之本發明之無電解鍍敷用前處理液係如下。
項1
一種無電解鍍敷用前處理液，其特徵係於使含有填充劑之絕緣樹脂基板進行粗化處理，使前述絕緣樹脂基板上生成之殘渣進行還原處理時，與還原處理同時使用之無電解鍍敷用前處理液，且前述處理液包含還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種。
項2
如上述項1之無電解鍍敷用前處理液，其進而包含氟
化合物。
項3
如上述項1或2之無電解鍍敷用前處理液，其中前述絕緣樹脂基板含有氧化矽系填充劑，前述絕緣樹脂基板中所佔之SiO2含量為30質量%以上。
且，可解決上述課題之本發明之印刷配線基板之製造方法如以下。
項4
一種印刷配線基板之製造方法，其特徵係包含下述步驟：使含有填充劑之絕緣樹脂基板進行粗化處理之粗化處理步驟，與使因前述粗化處理步驟而於前述絕緣樹脂基板上生成之殘渣進行還原之同時，去除前述絕緣樹脂基板中含有之填充劑之還原及填充劑去除步驟，及對於於前述還原及填充劑去除步驟中經蝕刻之絕緣樹脂實施無電解鍍敷之無電解鍍敷步驟，且於前述還原及填充劑去除步驟使用包含下述之處理液：還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種。
項5
如上述項4之印刷配線基板之製造方法，其中前述還原及填充劑去除步驟中，使用進而包含氟化合物之處理液。
項6
如上述項4或5之印刷配線基板之製造方法，其中前述絕緣樹脂基板含有氧化矽系填充劑，前述絕緣樹脂基板中所佔之SiO2含量為30質量%以上。
若使用本發明之前處理液，則可獲得含有填充劑之絕緣樹脂基板與鍍敷皮膜之密著性優異之印刷配線基板。
依據本發明，考慮例如高密度、高精細之印刷配線基板之製造，即使含有填充劑之絕緣樹脂基板之表面粗糙度未變粗(亦即含有填充劑之絕緣樹脂基板表面之凹凸較小時)，或絕緣樹脂中所含之填充劑含量較多時，亦可特別提高該基板與鍍敷皮膜之密著性。因此，本發明之技術可較好地使用於如高速信號或高密度配線等之表面粗糙度小的電路基板之製造。
又，本發明之技術並非僅適用於配線基板之製造方法、利用增層工法之高密度多層配線基板之製造，而亦適用於例如晶圓等級CSP(晶片尺寸環氧封裝或晶片等級環氧封裝)或TCP(帶承載之封裝)等中之多層配線
層之製造。
圖1(a)係表1之No.19(比較例)之表面SEM照片，圖1(b)係表1之No.5(本發明例)之表面SEM照片。
本發明人等為了提供用以製造即使含有填充劑之絕緣樹脂基板之表面粗糙度(Ra)約為0.01~0.3μm而較小，或絕緣樹脂中所含之填充劑(SiO2換算)之含量為約30質量%而較多，與鍍敷皮膜之密著性亦良好之印刷配線基板之表面處理方法(去膠渣處理)，而重複檢討。其結果，發現若使用如下之處理液，則可達成期望目的，因而完成本發明，該處理液係於含有填充劑之絕緣樹脂基板之粗化處理後，與還原處理(中和處理)同時使用之處理液(處理劑)，且其包含還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種。以下，本發明所用之乙二醇系二醇醚或丙二醇系二醇醚有時簡稱為二醇醚。
本發明中，所謂與還原處理同時使用之無電解鍍敷用前處理液(前處理劑)意指對含有填充劑之絕緣
樹脂基板進行粗化處理，使於前述絕緣樹脂基板上生成之殘渣進行還原處理時，與還原劑一起使用之前處理液。例如，若舉進行銅鍍敷製造印刷配線基板之方法為例，則於使含有填充劑之絕緣樹脂基板進行膨潤處理、粗化處理、用以使粗化處理所發生之氧化物還原之還原處理(中和處理)、根據需要之超音坡處理、乾燥、調節(清潔)、軟蝕刻、酸洗、觸媒賦予、無電解銅鍍敷、電解銅鍍敷而製造印刷配線基板時，於粗化處理後，與還原劑同時使用之前處理液。本發明中，與還原處理同時使用之上述無電解鍍敷用前處理液有時簡稱為前處理液。且含有填充劑之絕緣樹脂基板有時簡稱為絕緣樹脂基板或樹脂基板。
因此本發明之特徵部分在於與通常所用之還原劑一起使用上述二醇醚作為與還原處理(中和處理)同時使用之前處理液。依據本發明人等之檢討結果，判知藉由使上述二醇醚與還原劑一起使用於還原處理時，可發揮良好之填充劑去除作用。其結果，發現即使用迄今與鍍敷皮膜之密著性困難之表面粗糙度小的含有填充劑之絕緣樹脂基板或填充劑含量多的絕緣樹脂基板時，亦可獲得良好密著性，因而完成本發明。
針對該點，再稍微詳細說明。通常，藉由氧化劑(例如過錳酸鹽等之Mn等)之粗化處理，蝕刻含有填充劑之絕緣樹脂基板時，於絕緣樹脂基板中所含之填充劑表面及保持填充劑之樹脂表面上吸附Mn等之氧化劑。吸附於表面之Mn等之氧化劑，藉由隨後之還原劑(中和
劑)之還原處理(氧化還原處理)而溶解，且藉由此時發生之氧氣去除填充劑。不過，於粗化處理中，因蝕刻而於較小的填充劑與保持填充劑之樹脂之間形成非常狹小間隙(間隔)，由於通常之還原處理所用之還原劑(中和劑)浸透性差，故幾乎無法浸透至上述非常狹小間隙中。因此，上述氧化還原反應未充分進行，而難以去除填充劑。
相對於此，由於本發明所用之上述二醇醚浸透性優異，故即使是上述非常狹小之間隙亦能浸透。而且，伴隨二醇醚浸透於上述間隙(與二醇醚浸透一起)還原劑亦到達上述間隙並浸透，藉由進入間隙，而與Mn等之氧化劑反應並產生氧氣。認為藉由該氧氣擠出填充劑並去除，結果使樹脂基板與鍍敷皮膜之密著性格外提高。
亦即，本發明所用之二醇醚藉由與還原劑併用，而發揮良好的填充劑去除效果，具有有助於提高與鍍敷皮膜之密著性之作用。
如此，藉由本發明，對於施以膨潤處理之絕緣樹脂基板，藉由過錳酸鉀等進行粗化處理後，應用本發明之前處理液，可與因粗化處理所產生之處理殘渣之還原反應溶解去除同時去除填充劑。此認為係因為即使於進行藉由過錳酸鉀等之粗化處理前打算去除填充劑，填充劑亦以被樹脂覆蓋之方式含有，故無法有效去除填充劑，其結果，無法發揮使絕緣樹脂基板與鍍敷皮膜之充分密著性提高效果之故。因此，本發明中，首先將覆蓋填充劑之樹脂藉由使樹脂基板粗化而去除後，與去除藉由粗化處理產生
之氧化物等殘渣同時去除填充劑。
本發明之無電解鍍敷用前處理液包含還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種。
首先，針對本發明所用之二醇醚加以說明。二醇醚係有機溶劑之一種，係作為例如塗料、墨水等之溶劑使用。二醇醚包含例如以乙二醇為基礎之乙二醇系(E.O.系)、以丙二醇為基礎之丙二醇系(P.O.系)等。本發明人等發現上述之E.O.系及P.O.系之二醇醚中，尤其是以下式(1)表示之乙二醇系二醇醚及以下式(2)表示之丙二醇系二醇醚與還原劑併用時，氧化矽系填充劑等之作為去除處理劑(填充劑去除處理劑)的作用更提高；其結果，顯著提高絕緣樹脂基板與鍍敷皮膜之密著性。作為藉由使用上述二醇醚而提高密著性之理由，舉例為例如因上述機制而使粗化處理後露出於樹脂表面上之填充劑效率良好地去除。且，推測於粗化處理後，藉由包含還原劑與上述二醇醚之前處理液進行處理，而使填充劑周邊之樹脂膨潤，使鍍敷皮膜易於填充劑與樹脂之間析出，亦為密著性提高之一要因。
CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)…(1)
CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)…(2)
因此本發明就發現到二醇醚中，尤其是上式(1)、(2)表示之二醇醚與還原劑同時使用時可作為良好的填充劑去除劑發揮作用之方面係具有技術意義上之發明。
又，前述專利文獻1亦與本發明同樣，揭示與還原劑同時使用之前處理液，但上述專利文獻1中，就作為還原時之填充劑去除劑係使用氟化合物之方面，與使用上述二醇醚作為還原時之填充劑去除劑之本發明不同。如本發明之使用上述二醇醚之情況，與使用氟化合物之情況相比，由於更有效發揮填充劑去除效果，故結果，更提高與鍍敷皮膜之密著性。此方面於後述之實施例欄中亦獲得證實，於代替二醇醚而使用氟化合物之表1的No.22中，成為密著性指標之剝離強度降低。
作為上式(1)表示之乙二醇系二醇醚，舉例為乙二醇甲醚(n=1，m=1)、乙二醇乙醚(n=1，m=2)、乙二醇丙醚(n=1，m=3)、乙二醇丁醚(n=1，m=4)、二乙二醇甲醚(n=2，m=1)、二乙二醇乙醚(n=2，m=2)、二乙二醇丙醚(n=2，m=3)、二乙二醇丁醚(n=2，m=4)、三乙二醇甲醚(n=3，m=1)、三乙二醇乙醚(n=3，m=2)、三乙二醇丙醚(n=3，m=3)、三乙二醇丁醚(n=3，m=4)、四乙二醇甲醚(n=4，m=1)、四乙二醇乙醚(n=4，m=2)、四乙二醇丙醚
(n=4，m=3)、四乙二醇丁醚(n=4，m=4)。
又，作為上式(2)表示之丙二醇系二醇醚，舉例為丙二醇甲醚(x=1，y=1)、二丙二醇甲醚(x=1，y=2)、三丙二醇甲醚(x=1，y=3)、丙二醇乙醚(x=2，y=1)、二丙二醇乙醚(x=2，y=2)、三丙二醇乙醚(x=2，y=3)、丙二醇丙醚(x=3，y=1)、二丙二醇丙醚(x=3，y=2)、三丙二醇丙醚(x=3，y=3)、丙二醇丁醚(x=4，y=1)、二丙二醇丁醚(x=4，y=2)、三丙二醇丁醚(x=4，y=3)。
此處，上式(1)、(2)表示之二醇醚中之丙基、丁基可為直鏈狀亦可為分支狀。
該等中，若考慮密著性更提高等，較佳之二醇醚較好為上式(1)表示之乙二醇系二醇醚，更好為二乙二醇丁醚(例如二乙二醇單正丁醚等)。
本發明中，以上式(1)、(2)表示之二醇醚可單獨使用，亦可併用兩種以上。作為併用例，舉例為使用兩種以上之上式(1)表示之二醇醚之例，使用兩種以上之上式(2)表示之二醇醚之例，使用兩種以上之上式(1)表示之二醇醚與上式(2)表示之二醇醚之例。
本發明之前處理液包含上述二醇醚與還原劑。本發明所用之還原劑若為粗化處理後於還原處理中通常使用之還原劑，則未特別限定，舉例為例如過氧化氫、硫酸羥基銨、乙醛酸、硫酸羥基胺、乙二胺、二伸乙三胺、三伸乙四胺、四伸乙五胺、單乙醇胺、二乙醇胺、乙
二胺四乙酸、氮基三乙酸等之各種胺系化合物等。
本發明之前處理液之pH大約為3.0以下。藉此有效地發揮還原劑之作用。
此處，將上述二醇醚、還原劑與水之合計量設為「前處理液總量」時，相對於上述前處理液總量的上述二醇醚之較佳含量(單獨含有時為單獨量，含兩種以上時為合計量)為30g/L以上、800g/L以下，更好為50g/L以上、600g/L以下。低於上述下限時，無法有效發揮二醇醚之添加效果，使鍍敷密著性降低。另一方面，即使超過上述上限而添加，二醇醚之添加效果亦已飽和，就經濟上較浪費。
又，相對於上述前處理液總量的還原劑之較佳含量為0.1g/L以上、500g/L以下，更好為1g/L以上、300g/L以下。低於上述下限時，無法有效發揮還原劑之添加效果，吸附於基板之錳去除性能降低。另一方面，即使超過上述上限而添加，還原劑之添加效果亦已飽和，就經濟上較浪費。
本發明之處理液含有還原劑與上述二醇醚，只要前述處理液之pH滿足上述區域，則亦可含有還原處理所用之其他成分。
例如上述前處理液可進而含有氟化合物。藉由添加氟化合物，更提高密著性。作為本發明所用之氟化合物，舉例為例如酸性氟化鈉、酸性氟化銨、日本特開2010-106337號公報中記載之二氟化氫銨、前述專利文獻1
中記載之氟化合物(氟化氫；硼氟化氫酸；氟化鈉、氟化氫鈉等之鈉鹽；氟化氫銨、六氟矽酸銨、六氟磷酸銨等之銨鹽等)。該等可單獨添加，亦可併用兩種以上。
上述氟化合物可用於提高絕緣樹脂基板與鍍敷皮膜之密著強度。本發明中較好使用之氟化合物為酸性氟化鈉或酸性氟化銨，更好為酸性氟化銨。
相對於上述前處理液總量的上述氟化合物之較佳含量(單獨含有時為單獨量，含兩種以上時為合計量)為0.01g/L以上、100g/L以下，更好為1g/L以上、50g/L以下。低於上述下限時，無法有效發揮氟化合物之添加效果，使密著性降低。另一方面，即使超過上述上限而添加，氟化合物之添加效果亦已飽和，就經濟上較浪費。
進而上述前處理液亦可含有界面活性劑，藉此，提高浸透性等。上述界面活性劑種類並未特別限定，可使用非離子(nonionic)性界面活性劑、離子性界面活性劑兩者。該等可單獨添加，亦可併用兩種以上。
該等非離子(nonionic)性界面活性劑作為前處理劑之表面張力減低劑為有用。又，進而使用陽離子性界面活性劑作為界面活性劑時，亦發揮作為上述陽離子性界面活性劑之分散劑之作用。較佳之非離子界面活性劑為聚氧乙烯烷基醚；聚氧乙烯辛基苯基醚、聚氧乙烯壬基苯基醚等之聚氧乙烯烷基苯基醚。上述非離子性界面活性劑可單獨添加，亦可併用兩種以上。
又，離子性界面活性劑包含陽離子性界面活性劑、陰離子性界面活性劑、兩性界面活性劑，本發明中可使用任一者。
此等上述陽離子性界面活性劑具有吸附於帶負電荷之絕緣樹脂基板表面而中和電荷之作用。較佳之陽離子性界面活性劑為聚氯化二烯丙基二甲基銨、聚氯化二烯丙基二甲基銨與丙烯醯胺之共聚物、聚伸乙基亞胺。
上述陰離子性界面活性劑具有吸附於帶正電荷之絕緣樹脂基板表面而中和電荷之作用。作為陰離子性界面活性劑，可使用例如日本特開2011-228517號公報中記載者。
上述兩性界面活性劑係於鹼性區域顯示陰離子性界面活性劑之性質，於酸性區域顯示陽離子性界面活性劑之性質者。如後述之本發明之前處理液，由於較好顯示pH3.1以下之酸性，故藉由使用兩性界面活性劑，發揮陽離子性界面活性劑之性質。作為上述兩性界面活性劑，可使用例如日本特開2011-228517號公報中記載者。
本發明中，相對於上述前處理液總量的上述界面活性劑之較佳含量(單獨含有時為單獨量，含兩種以上時為合計量)為0.1g/L以上、500g/L以下，更好為1g/L以上、100g/L以下。低於上述下限時，無法有效發揮界面活性劑之添加效果，使無電解Cu鍍敷對於玻璃之析出性降低。另一方面，即使超過上述上限而添加，界面活性劑之添加效果亦已飽和，就經濟上較浪費。
以上針對構成本發明之前處理液之成分加以詳述。
其次，針對本發明之印刷配線基板之製造方法加以說明。本發明之製造方法包含下述步驟：使含有填充劑之絕緣樹脂基板進行粗化處理之粗化處理步驟，與使因前述粗化處理步驟而於前述絕緣樹脂基板上生成之殘渣進行還原之同時，去除前述絕緣樹脂基板中含有之填充劑之還原及填充劑去除步驟，及對於於前述還原及填充劑去除步驟中經蝕刻之絕緣樹脂實施無電解鍍敷之無電解鍍敷步驟，其特徵為於前述還原及填充劑去除步驟使用前述之本發明之前處理液。本發明之製造方法，由於使用前述之本發明之前處理液，故獲得含有填充劑之絕緣樹脂基板與鍍敷皮膜之密著性極優異之印刷配線基板。
以下針對各步驟加以說明。
首先，準備含有填充劑之絕緣樹脂基板。作為本發明所用之絕緣樹脂，若為去膠渣處理等中通常使用者，則未特別限定，例如除了作為電絕緣樹脂而廣泛使用之環氧樹脂以外，又舉例為醯亞胺樹脂、酚甲醛樹脂、酚醛清漆樹脂、三聚氰胺樹脂、聚苯醚樹脂、雙馬來醯亞胺-三嗪樹脂、矽氧烷樹脂、馬來醯亞胺樹脂、聚醚醚酮樹脂、聚醚醯亞胺樹脂、聚醚碸等。當然，不限定於該等，上述以外，亦可使用例如以任意比例混合選自前述樹脂之2種以上之樹脂而生成之樹脂等。
本發明所用之填充劑代表性舉例為氧化矽系
填充劑。氧化矽系填充劑於提高絕緣樹脂基板之機械特性、電特性等有用，並且藉由粗化處理時之錨定效果亦有助於提高絕緣樹脂基板與鍍敷皮膜之密著性。
本發明之前處理液之優異鍍敷密著性，於絕緣樹脂中所含之SiO2含量為例如30質量%以上(進而例如40質量%以上、95質量%以下)時，即使於比通常之氧化矽系填充劑更多時亦可有效發揮。
又，本發明之前處理液之優異密著性，即使於含有填充劑之絕緣樹脂基板之表面粗糙度(Ra)較小為約0.01~0.1μm時亦可有效發揮。
其次，對上述含有填充劑之絕緣樹脂基板進行膨潤處理。藉由膨潤處理，後續步驟之粗化處理中基板表面之粗化變容易。作為上述膨潤處理所用之膨潤液，舉例為例如N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺、γ-丁內酯、乙二醇單丁醚等。膨潤處理較好使含有填充劑之絕緣樹脂基板於約60~90℃左右之溫度於上述膨潤液中浸漬10~30分鐘而進行。
其次，膨潤處理後之含有填充劑之絕緣樹脂基板經水洗後，使基板表面進行粗化處理(蝕刻)。作為上述粗化處理所用之蝕刻液，舉例為例如過錳酸鈉、過錳酸鉀、鉻酸鈉、鉻酸鉀等之氧化劑。粗化處理係於上述蝕刻液之鹼溶液中，與前述水洗後之含有填充劑之絕緣樹脂基板接觸而進行。作為接觸方法，舉例為例如浸漬等。具體而言，較好於例如50~80℃左右之溫度接觸1~10分鐘，
使樹脂表面粗化。
如此使樹脂基板表面粗化後，使用本發明之前處理液進行還原及填充劑之去除。具體而言，與藉由對於因粗化處理而於樹脂基板表面產生之錳氧化物等之處理殘渣進行還原反應之溶解處理(還原處理)同時進行上述二醇醚之填充劑之去除處理。
上述之還原及填充劑之去除較好係例如將粗化後之含有填充劑之絕緣樹脂基板浸漬於本發明之前處理液中，於約20~80℃左右之溫度處理約5秒~10分鐘而進行。藉此，不僅進行錳氧化物等之粗化處理殘渣之溶解去除，亦進行填充劑之去除。
其次，根據需要，亦可進行超音波處理，藉此，提高填充劑之去除效果，密著性更提高。作為超音波處理條件，較好將頻率控制為例如20~200kHz之範圍。更好為24~100kHz。頻率低於上述下限時，無法有效發揮上述效果。另一方面，頻率超過上限時，對基板之損傷增大。且，超音波之照射時間較好控制於約10秒~10分鐘之範圍。照射時間未達10秒時，無法有效發揮上述效果。另一方面，照射時間超過10分鐘時，有產生對內層金屬過度蝕刻之虞。
其次，藉由周知方法實施清淨處理而清潔樹脂基板。藉由該清淨處理，去除樹脂基板表面之髒汙等而使表面清淨化，並且由於對樹脂基板賦予水濡濕性，故與於後續步驟所形成之鍍敷皮膜之密著性更提高。上述清淨
處理所用之溶液種類並未特別限定，可使用例如至少含有非離子界面活性劑及陽離子界面活性劑兩者之清潔劑‧調節劑等。具體而言，較好於清潔劑‧調節劑中，於約40℃下使經施以上述表面處理之樹脂基板浸漬5分鐘。
如以上之進行鍍敷前處理後，施以鍍敷處理。鍍敷處理方法並未特別限定，例如採用半添加法、全添加法等通常使用之方法形成鍍敷皮膜。鍍敷處理之細節可參考例如前述之專利文獻1或日本特開2015-71821號公報之記載等。
以下針對全添加法之鍍敷處理方法詳細加以說明。又，以下中，針對形成銅鍍敷皮膜之例加以說明，但鍍敷皮膜種類不限定於銅鍍敷皮膜，可為鎳等之其他金屬鍍敷皮膜。又，亦可不使用全添加法之鍍敷處理，而使用半添加法，藉由電鍍形成鍍敷皮膜。
前述之膨潤處理、粗化處理後，使用本發明之前處理液對於因粗化處理所發生之處理殘渣進行還原溶解處理及填充劑去除。
其次，對形成電路圖型之樹脂基板表面賦予觸媒。上述觸媒賦予所用之觸媒種類若為通常所用者，則未特別限定，可使用例如含2價鈀離子(Pd2+)之觸媒液；含氯化鈀(PdCl2‧2H2O)與氯化亞錫(SnCl2‧2H2O)與鹽酸(HCl)之混合液等。作為上述混合溶液之濃度，較好控制為Pd濃度：100~300mg/L，Sn濃度：10~20g/L，HCl濃度：150~250mL/L之範圍。於此種觸媒
溶液中使絕緣樹脂基板於例如30~40℃之溫度浸漬1~3分鐘，而首先使Pd-Sn膠體吸附於樹脂基板表面。其次，於常溫條件下，浸漬於例如由50~100mL/L之硫酸或鹽酸所成之加速劑(促進劑)中，進行觸媒之活化。藉由該觸媒活化處理，去除錯化合物之錫，成為鈀吸附粒子，最終作為鈀觸媒，促進隨後之利用無電解銅鍍敷之銅析出。又，亦可使用氫氧化鈉或氨溶液作為加速劑。又，對於該樹脂基板賦予觸媒時，施以使用調節液或預浸漬液之前處理，亦可進而施以可使樹脂基板與銅鍍敷皮膜之密著性進一步提高，進而使觸媒對樹脂基板表面之親和性良好之前處理。
其次，如此對絕緣樹脂基板賦予觸媒後，形成用以適當形成期望電路圖型之鍍敷抗蝕劑。亦即，於下一步驟，形成將構成電路圖型之銅鍍敷皮膜析出之部位以外遮蔽之抗蝕劑圖型。此抗蝕劑圖型可於鍍敷處理結束後藉由蝕刻操作等剝離去除，但亦可於鍍敷處理後不剝離去除，而作為焊料抗蝕劑發揮功能。鍍敷抗蝕劑之形成方法可使用周知方法進行。
形成鍍敷抗蝕劑後，藉由無電解鍍敷法，析出銅鍍敷皮膜，形成電路圖型。又，藉由無電解鍍敷法析出銅鍍敷皮膜時，亦可於形成鍍敷抗蝕劑後，使用例如10%硫酸及還原劑，使附著於樹脂基板表面之觸媒的鈀吸附粒子還原而使觸媒活化，而提高樹脂基板上之銅鍍敷之析出。
具體而言，作為上述無電解銅鍍敷所用之鍍敷浴，例如可使用含EDTA作為錯化劑之鍍敷浴。作為上述無電解銅鍍敷浴之組成之一例，可使用含有硫酸銅(10g/L)、EDTA(30g/L)，且藉由氫氧化鈉將pH調整至約12.5左右之無電解銅鍍敷浴。又，亦可使用羅歇爾鹽(Rochelle salt)作為錯化劑之無電解銅鍍敷浴。而且，該無電解鍍敷浴中之絕緣樹脂基板於例如60~80℃之溫度浸漬30~600分鐘而形成銅鍍敷皮膜。且，例如於多層配線基板中形成用以與下層導通之通孔(via)時，亦可充分進行液之攪拌，對通孔充分進行離子之供給。攪拌方法並未特別限定，可適用例如利用空氣攪拌、泵循環等之攪拌等方法。
又，該鍍敷處理中，為了更提高絕緣樹脂基板之密著，亦可施以兩階段鍍敷。亦即，於樹脂基板上進行形成基底鍍敷皮膜之一次鍍敷處理，於所形成之基底鍍敷皮膜上，進行形成膜厚比基底鍍敷皮膜更厚之厚鍍敷皮膜之二次鍍敷處理而形成電路圖型。尤其於一次鍍敷處理時，亦可進行形成基底鍍敷皮膜之無電解鍍敷浴之鍍敷處理，該基底鍍敷皮膜具有與藉二次鍍敷處理形成之厚鍍敷皮膜之內部應力方向不同方向之內部應力，換言之，具有方向與二次鍍敷處理所形成之厚鍍敷皮膜之內部應力相反方向之內部應力且一般係拉伸內部應力。
本申請案係基於2016年8月10日提出申請之日本專利申請第2016-158009號主張優先權利益者。2016年8
月10日提出申請之日本專利申請第2016-158009號之說明書全部內容於本申請案中加以援用供參考。
[實施例]
以下列舉實施例更具體說明本發明，但本發明不受下述實施例之限制，亦可在可適合前/後主旨之範圍內加以變更並實施，該等均包含於本發明之技術範圍。
實施例1
本實施例中，使用包含表1中記載之成分的前處理液，製作以下試料。表1中，氟化合物意指酸性氟化銨(KISHIDA化學股份有限公司製之酸性氟化銨)。氟化合物之濃度均為5g/L。且還原劑濃度均為20g/L。
具體而言，首先，使用於玻璃‧環氧樹脂基板(NEMA記號FR-4)上層合味之素精密科技公司製之樹脂膜ABF-GX92R(絕緣樹脂基板中含有以SiO2換算為45質量%之氧化矽系填充劑)之絕緣樹脂基板，依表2中記載之順序，進行膨潤、粗化、使用表1中記載之各種前處理液之處理、依據需要之超音波處理(頻率28KHz)、乾燥、藉由清潔劑‧調節劑之處理。此時之表面粗糙度Ra為0.18μm。其次，進行軟蝕刻、酸洗後，藉由觸媒賦予製程(預浸漬、活化劑、還原劑、加速劑)賦予Pd觸媒後，進行無電解銅鍍敷並乾燥，形成厚度0.8μm之鍍敷皮膜。進而進行乾燥、熱處理、清潔劑、酸洗後，以2.5A/dm2之條
件進行銅電鍍，形成厚度25μm之銅鍍敷皮膜。隨後，進行防止變色處理、乾燥、熱處理，製作試料。
使用如此製作之試料，如以下測定鍍敷皮膜與絕緣樹脂基板之密著強度。
(鍍敷皮膜與絕緣樹脂基板之密著強度之測定)
對上述試料切入1cm寬之切痕，基於JIS-C5012「8.5鍍敷密著性」中記載之方法，進行90剝離試驗，測定剝離強度。剝離強度使用島津製作所製AUTOGRAPH AGS-X進行測定。
該等結果一併記於表1。
用於參考，顯示表1之No.19(比較例)與No.5(本發明例)之表面SEM照片。
由表1可探討如下。
首先，No.1~18為使用本發明之前處理液之本發明例，乙二醇系(No.1~13)、丙二醇系(No.14~18)
任一者均獲得剝離強度為600gf/cm以上，與鍍敷皮膜之密著性優異之試料。詳細而言，No.2、5~7、10均為以濃度200g/L之濃度使用二乙二醇單正丁醚(n=2，m=4)之例，不管還原劑種類，均獲得良好密著性。上述效果於前處理液之處理後，進行超音波處理時，比未進行超音波處理之No.10更提高。未進行超音波處理之上述例中，進而添加氟化合物之No.5，密著性進一步提高，剝離強度超過700gf/cm。
又，No.20係乙二醇中之二醇醚的濃度低之參考例，密著性降低。
相對於此，使用未滿足本發明任一要件之處理液的No.19、21、22之比較例具有以下缺點。
No.19係僅含有還原劑，不含本發明規定之二醇醚之比較例，由於還原時填充劑去除效果不充分，故密著性降低。
No.21係並非本發明之前處理液，而使用含有膨潤處理通常所用之N-甲基-2-吡咯啶酮與還原劑之處理液的比較例，無法有效發揮還原時之填充劑去除效果，密著性降低。
No.22係模擬專利文獻1之比較例，並非使用本發明規定之二醇醚，而使用氟化合物之例。藉由氟化合物之添加，No.22之剝離強度相較於No.19、21之比較例更為提高，可知比本發明例之No.1~18差。
又，由圖1可知，本發明之前處理液，還原時
之填充劑去除效果優異。詳言之，No.19之比較例，係如圖1(a)所示，未經去除之填充劑(圖中以箭頭表示)大量殘存於表面，相對於此，No.5之本發明例如圖1(b)所示，幾乎未觀察到填充劑。
由該等結果證明，為了確保期望之密著性，使用還原劑與本發明規定之二醇醚之處理液為有用。
Claims (3)
- 一種無電解鍍敷用前處理液，其特徵係於使含有填充劑之絕緣樹脂基板進行粗化處理，使前述絕緣樹脂基板上生成之殘渣進行還原處理時，與還原處理同時使用之無電解鍍敷用前處理液，且前述前處理液包含選自過氧化氫及乙醛酸所成群之還原劑；與選自由以CmH(2m+1)-(OC2H4)n-OH(m=1~4之整數，n=1~4之整數)表示之乙二醇系二醇醚及以CxH(2x+1)-(OC3H6)y-OH(x=1~4之整數，y=1~3之整數)表示之丙二醇系二醇醚所成之群中之至少一種，前述乙二醇系二醇醚、還原劑與水之合計量設為「前處理液總量」時，相對於前述前處理液總量的前述乙二醇系二醇醚之含量合計為30g/L以上。
- 如請求項1之無電解鍍敷用前處理液，其進而包含氟化合物。
- 如請求項1或2之無電解鍍敷用前處理液，其中前述絕緣樹脂基板含有氧化矽系填充劑，前述絕緣樹脂基板中所佔之SiO2含量為30質量%以上。
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| JP2016158009A JP6982383B2 (ja) | 2016-08-10 | 2016-08-10 | 還元処理と同時に用いられる無電解めっき用前処理液、およびプリント配線基板の製造方法 |
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| TW106121127A TWI805550B (zh) | 2016-08-10 | 2017-06-23 | 印刷配線基板之製造方法 |
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| JP7228468B2 (ja) * | 2019-05-28 | 2023-02-24 | 上村工業株式会社 | プリント配線基板の製造方法 |
| CN110670050B (zh) * | 2019-10-24 | 2021-11-12 | 深圳市松柏实业发展有限公司 | 化学镀铜活化液及其制备方法 |
| CN112095110B (zh) * | 2020-11-18 | 2021-03-12 | 苏州天承化工有限公司 | 一种abf表面处理剂及其制备方法和应用 |
| WO2023242157A1 (en) * | 2022-06-14 | 2023-12-21 | Atotech Deutschland GmbH & Co. KG | Method for cleaning a nonconductive surface and use |
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| WO2018029990A1 (ja) | 2018-02-15 |
| US20190264329A1 (en) | 2019-08-29 |
| KR20190039093A (ko) | 2019-04-10 |
| CN109563623A (zh) | 2019-04-02 |
| KR102502531B1 (ko) | 2023-02-21 |
| EP3498884A1 (en) | 2019-06-19 |
| TW201816181A (zh) | 2018-05-01 |
| EP3498884A4 (en) | 2020-04-01 |
| US20210047734A1 (en) | 2021-02-18 |
| JP2018024916A (ja) | 2018-02-15 |
| US10927463B2 (en) | 2021-02-23 |
| TWI805550B (zh) | 2023-06-21 |
| JP6982383B2 (ja) | 2021-12-17 |
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