TWI629322B - 用於金及金合金之表面處理溶液 - Google Patents

用於金及金合金之表面處理溶液 Download PDF

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TWI629322B
TWI629322B TW105118039A TW105118039A TWI629322B TW I629322 B TWI629322 B TW I629322B TW 105118039 A TW105118039 A TW 105118039A TW 105118039 A TW105118039 A TW 105118039A TW I629322 B TWI629322 B TW I629322B
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gold
composition
surface treatment
cationic polymer
phosphorus compound
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TW201700655A (zh
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水野陽子
Yoko Mizuno
近藤誠
Makoto Kondo
蓬田浩一
Koichi Yomogida
森永俊幸
Toshiyuki MORINAGA
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美商羅門哈斯電子材料有限公司
Rohm And Haas Electronic Materials Llc
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Abstract

本發明係關於一種組合物，其含有自含氮雜環化合物與表鹵代醇之反應產物獲得之陽離子聚合物；及磷化合物。所述組合物可用作金或金合金之表面處理劑。所述組合物可密封金或金合金之表面上之小孔。

Description

用於金及金合金之表面處理溶液
本發明係關於用於金或金合金之表面處理溶液，且更特定言之，係關於用於金或金合金之表面之密封劑。
近來年，鍍金已廣泛用於電子設備及電子組件中，尤其用於保護電子組件之連接端表面，因為金具有極佳的電特性、防腐蝕性及其類似性質。鍍金亦用作半導體元件之電極端之表面處理及電子組件(諸如用於連接電子設備之連接器)之表面處理。電子組件，諸如連接器，通常由銅或銅合金製成。通常為了在此等電子組件上應用鍍金，首先在銅表面上施用電鍍鎳作為基底電鍍，接著在鍍鎳層上鍍金。然而，因為金為昂貴的貴金屬，所以在製造此等電子組件時，儘可能地降低鍍金膜之厚度以使用更少量之金及降低製造成本。
然而，鍍金膜中小孔之數目隨著鍍金膜厚度降低而增加。若水、氯化物及其他此類腐蝕性物質滲透小孔，則此等小孔引起諸如下伏金屬鎳及母材銅腐蝕、由於表面上腐蝕反應產物之沈積而使接觸電阻公升高及其類似問題。
密封處理為解決此問題之方法之一。密封處理為 用於金之表面處理，以便藉由鍍金膜表面上化學物質之作用覆蓋小孔來改良耐腐蝕性。日本特許公開專利公開案第9-170096號描述含有抑制劑及自體乳化劑之密封處理溶液，且日本特許公開專利公開案第2003-129257號描述含有抑制劑、界面活性劑及胺化合物之基於水之密封劑。在此等文獻中，苯并三唑及其類似物例示為抑制劑，且在密封處理期間，使用電鍍材料作為陽極進行DC電解。然而，對於在密封處理中進行電解之方法，需要輔助設備進行密封處理。另一方面，本發明人進行研究且發現，當使用含有苯并三唑之水性溶液作為密封劑且不進行DC電解時，小孔之密封不足，因此可能發生腐蝕。因此，需要研發在不進行電解之簡單處理方法情況下能夠高度密封小孔之密封劑。
作為集中研究之結果，本發明人發現藉由使用含有陽離子聚合物及磷化合物之組合物，有可能在不進行如先前技術文獻中提及之電解之情況下進行高度密封處理，其中所述陽離子聚合物為含氮雜環化合物與表鹵代醇之反應產物。因此，基於此等發現，已實現本發明。
本發明係關於一種組合物，其含有陽離子聚合物及磷化合物，所述陽離子聚合物為含氮雜環化合物與表鹵代醇之反應產物。磷化合物較佳為至少一種選自由以下各者組成之群之化合物：磷酸、聚磷酸及其鹽以及磷酸酯。
本發明亦係關於用於金或金合金之表面處理劑，其含有陽離子聚合物及磷化合物，所述陽離子聚合物為含氮雜環化合物與表鹵代醇之反應產物。磷化合物較佳為至 少一種選自由以下各者組成之群之化合物：磷酸、聚磷酸及其鹽以及磷酸酯。陽離子聚合物及磷化合物之含量較佳分別為0.01至70g/L及0.01至50g/L。
本發明亦係關於用於金或金合金之表面處理方法，其包括使金或金合金之表面與含有陽離子聚合物及磷化合物之水性溶液接觸之步驟，所述陽離子聚合物為含氮雜環化合物與表鹵代醇之反應產物。
因此，本發明之一個主要目標為提供用於金或金合金之表面之密封劑，其能夠密封金或金合金之表面。
如在整個說明書中所使用，℃為攝氏度，g/L為公克/公升，ml/L為毫升/公升，μm為微米，m/min為公尺/分鐘，且A/dm2及ASD為安培/平方公分。
本發明係關於由含有陽離子聚合物及磷化合物之組合物製成之表面處理劑，所述陽離子聚合物為自含氮雜環化合物及表鹵代醇獲得之反應產物。含氮雜環化合物之實例包含咪唑及吡啶。表鹵代醇中之鹵素包含氟、氯、溴或碘。表鹵代醇之實例包含表氯醇及表溴醇。藉由使含氮雜環化合物與表鹵代醇反應而獲得之陽離子聚合物之實例包含藉由在相同溶劑中以所需濃度溶解咪唑及表氯醇且使其反應而獲得之陽離子聚合物；然而，亦可以使用市售產品。市售產品之實例包含由Raschig chemicals製造之RALU®PLATE IME(產品名稱)(CAS編號：68797-57-9)。組合物中藉由使含氮雜環 化合物與表鹵代醇反應而獲得之陽離子聚合物之含量為0.01至70g/L，較佳為1至20g/L。
本發明之組合物使用藉由使含氮雜環化合物與表鹵代醇反應而獲得之陽離子聚合物與磷化合物之混合物。磷化合物包含磷酸、聚磷酸及其鹽以及磷酸酯，較佳至少一種選自此等類型。此處，聚磷酸為藉由兩種或更多種磷酸之脫水縮合而獲得。聚磷酸包含偏磷酸及三聚磷酸。磷酸及聚磷酸之鹽指此等酸之無機或有機鹽。其實例包含鈉、鉀、銨及胍鹽。磷酸酯係藉由(C1至C6)烷基取代磷酸之至少一個羥基中之氫原子而獲得。實例包含磷酸三甲基、磷酸三乙基及其類似物。組合物中磷化合物之含量為0.01至50g/L，較佳為10至30g/L。
本發明之組合物亦可以含有pH值調節劑、濕潤劑作為視情況選用之組份。本發明之組合物亦使用水作為溶劑；較佳可使用去離子水。本發明之組合物之pH值為6至12，較佳為8至12。
本發明之組合物可以金或金合金之表面處理劑形式使用。更佳的是，其用作金或金合金之密封劑以藉由覆蓋金或金合金上之產生之小孔來防止腐蝕。
如上文所描述，在用本發明之密封劑進行金或金合金之表面處理時，使用由銅或銅合金製成之電子組件作為經處理之材料，所述由銅或銅合金製成之電子組件通常經歷鎳電鍍作為基底電鍍，接著在電鍍之鎳上電鍍金或金合金。將本發明之組合物調節至20℃至80℃，較佳30℃至60℃。使經處理之材料與以上組合物接觸0.1秒至5分鐘，較佳1 秒至1分鐘。可藉由浸漬、噴霧或其他此類方法實現接觸。接著較佳用去離子水洗滌1至60秒且乾燥。
本發明之組合物適用於在表面上具有金或金合金電鍍膜之電子設備及電子組件之表面處理劑；較佳的是，其可用作在電子組件之連接端表面上形成之金或金合金電鍍膜之表面處理劑。舉例而言，組合物可用作在半導體元件之電極端、用於連接電子設備之連接器等之表面上形成之金或金合金電鍍膜之表面處理劑。對於金或金合金電鍍，通常使用硬金電鍍溶液，例如金鈷合金電鍍、金鎳合金電鍍及其類似物。
下文中，將參考實例說明本發明；然而，本發明不限於此等實例。
實例1
使用經歷鍍鎳(2微米厚度之塗層)，接著經歷鍍金(0.026微米厚度之塗層)之銅材料之電子組件(銅合金194)作為測試樣品。將以下組合物中之組合物1調節至45℃，且將測試樣品浸沒5秒，且進行表面處理。接著用去離子水沖洗測試樣品且用氣刀及熱氣乾燥。
組合物1
自咪唑及表氯醇獲得之陽離子聚合物(產品名稱：由Raschig Chemicals製造之RALU®PLATE)：20g/L
聚磷酸鈉(由Taihei Chemical Industrial Co.,Ltd.製造)：20g/L
其餘部分：水
腐蝕測試
中性鹽霧試驗(NSS測試)
條件
噴霧溶液：5%氯化鈉水溶液
溫度：34℃至36℃
pH值：6.5至7.2
噴霧量：水平收集面積為0.5至3.0ml/h(每80cm2)
噴霧時間：48小時或72小時
噴霧角度：20度至垂直線
評估方法：用肉眼檢驗經過預定時間之後，測試樣品之表面上產生之腐蝕狀態，且根據以下準則評級。接著，用10倍顯微鏡對凹槽類腐蝕進行計數。
評估準則
第0級：未腐蝕
第1級：約1%至9%測試樣品表面區域腐蝕
第2級：約10%至29%測試樣品表面區域腐蝕
第3級：約30%至49%測試樣品表面區域腐蝕
第4級：約50%或更多之測試樣品表面區域腐蝕
實例2-3，比較實例1至8
除了組合物之濃度變成如表1至3中所描述之組合物以外，以與實例1相同之方式進行操作，以評估腐蝕程度。結果展示於表1至3中。
酯之共聚物，由Osaka Organic Chemical Co.,Ltd.製造。

Claims (5)

  1. 一種組合物，其主要由陽離子聚合物、磷化合物及水所組成，所述陽離子聚合物包括含氮雜環化合物及表鹵代醇。
  2. 如申請專利範圍第1項之組合物，其中所述磷化合物選自由以下各者組成之群：磷酸、聚磷酸及其鹽以及磷酸酯。
  3. 如申請專利範圍第1項之組合物，其中所述陽離子聚合物之量為0.01至70g/L，且所述磷化合物之量為0.01至50g/L。
  4. 一種用於金或金合金之表面處理方法，其包括：使金或金合金之表面與如申請專利範圍第1項所述的組合物接觸。
  5. 如申請專利範圍第4項之表面處理方法，其中所述磷化合物選自由以下各者組成之群：磷酸、聚磷酸及其鹽以及磷酸酯。
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