TWI772655B - 抗氧化導電銅漿及其製造方法與應用 - Google Patents
抗氧化導電銅漿及其製造方法與應用 Download PDFInfo
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- TWI772655B TWI772655B TW108122143A TW108122143A TWI772655B TW I772655 B TWI772655 B TW I772655B TW 108122143 A TW108122143 A TW 108122143A TW 108122143 A TW108122143 A TW 108122143A TW I772655 B TWI772655 B TW I772655B
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- Prior art keywords
- copper paste
- oxidation
- substrate
- conductive
- conductive copper
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Abstract
本發明係關於一種抗氧化導電銅漿及其製造方法與應用，本發明抗氧化導電銅漿係以70wt%~90wt%之銅粒子，黏結劑，觸變劑以及溶劑所組成；本發明抗氧化導電銅漿的製造方法包含將黏結劑，觸變劑與乙醇混合均勻，獲得第一混合液；將溶劑加入第一混合液，混均以獲得第二混合液；將銅粒子加入第二混合液，以獲得導電銅漿前驅液；以及移除導電銅漿前驅液之乙醇，以獲得本發明抗氧化導電銅漿；本案之抗氧化導電銅漿具有良好的分散性、導電性、耐熱性且不易氧化，可應用於製備導電薄膜，且導電薄膜可藉由印刷流程形成，以製成電路板或太陽能電池電極。
Description
本發明有關於一種抗氧化導電銅漿及其製造方法與應用，尤其是一種分散性佳且不易氧化的導電銅漿及其製造方法與應用。
目前在電子產品的研發上，尤其是個人隨身攜帶的電子產品研發上，如何使產品更為輕薄為重要的開發方向，因此電子元件或是電路基板的微型化為相當重要的研發方向。導電膠體為一種固化後或是乾燥之後具有導電性的物質，可以做為電子零件的電性傳導物質，且其作用時的溫度較低，較不會對電子零件造成傷害；又，導電膠體亦能以漿料的形式存在，並經由高精密度的印刷或是加工方法塗佈於基板上以形成電路，以製備輕薄的電路基板；此外，導電膠體的可塗佈成型且導電性佳的特性，亦可以應用於製備太陽能電池的電極及疊片模組膠料。
目前現有的導電膠體大多為導電銀膠或是導電鋁膠，但是導電銀膠價格較高，又導電鋁膠具有高收縮性而容易產生捲曲或變形的
現象，因此仍亟需開發兼具有低成本且穩定性高的導電膠體或導電漿體。
今，發明人鑑於現有導電膠體或導電漿體於實際使用時仍有不足之處，於是乃一本孜孜不倦之精神，並藉由其豐富專業知識及多年之實務經驗所輔佐，研創出本發明。
本發明提供一抗氧化導電銅漿及其製造方法與應用，抗氧化導電銅漿內含有的銅粒子可以均勻分散，製成之抗氧化導電銅漿導電性高，亦具有不易氧化的優點。
本發明之抗氧化導電銅漿，包含70wt%~90wt%之導電粒子，4wt%~16wt%之黏結劑，0.5wt%~7wt%之觸變劑，以及5wt%~25wt%之溶劑；其中導電粒子為一奈米銅粒子，一次微米銅粒子與一微米銅粒子其中至少之一者；以及該黏結劑係包含一有機樹脂與一無機化合物。
本發明抗氧化導電銅漿之製備方法包含：步驟一，將一黏結劑，一觸變劑與一乙醇混合均勻，以獲得一第一混合液，其中該黏結劑包含一有機樹脂與一無機化合物；步驟二，將一溶劑加入該第一混合液，混合均勻後以獲得一第二混合液；步驟三，將一導電粒子加入該第二混合液，使用均質刀具混合均勻以獲得一導電銅漿前驅液，其中該導電粒子為一奈米銅粒子，一次微米銅粒子或一微米銅粒子；以及步驟四，移除該導電銅漿前驅液之乙醇，以獲得本發明之抗氧化導電銅漿。
本發明之抗氧化導電銅漿，可應用於製備導電薄膜，且導電薄膜可藉由一印刷流程形成，該印刷流程為網版印刷、塗佈印刷、浸塗印刷、噴塗印與噴墨印刷其中至少之一。
於本發明之一實施例中，導電粒子之粒徑係介於50nm~3000nm。
於本發明之一實施例中，有機樹脂包含一纖維素醚、一酚醛樹脂與一酚醛環氧樹脂其中至少之一者，且該無機化合物係為一二氧化矽(SiO2)或一氧化錫(SnO2)。
於本發明之一實施例中，觸變劑係包含一聚醯胺蠟類或一氧化聚乙烯蠟。
於本發明之一實施例中，溶劑係包含一二乙二醇丁醚、一松油醇與一2,2,4-三甲基-1,3戊二醇單異丁酸酯其中至少之一者。
於本發明之一實施例中，抗氧化導電銅漿係塗佈於一基板，並經一加熱固化步驟後以獲得一導電薄膜印刷基板，其中該基板為一玻璃基板、一ITO玻璃基板、一可撓性聚醯亞胺基板(PI基板)、一異質PI基板(MPI)、聚對苯二甲酸乙二醇酯基板(PET基板)、一化鎳鍍金基板、一美拉基板(Mylar基板)、一矽基板、一銅箔基板、一銅箔軟板、一玻璃纖維板FR4、一液晶高分子(LCP)板材或一陶瓷基板。
於本發明之一實施例中，加熱固化步驟係將塗佈有該抗氧化導電銅漿之該基板於140~850℃作用5~120分鐘。
於本發明之一實施例中，網版印刷所使用之網版的網目數係為32網目至520網目。
於本發明之一實施例中，網版印刷所獲得的之一圖案的網印圖案之印製厚度係為5微米(μm)至200微米(μm)，印製線寬係至少為50微米(μm)。
於本發明之一實施例中，導電薄膜印刷基板之電阻率係介於10-3歐姆-公分至10-7歐姆-公分。
本案之抗氧化導電銅漿及其製造方法與應用，所製得的抗氧化導電銅漿組成均勻且分散性佳，能穩固的附著於基板上，並能提供優良的導電能力。
S1:步驟一
S2:步驟二
S3:步驟三
S4:步驟四
第一圖：本發明抗氧化導電銅漿製備流程圖。
第二圖：本發明抗氧化導電銅漿固化後之掃描式電子顯微鏡照片。
第三圖(A)：本發明抗氧化導電銅漿印刷之電路板示意圖。
第三圖(B)：本發明抗氧化導電銅漿製備之太陽能電池電極示意圖。
第四圖(A)：本發明抗氧化導電銅漿之印刷精密度光學顯微鏡照片。
第四圖(B)：本發明抗氧化導電銅漿之印刷精密度電子顯微鏡照片。
第五圖：本發明抗氧化導電銅漿附著力之百格測試分析圖。
第六圖(A)：本發明抗氧化導電銅漿之抗氧化能力分析圖(一)。
第六圖(B)：本發明抗氧化導電銅漿之抗氧化能力分析圖(二)。
本發明之目的及其結構功能上的優點，將依據以下圖面所示之結
構，配合具體實施例予以說明，俾使審查委員能對本發明有更深入且具體之瞭解；此外，藉由下述具體實施例，可進一步證明本發明可實際應用之範圍，但不意欲以任何形式限制本發明之範圍。
一、抗氧化導電銅漿的製造方法
本發明之抗氧化導電銅漿係包含70wt%~90wt%之一導電粒子，4wt%~16wt%之一黏結劑，0.5wt%~7wt%之一觸變劑，以及5wt%~25wt%之一溶劑。於一較佳實施例中，本發明抗氧化導電銅漿含有80-90wt%之一導電粒子，4wt%~16wt%之一黏結劑，0.5wt%~7wt%之一觸變劑以及5wt%~15wt%之溶劑。
其中，導電粒子為為一奈米銅粒子，一次微米銅粒子與一微米銅粒子其中至少之一者，且粒徑係介於50nm~3000nm；黏結劑包含一有機樹脂與一無機化合物，有機樹脂包含一纖維素醚、一酚醛樹脂與一酚醛環氧樹脂其中至少之一者，且該無機化合物係為二氧化矽(SiO2)或氧化錫(SnO2)，其中有機樹脂與無機化合物之比例係介於1：0.1~1：10之間；觸變劑包含一聚醯胺蠟類或一氧化聚乙烯蠟；溶劑包含二乙二醇丁醚、松油醇與2,2,4-三甲基-1,3戊二醇單異丁酸酯其中至少之一者。
請參見第一圖，本案抗氧化導電銅漿的製造方法為：步驟一(S1)，將一黏結劑，一觸變劑與一乙醇混合均勻，以獲得一第一混合液，其中該黏結劑係包含一有機樹脂與一無機化合物；步驟二(S2)，將一溶劑加入該第一混合液，混合均勻後以獲得一第二混合液；步驟三(S3)，將一導電粒子加入該第二混合液，混合均勻以獲得一導電銅漿前驅液，其中該導電粒子為一奈米銅粒子，一
次微米銅粒子或一微米銅粒子；以及步驟四(S4)，移除該導電銅漿前驅液之乙醇，以獲得該抗氧化導電銅漿。其中，步驟一所使用之乙醇為無水乙醇。
黏結劑為本發明抗氧化導電銅漿的黏度來源，於導電漿體或導電膠體的製備上，即利用黏結劑之黏結作用將導電粒子結合在一起，以形成導電通路，本發明使用的黏結劑包含有機樹脂與無機化合物，其中的有機樹脂包含纖維素醚、酚醛樹脂與酚醛環氧樹脂其中至少之一者。
纖維素醚為纖維素製成、具有醚結構的高分子化合物，可為陰離子型、陽離子型和非離子型纖維素醚，且纖維素醚具有熱塑性，可作為增稠劑、分散劑等等，可為甲基纖維素、羧甲基纖維素、乙基纖維素、苄基纖維素、羥乙基纖維素、羥丙基甲基纖維素、氰乙基纖維素、苄基氰乙基纖維素、羧甲基羥乙基纖維素和苯基纖維素其中至少之一。
酚醛樹脂具有良好的耐熱性、耐燃性與耐水性，且具有高黏結強度，包含了熱固性酚醛樹脂或熱塑性酚醛樹脂。酚醛環氧樹脂的環氧基含量高，具有較大的黏度，且固化之後產物的交聯密度高，可為苯酚型酚醛環氧樹脂、鄰甲酚型酚醛環氧樹脂或是雙酚A型酚醛環氧樹脂。
本發明黏結劑中的無機化合物為二氧化矽(SiO2)或氧化錫(SnO2)；二氧化矽或氧化錫與多種材料基板之間具有穩定且高強度的鍵結或連結性，可提高本發明附著於不同基板上的附著性；此外二氧化矽或氧化錫，亦可提高本發明製成的導電薄膜的機械強度與
拉伸強度，且降低本發明製成之導電薄膜的膨脹係數，使導電薄膜更具有金屬性質，以提高其穩定性及導電性。
觸變劑是一種令溶液具有觸變現象的助劑，觸變劑可以與纖維素醚或是樹脂一起使用，能使樹脂膠液在靜止時具有較大的黏度，但是在外力作用下，例如於攪拌樹脂膠液或是將樹脂膠液塗佈於一基質上時，觸變劑會受到外力的剪切作用而降低其黏度，使樹脂膠液變稀而易於攪拌或是易於塗佈；而當攪拌完成或是塗佈完成後，觸變劑的黏度又會回復以使樹脂膠液變稠而降低其流動性，並避免樹脂膠液任意流淌。
本發明使用的觸變劑包含一聚醯胺蠟類或一氧化聚乙烯蠟。聚醯胺蠟類具有高觸變及高抗流掛性，觸變行為較大，於低剪切力時黏度高，高剪切力時黏度低，適用範圍廣。氧化聚乙烯蠟為一種具有極性的蠟，亦具有觸變特性。
又，本案抗氧化導電銅膠中含有高比例的銅粒子，為了避免製備時使用水分作為溶劑而導致銅粒子的氧化而降低導電性，因此本案使用的溶劑選用不含水分之二乙二醇丁醚、松油醇與2,2,4-三甲基-1,3戊二醇單異丁酸酯其中至少之一者；本案選用之溶劑亦具有隔絕空氣的效果，以降低本發明使用的導電銅粒子氧化。
於本發明之一實際實施例中，先將50g黏結劑、10mL觸變劑與200mL之無水乙醇，於室溫中混合均勻，以獲得一第一混合液，其中黏結劑包含30g之纖維素醚和酚醛環氧樹脂與20g之二氧化矽，且觸變劑為聚醯胺蠟類；接著，將30g之二乙二醇丁醚加入第一混合液中，於室溫下混勻以獲得第二混合液；再將200g之銅粒子加入第二混合液中混合均勻，例如以一均質刀具進行混合步驟，以
獲得一導電銅漿前驅液，此實施例中所使用之銅粒子的粒徑為300nm~1μm；最後，再去除導電銅漿前驅液所含有的乙醇，以獲得抗氧化導電銅漿，並將此實施例所獲得的抗氧化導電銅漿命名為樣品一；最後可再使用一滾輪分散本發明之抗氧化導電銅漿，以移除其內部氣泡，以利後續使用。
請參見第二圖，為本發明樣品一的抗氧化導電銅漿於固化後的掃描式電子顯微鏡分析圖，第二圖(A)為放大5000倍觀察照片，且第二圖(B)為放大10000倍之觀察照片。根據第二圖之照片，本發明之抗氧化導電銅漿組成均勻，分散性佳，且經熱固化後，導電銅粒子會熔融為一體，以使本發明固化後具有良好的導電性；此外，本發明之抗氧化導電銅漿熱固化之後製成的導電薄膜具有不易氧化的優點，將製成的導電薄膜，例如一電極，經過85℃之高溫與85%高濕度處理至少2000小時後，其整體特性仍未有明顯改變。
二、以印刷方式將本發明抗氧化導電銅漿製備成導電薄膜
本發明之抗氧化導電銅漿可用於製備導電薄膜，且可藉由一印刷流程、將本發明抗氧化導電銅漿塗佈於一基板後，再經一加熱固化步驟，以形成覆有導電薄膜的印刷基板，所使用的印刷流程可包含網版印刷、塗佈印刷、浸塗印刷、噴塗印刷與噴墨印刷其中至少之一；所使用的基板可包含玻璃基板、ITO玻璃基板、可撓性聚醯亞胺基板(PI基板)、異質PI基板(MPI)、聚對苯二甲酸乙二醇酯基板(PET基板)、化鎳鍍金基板、美拉基板(Mylar基板)、矽基板、銅箔基板、銅箔軟板、玻璃纖維板FR4、液晶高分子(LCP)板材或陶瓷基板。
以網版印刷將本發明抗氧化導電銅漿塗佈於基板以製備導電薄膜時，所使用的網版的網目數可介於32網目(mesh)至520網目之間，且將抗氧化導電銅漿塗佈於基板上後，使塗佈有抗氧化導電銅漿的基板於140~850℃作用5~120分鐘，以完成一加熱固化步驟，並使本發明抗氧化導電銅漿附著於基板上，製得一覆有導電薄膜的印刷基板(後稱為導電薄膜印刷基板)。
於一網版印刷之實施例中，係取少量上述樣品一的抗氧化導電銅漿，放置於網目數為325網目、張力27~28NT的網版上，並將抗氧化導電銅漿網印於一玻璃纖維板FR4上，再進行加熱固化步驟，以使抗氧化導電銅漿固化於玻璃纖維板FR4上，此實施例中，加熱固化步驟的作用溫度為180℃，作用時間為40分鐘。請參見第三圖(A)，為本發明抗氧化導電銅漿於玻璃纖維板FR4上印刷成電路板的實施例示意圖。此外，本發明亦可應用於製備太陽能電池的電極板，請再參見第三圖(B)，即為將本發明抗氧化導電銅漿以上述加熱固化條件處理後，製成的太陽能電池電極板示意圖。
進一步，將本發明抗氧化導電銅漿，放置於網目數為500網目、張力為25NT、厚度為12μm之網版，並印刷至一玻璃纖維板FR4上，以觀察其印刷精密度；請參見第四圖(A)之光學顯微鏡照片，以及第四圖(B)之掃描式電子顯微鏡觀察照片，本發明抗氧化導電銅漿可於基板上形成線寬至少40微米(μm)、厚度約為5~10微米(μm)之線條。
三、本發明抗氧化導電銅漿之附著性測試
此實施例係利用百格測試法測試本發明抗氧化導電銅漿的附著性；先將樣品一塗佈於玻璃基板上，並以溫度200℃作用40分鐘加
熱固化處理後，以獲得一導電薄膜印刷基板，再以百格刀於導電薄膜印刷基板表面進行劃痕以使導電薄膜印刷基板表面生成複數個網格，且劃痕深度需要深及至基板處，再進行後續的百格測試，測試本發明抗氧化導電銅漿的附著力，測試方法簡述如下：把3M公司生產、型號為3M#600的工業用測試膠帶或是具有等同效力的膠紙牢牢黏住欲測試的區域，並以橡皮擦用力擦拭膠帶或膠紙，以使測試膠帶能確實的黏附於被測試區域，且使測試膠帶與被測試區域的黏附接觸程度完全一致；接著，用手抓住膠帶一端，往垂直方向(90°)迅速撕下膠帶或膠紙，並於同一位置進行兩次測試，以測試導電銅漿於基板上的附著能力。請參見第五圖，撕除膠紙後的導電薄膜印刷基板上，本發明之抗氧化導電銅漿加熱固化後的形成的導電薄膜都能完整地附著於玻璃基板上，表示本發明抗氧化導電銅漿具有良好的附著性；且經過評估，本發明抗氧化導電銅漿製備成的導電薄膜印刷基板，其附著力的ISO class≦1，且ASTM class≧5。
此外，以本發明抗氧化導電銅漿製備成的導電薄膜印刷基板，經測試，其電阻率介於10-3歐姆-公分至10-7歐姆-公分，因此本發明抗氧化導電銅漿製成之導電薄膜印刷基板具有優秀的導電能力。
四、抗氧化功效測試
取以本發明抗氧化導電銅漿製成之導電薄膜印刷基板，以高溫與高濕度條件處理至少3000小時，再測試其薄膜電阻值(sheet resistance)的變化。請參見第六圖(A)，為將樣品一於65℃、相對溼度65%之條件處理1000~6000小時，再測試不同時間處理後樣品一的薄膜電阻值；根據第六圖(A)，以65℃、相對溼度65%之條件長
時間處理後，各樣品一的薄膜電阻值仍維持穩定狀態，又此測試條件可代表樣品一在室溫環境下能維持至少25年的穩定性。又，請參見第六圖(B)，為將樣品一於85℃、相對溼度85%之條件處理500~3000小時，再測試樣品一的薄膜電阻；根據第六圖(B)，樣品一於處理後的薄膜電阻值亦相當穩定且變化不大，且此測試條件可代表樣品一能在室溫下維持至少25年的穩定性。第六圖的測試結果顯示，以本發明抗氧化導電銅漿製成的導電薄膜印刷基板，即使以高溫、高濕度處理，其導電性質仍能維持穩定狀態，表示本發明之抗氧化導電銅漿確實不易氧化且相當穩定。
本發明抗氧化導電銅漿及其製造方法與應用，與現有技術相比，含有更高比例的銅粒子，且所製得的抗氧化導電銅漿分散性佳、具有高附著力、高導電性以及不易氧化之突出功效，同時兼具了低成本與高穩定性之優點。此外，本發明之抗氧化導電銅漿亦具有良好的耐熱性質，其耐熱溫度可介於140~850℃之間。
綜上所述，本發明之抗氧化導電銅漿及其製造方法與應用，的確能藉由上述所揭露之實施例，達到所預期之使用功效，且本發明亦未曾公開於申請前，誠已完全符合專利法之規定與要求。爰依法提出發明專利之申請，懇請惠予審查，並賜准專利，則實感德便。
惟，上述所揭之圖示及說明，僅為本發明之較佳實施例，非為限定本發明之保護範圍；大凡熟悉該項技藝之人士，其所依本發明之特徵範疇，所作之其它等效變化或修飾，皆應視為不脫離本發明之設計範疇。
S1:步驟一
S2:步驟二
S3:步驟三
S4:步驟四
Claims (13)
- 一種抗氧化導電銅漿，係以70wt%~90wt%之一導電粒子，4wt%~16wt%之一黏結劑，0.5wt%~7wt%之一觸變劑，以及5wt%~25wt%之一溶劑所組成，其中該黏結劑係包含一有機樹脂與一無機化合物，且其中該導電粒子係為一奈米銅粒子，一次微米銅粒子與一微米銅粒子其中至少之一者，該觸變劑係包含一聚醯胺蠟類或一氧化聚乙烯蠟。
- 如請求項1所述之抗氧化導電銅漿，其中該導電粒子之粒徑係介於50nm~3000nm。
- 如請求項1所述之抗氧化導電銅漿，其中該有機樹脂包含一纖維素醚(cellulose ether)、一酚醛樹脂(phenol-formaldehyde resin)與一酚醛環氧樹脂(phenolic epoxy resin)其中至少之一者，且該無機化合物係為一二氧化矽(SiO2)或一氧化錫(SnO2)。
- 如請求項1所述之抗氧化導電銅漿，其中該溶劑係包含一二乙二醇丁醚(diethylene glycol monobutyl ether)、一松油醇(terpineol)與一2,2,4-三甲基-1,3戊二醇單異丁酸酯(2,2,4,-trimethyl-1,3-pentanediolmono(2-methylpropanoate))其中至少之一者。
- 一種如請求項1所述之抗氧化導電銅漿的製造方法，包含：步驟一：將一黏結劑，一觸變劑與一無水乙醇混合均勻，以獲得一第一混合液，其中該黏結劑係包含一有機樹脂與一無機化合物； 步驟二：將一溶劑加入該第一混合液，混合均勻後以獲得一第二混合液；步驟三：將一導電粒子加入該第二混合液，混合均勻以獲得一導電銅漿前驅液，其中該導電粒子為一奈米銅粒子，一次微米銅粒子與一微米銅粒子其中至少之一者；以及步驟四：移除該導電銅漿前驅液之無水乙醇，以獲得該抗氧化導電銅漿。
- 如請求項5所述之抗氧化導電銅漿的製造方法，其中該導電粒子之粒徑係介於50nm~3000nm。
- 如請求項5所述之抗氧化導電銅漿的製造方法，其中該有機樹脂包含一纖維素醚、一酚醛樹脂與一酚醛環氧樹脂其中至少之一者，且該無機化合物係為一二氧化矽(SiO2)或一氧化錫(SnO2)；其中該溶劑係包含一二乙二醇丁醚、一松油醇與一2,2,4-三甲基-1,3戊二醇單異丁酸酯其中至少之一者。
- 一種以請求項1所述之抗氧化導電銅漿製備的導電薄膜，該導電薄膜係藉由一印刷流程形成，其中該印刷流程為網版印刷、塗佈印刷、浸塗印刷、噴塗印刷或是噴墨印刷其中至少之一。
- 如請求項8所述之以抗氧化導電銅漿製備的導電薄膜，其中該抗氧化導電銅漿係藉由該印刷流程塗佈於一基板，並經一加熱固化步驟後以獲得一導電薄膜印刷基板，其中該基板為一玻璃基板、一ITO玻璃基板、 一可撓性聚醯亞胺基板(PI基板)、一異質PI基板(MPI)、聚對苯二甲酸乙二醇酯基板(PET基板)、一化鎳鍍金基板、一美拉基板(Mylar基板)、一矽基板、一銅箔基板、一銅箔軟板、一玻璃纖維板FR4、一液晶高分子(LCP)板材或一陶瓷基板。
- 如請求項9所述之以抗氧化導電銅漿製備的導電薄膜，其中該加熱固化步驟係將塗佈有該抗氧化導電銅漿之該基板於140~850℃作用5~120分鐘。
- 如請求項8所述之以抗氧化導電銅漿製備的導電薄膜，其中該網版印刷所使用之網版的網目數為32網目至520網目。
- 如請求項8所述之以抗氧化導電銅漿製備的導電薄膜，其中該網版印刷所獲得的之一網印圖案的印製厚度係為5微米(μm)至200微米(μm)，印製線寬係至少為40微米(μm)。
- 如請求項9所述之以抗氧化導電銅漿製備的導電薄膜，其中該導電薄膜印刷基板之電阻率係介於10-3歐姆-公分至10-7歐姆-公分。
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| CN108172320A (zh) | 2017-12-27 | 2018-06-15 | 南京足智人信息科技有限公司 | 一种导电铜浆 |
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