TW202233771A - 水性塗料組成物及塗裝物品 - Google Patents
水性塗料組成物及塗裝物品 Download PDFInfo
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- TW202233771A TW202233771A TW110141327A TW110141327A TW202233771A TW 202233771 A TW202233771 A TW 202233771A TW 110141327 A TW110141327 A TW 110141327A TW 110141327 A TW110141327 A TW 110141327A TW 202233771 A TW202233771 A TW 202233771A
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Abstract
本發明提供一種能夠於銅箔等金屬基材上在不產生落粉等問題之情況下進行氟樹脂被覆之水性塗料組成物。
本發明係一種水性塗料組成物,其係含有能夠熔融成型之氟樹脂粒子(A)者,且特徵在於:
進而含有黏合劑樹脂(B)、非氟系界面活性劑(C)及水(D),
上述黏合劑樹脂(B)於N
2下、10℃/分鐘之條件測得之在400℃之重量減少為55%以上,並且,該水性塗料組成物以相對於塗料組成物之固形物總量為10質量%以下之比例包含上述黏合劑樹脂(B)。
Description
本發明係關於一種水性塗料組成物及塗裝物品。
已知氟樹脂因其優異之耐熱性、耐候性、耐油性、耐溶劑性、耐化學品性及非黏著性而利用於各種用途,且具有粉末、膜等各種使用形態。近年來,氟樹脂亦作為應對高頻段頻率之印刷基板材料而廣受矚目。
專利文獻1~3中揭示有用以於金屬基材上形成氟樹脂之被覆層之水性塗料組成物。
專利文獻4中揭示有用以於金屬基材上形成氟樹脂之被覆層之塗料組成物,進而揭示向其中摻合樹脂成分。
專利文獻5中揭示有含有含氟系粉末之液狀組成物。
先前技術文獻
專利文獻
專利文獻1:國際公開1994/05729
專利文獻2:日本特開2009-1767號公報
專利文獻3:日本特開平5-301974號公報
專利文獻4:國際公開2020/071382
專利文獻5:國際公開2018/016644
[發明所欲解決之課題]
本發明之目的在於:提供一種水性塗料組成物,其能夠於銅箔等金屬基材上進行既不產生落粉等問題,亦不會在用以形成塗膜之加熱後產生著色等問題之氟樹脂被覆。
[解決課題之技術手段]
本發明係一種水性塗料組成物,其係含有能夠熔融成型之氟樹脂粒子(A)者,且特徵在於:
進而含有黏合劑樹脂(B)、非氟系界面活性劑(C)及水(D),
上述黏合劑樹脂(B)於N
2下、10℃/分鐘之條件測得之在400℃之重量減少為55%以上,並且,該水性塗料組成物以相對於塗料組成物之固形物總量為10質量%以下之比例包含上述黏合劑樹脂(B)。
上述氟樹脂粒子(A)較佳為平均粒徑為0.05~1000 μm。
上述氟樹脂粒子(A)較佳為體積基準累積50%粒徑為0.05~40 μm。
上述黏合劑樹脂(B)較佳為水中之溶解性為2質量%以上。
上述非氟系界面活性劑(C)較佳為聚矽氧系界面活性劑。
上述水性塗料組成物較佳為進而含有二醇系溶劑(E)。
上述二醇系溶劑(E)較佳為於氟樹脂粒子(A)之燒成後不會殘留。
上述水性塗料組成物較佳為進而含有無機填料(F)。
上述無機填料(F)較佳為二氧化矽(silica)。
上述無機填料(F)較佳為平均粒徑為0.1~20 μm。
上述無機填料(F)較佳為最大粒徑為10 μm以下。
上述無機填料(F)亦可為利用聚矽氧化合物進行表面處理而得者。
上述聚矽氧化合物較佳為包含選自由矽烷偶合劑及有機矽氮烷所組成之群中之至少一種。
上述無機填料(F)之水分散性較佳為30質量%以上。
本發明亦為一種塗裝物品,其特徵在於:具有藉由塗裝上述水性塗料組成物而形成之被覆層。
上述塗裝物品亦可為於金屬基材上具有藉由塗裝上述水性塗料組成物而形成之被覆層之塗裝物品。
上述塗裝物品亦可為印刷基板、基板用介電材料或積層電路基板。
[發明之效果]
根據本發明,可獲得一種水性塗料組成物,其能夠抑制落粉且形成電物性及表面物性優異之氟樹脂被覆層。
氟樹脂層之形成係藉由以下方式進行,即,將含有氟樹脂之分散液塗布於基材之表面,使液狀分散介質揮發而於基材之表面形成粉末之填充層,進而使粉末熔融或加以燒成。然而,氟樹脂本質上為非黏著性,其粉末之粒子間缺乏相互作用。因此,於形成填充層時,粉末容易脫落(落粉)。為了防止此種落粉,業界一直在研究使用黏合劑樹脂。
含有氟樹脂粒子之水性塗料組成物為了形成塗膜而於高溫進行加熱。黏合劑樹脂會因此種加熱而發生分解。於此情形時,較佳為加熱時易分解,使塗膜中之殘存量變少。其原因在於:當黏合劑樹脂殘存於塗膜中時,會因此產生著色,而成為樹脂層劣化之原因。然而,為了獲得充分之黏著性,此前一直認為需要摻合一定量以上之黏合劑樹脂。本發明係在發現較佳為減少黏合劑之摻合量,進而使用在加熱時容易分解之黏合劑樹脂之基礎上完成者。
即,本發明係在發現以下情況之基礎上完成者,即,藉由選擇具有特定物性之黏合劑樹脂(B)來使用,而獲得具有優異效果之水性塗料組成物。
具體而言,上述黏合劑樹脂(B)係具有以下效果之黏合劑樹脂:因具有適度之水溶解性而使氟樹脂粒子(A)穩定地分散於水性塗料組成物之效果,以及在使水乾燥後氟樹脂粒子(A)亦存在於被覆層而抑制氟樹脂粒子(A)之落粉之效果。進而,加熱後之塗膜中上述黏合劑樹脂(B)所殘存之量較少,因此不會成為樹脂層之劣化或著色等之原因,就該方面而言亦較佳。
上述黏合劑樹脂(B)於N
2下、10℃/分鐘之條件測得之在400℃之重量減少為55%以上。上述重量減少較佳為60%以上,更佳為65%以上。
本發明人等發現,當黏合劑樹脂之重量減少處於該範圍內時,會發揮上述效果。藉由使用加熱時之重量變化較大之樹脂,能夠抑制樹脂層之劣化或著色等之原因。
再者,於本發明中,上述重量減少係藉由在N
2下、10℃/分鐘之條件之TG/DTA測定而獲得之值。
又,上述黏合劑樹脂(B)於水中之溶解性較佳為2質量%以上,更佳為5質量%以上,進而較佳為10質量%以上。
再者,上述黏合劑樹脂(B)可未完全溶解於塗料組成物中,亦可為分散狀態。於本發明中,水中之溶解性係藉由以下方式確認,即,秤量黏合劑樹脂、水置於容器,利用輥型轉子攪拌一晩後,即便靜置10分鐘亦不產生樹脂沉澱。
作為上述黏合劑樹脂(B),只要為滿足上述物性者則無特別限定,天然物聚合物中可例舉玉米澱粉、洋菜等。合成物聚合物中可例舉聚乙烯醇、甲基纖維素、聚乙烯吡咯啶酮、羥乙基纖維素、羧甲基纖維素、羧甲基纖維素鈉鹽、聚環氧乙烷、聚丙烯酸、聚丙烯酸鈉、丙烯酸/馬來酸共聚鈉、丙烯酸/磺酸系單體共聚物鈉、聚丙烯醯胺、聚伸乙基亞胺等。較佳者可例舉聚乙烯醇、甲基纖維素、聚環氧乙烷、聚乙烯吡咯啶酮。更佳者可例舉聚乙烯醇、甲基纖維素。
上述聚乙烯醇藉由調整分子量或皂化度,能夠調整其於水中之溶解能力或重量減少量,可容易地獲得與用途或目的相吻合之樹脂,就該方面而言較佳。於使用聚乙烯醇作為黏合劑樹脂(B)之情形時,皂化度較佳為30~90%。進而,分子量較佳為1000~1000000。藉由使用處於此種範圍者,可成為滿足上述物性之黏合劑樹脂(B),就該方面而言較佳。
上述黏合劑樹脂(B)之摻合量係相對於水性塗料組成物之固形物總量為10質量%以下之比例。當超過10質量%時,存在所獲得之被覆層之耐化學品性、耐熱性等物性降低之虞。又,黏合劑樹脂(B)之含量較佳為0.3質量%以上。當未達0.3質量%時,存在抑制落粉之效果變得不充分之虞,因此不佳。
上述摻合量較佳為10質量%以下,更佳為5質量%以下。
本發明之水性塗料組成物藉由選擇具有如上所述之性質之黏合劑樹脂(B)來使用,即便減少黏合劑樹脂(B)之摻合量,亦可獲得抑制落粉之效果。因此,藉由減少摻合量,可改善摻合大量之黏合劑樹脂(B)之情形所產生之各種問題。
上述能夠熔融成型之氟樹脂粒子(A)之組成並無特別限定,例如可例舉:四氟乙烯[TFE]/六氟丙烯[HFP]共聚物[FEP]、TFE/氟烷基乙烯基醚共聚物[PFA]、TFE/HFP/氟烷基乙烯基醚共聚物[EPA]、TFE/三氟氯乙烯[CTFE]共聚物、TFE/乙烯共聚物[ETFE]、聚偏二氟乙烯[PVdF]、分子量30萬以下之四氟乙烯[LMW-PTFE]等。該等化合物可使用1種,亦可混合2種以上使用。
作為上述氟烷基乙烯基醚,例如較佳為選自由以下者所組成之群中之至少1種:
通式(110):CF
2=CF-ORf
111(式中,Rf
111表示全氟有機基)所表示之氟單體、
通式(120):CF
2=CF-OCH
2-Rf
121(式中,Rf
121為碳數1~5之全氟烷基)所表示之氟單體、
通式(130):CF
2=CFOCF
2ORf
131(式中,Rf
131為碳數1~6之直鏈或支鏈狀全氟烷基、碳數5~6之環式全氟烷基、包含1~3個氧原子之碳數2~6之直鏈或支鏈狀全氟氧烷基)所表示之氟單體、
通式(140):CF
2=CFO(CF
2CF(Y
141)O)
m(CF
2)
nF
(式中,Y
141表示氟原子或三氟甲基;m為1~4之整數;n為1~4之整數)所表示之氟單體、以及
通式(150):CF
2=CF-O-(CF
2CFY
151-O)
n-(CFY
152)
m-A
151(式中,Y
151表示氟原子、氯原子、-SO
2F基或全氟烷基;全氟烷基亦可包含醚性氧及-SO
2F基;n表示0~3之整數;n個Y
151可相同亦可不同;Y
152表示氟原子、氯原子或-SO
2F基;m表示1~5之整數;m個Y
152可相同亦可不同;A
151表示-SO
2X
151、-COZ
151或-POZ
152Z
153;X
151表示F、Cl、Br、I、-OR
151或-NR
152R
153;Z
151、Z
152及Z
153相同或不同,表示-NR
154R
155或-OR
156;R
151、R
152、R
153、R
154、R
155及R
156相同或不同,表示H、銨、鹼金屬、可包含氟原子之烷基、芳基、或含有磺醯基之基)所表示之氟單體。
於本說明書中,上述「全氟有機基」意指與碳原子鍵結之氫原子全部被取代為氟原子而成之有機基。上述全氟有機基亦可具有醚氧。
作為通式(110)所表示之氟單體,可例舉Rf
111為碳數1~10之全氟烷基之氟單體。上述全氟烷基之碳數較佳為1~5。
作為通式(110)中之全氟有機基,例如可例舉:全氟甲基、全氟乙基、全氟丙基、全氟丁基、全氟戊基、全氟己基等。
作為通式(110)所表示之氟單體,進而可例舉:上述通式(110)中,Rf
111為碳數4~9之全氟(烷氧基烷基)者;Rf
111為下述式:
(式中,m表示0或1~4之整數)所表示之基者;Rf
111為下述式:
(式中,n表示1~4之整數)所表示之基者等。
作為通式(110)所表示之氟單體,其中,較佳為
通式(160):CF
2=CF-ORf
161(式中,Rf
161表示碳數1~10之全氟烷基)所表示之氟單體。Rf
161較佳為碳數1~5之全氟烷基。
氟烷基乙烯基醚較佳為選自由通式(160)、(130)及(140)所表示之氟單體所組成之群中之至少1種。
通式(160)所表示之氟單體較佳為選自由全氟(甲基乙烯基醚)、全氟(乙基乙烯基醚)、及全氟(丙基乙烯基醚)所組成之群中之至少1種,更佳為選自由全氟(甲基乙烯基醚)、及全氟(丙基乙烯基醚)所組成之群中之至少1種。
通式(130)所表示之氟單體較佳為選自由CF
2=CFOCF
2OCF
3、CF
2=CFOCF
2OCF
2CF
3、及CF
2=CFOCF
2OCF
2CF
2OCF
3所組成之群中之至少1種。
通式(140)所表示之氟單體較佳為選自由CF
2=CFOCF
2CF(CF
3)O(CF
2)
3F、CF
2=CFO(CF
2CF(CF
3)O)
2(CF
2)
3F、及CF
2=CFO(CF
2CF(CF
3)O)
2(CF
2)
2F所組成之群中之至少1種。
通式(150)所表示之氟單體較佳為選自由CF
2=CFOCF
2CF
2SO
2F、CF
2=CFOCF
2CF(CF
3)OCF
2CF
2SO
2F、CF
2=CFOCF
2CF(CF
2CF
2SO
2F)OCF
2CF
2SO
2F及CF
2=CFOCF
2CF(SO
2F)
2所組成之群中之至少1種。
於本說明書中,「有機基」意指含有1個以上碳原子之基或者從有機化合物中去除1個氫原子所形成之基。
該「有機基」之例包含:
可具有1個以上取代基之烷基、
可具有1個以上取代基之烯基、
可具有1個以上取代基之炔基、
可具有1個以上取代基之環烷基、
可具有1個以上取代基之環烯基、
可具有1個以上取代基之環烷二烯基、
可具有1個以上取代基之芳基、
可具有1個以上取代基之芳烷基、
可具有1個以上取代基之非芳香族雜環基、
可具有1個以上取代基之雜芳基、
氰基、甲醯基、RaO-、RaCO-、RaSO
2-、RaCOO-、RaNRaCO-、RaCONRa-、RaOCO-、RaOSO
2-、及RaNRbSO
2-
(該等式中,Ra獨立地為
可具有1個以上取代基之烷基、
可具有1個以上取代基之烯基、
可具有1個以上取代基之炔基、
可具有1個以上取代基之環烷基、
可具有1個以上取代基之環烯基、
可具有1個以上取代基之環烷二烯基、
可具有1個以上取代基之芳基、
可具有1個以上取代基之芳烷基、
可具有1個以上取代基之非芳香族雜環基、或
可具有1個以上取代基之雜芳基、
Rb獨立地為H或可具有1個以上取代基之烷基)。
上述有機基較佳為可具有1個以上取代基之烷基。
就非黏著性、表面平滑性之方面而言,上述氟樹脂粒子(A)較佳為FEP、PFA或EPA,PFA之熔點為300℃以上,焊料加工時不會變形,因此特佳為PFA。
上述氟樹脂粒子(A)之平均粒徑較佳為0.05~1000 μm,更佳為0.1~100 μm,進而較佳為0.1~30 μm。當平均粒徑處於上述範圍內時,可獲得膜薄且平滑之樹脂被覆層,故較佳。
上述平均粒徑例如係利用雷射繞射散射法所測得之體積平均粒徑。為了使上述氟樹脂粒子(A)成為所需之粒徑,亦可利用篩或風力進行分級。
上述氟樹脂粒子(A)之體積基準累積50%粒徑較佳為0.05~40 μm,更佳為7~40 μm。上述體積基準累積50%粒徑係利用雷射繞射散射法測定粒度分布,將粒子集群之整體體積設為100%,求出累積曲線,於該累積曲線上累積體積成為50%之點的粒徑。當上述體積基準累積50%粒徑處於上述範圍內時,可形成膜薄且平滑之被覆樹脂層,故較佳。
上述氟樹脂粒子(A)之製造方法並無特別限定,具體而言,例如可利用日本特開2009-1767號公報中所記載之方法等進行製造。
構成上述氟樹脂粒子(A)之氟樹脂之聚合方法並無特別限制,可例舉塊狀聚合、懸浮聚合、溶液聚合、乳化聚合等。於上述聚合中,溫度、壓力等各條件、聚合起始劑或其他添加劑可根據所需之氟樹脂之組成或量來適當地進行設定。
上述水性塗料組成物中之氟樹脂粒子(A)之摻合量為全部組成物質量之10~80質量%,較佳為15~75質量%,更佳為20~50質量%。當氟樹脂粒子(A)之摻合量少於上述下限時,黏度過低,即便塗裝於物品表面亦立即產生垂流,又,亦無法厚塗。另一方面,當氟樹脂粒子(A)之摻合量過多時,塗料組成物不具有流動性,無法塗裝。具體之摻合量則考慮塗裝方法或膜厚之調整等而於上述範圍內適當選定即可,於噴霧塗裝等之情形時較佳為設為相對較低之濃度,另一方面,於壓抵塗裝等之情形時較佳為設為成為糊狀之50質量%以上。
於本發明中,水性塗料組成物之固形物成分濃度係利用加熱殘存質量測定法進行測定。
本發明之水性塗料組成物進而含有非氟系界面活性劑(C)。考慮到成本方面,本發明之水性塗料組成物含有非氟系界面活性劑而不是氟系界面活性劑,此亦為本發明之水性塗料組成物較佳之原因之一。
作為上述非氟系界面活性劑(C),只要為能夠使氟樹脂粒子(A)穩定地分散於組成物中者,則無特別限定,可使用陰離子性界面活性劑、陽離子性界面活性劑、非離子性界面活性劑、兩性界面活性劑中之任一者。例如可例舉:烷基硫酸鈉、烷基醚硫酸鈉、烷基硫酸三乙醇胺、烷基醚硫酸三乙醇胺、烷基硫酸銨、烷基醚硫酸銨、烷基醚磷酸鈉、氟烷基羧酸鈉等陰離子性界面活性劑;烷基銨鹽、烷基苄基銨鹽等陽離子性界面活性劑;聚氧乙烯烷基醚、聚氧乙烯苯基醚、聚氧乙烯烷基酯、丙二醇-環氧丙烷共聚物、全氟烷基環氧乙烷加成物、2-乙基己醇環氧乙烷加成物等非離子性界面活性劑;烷基胺基乙酸甜菜鹼、烷基醯胺基乙酸甜菜鹼、咪唑鎓甜菜鹼等兩性界面活性劑等。其中,較佳為陰離子性及非離子性界面活性劑。特佳之界面活性劑係具有熱分解餘量較少之氧乙烯鏈之非離子性界面活性劑。
上述非氟系界面活性劑(C)亦可使用烴系界面活性劑、聚矽氧系界面活性劑、乙炔二醇等乙炔系界面活性劑等。又,可使用該等非氟系界面活性劑中之一種,或亦可將2種以上組合而使用。再者,較佳為不使用壬基苯酚系界面活性劑。
作為上述非氟系界面活性劑(C),尤佳為聚矽氧系界面活性劑。上述聚矽氧系界面活性劑並無特別限定,例如可例舉聚氧乙烯(POE)改質有機聚矽氧、聚氧乙烯-聚氧丙烯(POE-POP)改質有機聚矽氧、POE山梨醇酐改質有機聚矽氧、POE甘油基改質有機聚矽氧等經親水基改質之有機聚矽氧等。
作為具體例,可例舉:DBE-712、DBE-821(AZmax公司製造);KP系列、KF-6015、KF-6016、KF-6017、KF-6028(信越化學工業公司製造);ABIL-EM97(Goldschmidt公司製造);Polyflow KL-100、Polyflow KL-401、Polyflow KL-402、Polyflow KL-700(共榮社化學製造);「FZ-77」(Dow Corning Toray股份有限公司製造);「BYK-333」(BYK-Chemie Japan股份有限公司製造)等。
關於上述非氟系界面活性劑(C)之摻合量,相對於上述氟樹脂粒子(A)100質量%,較佳為0.01~50質量%,較佳為0.1~30質量%,更佳為0.2~20質量%。當界面活性劑之添加量過少時,氟樹脂粒子之分散變得不均勻,有時一部分會浮起。另一方面,當界面活性劑之添加量過多時,由燒成而產生之界面活性劑之分解殘渣變多,產生著色,此外,被覆膜之耐熱性、非黏著性等亦會降低。
本發明之水性塗料組成物係含有水(D)作為溶劑者。因介質為水,故就對環境造成之不良影響較少之方面而言較佳。
進而,本發明之水性塗料組成物較佳為與水併用而含有水溶性溶劑。上述水溶性溶劑具有使上述氟樹脂粒子(A)潤濕之作用,進而高沸點者於塗裝後進行乾燥時作為將樹脂彼此連結以防止龜裂產生之乾燥延遲劑而發揮作用。即便為高沸點溶劑亦會於氟樹脂之燒成溫度蒸發,因此不會對被覆膜造成不良影響。
關於上述水溶性溶劑之具體例,作為沸點至高為100℃之低沸點有機溶劑,可例舉甲醇、乙醇、異丙醇、第二丁醇、第三丁醇、丙酮、甲基乙基酮等;作為沸點為100~150℃之中沸點有機溶劑,可例舉甲基賽珞蘇、乙基賽珞蘇等;作為沸點為150℃以上之高沸點有機溶劑,可例舉N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺、3-丁氧基-N,N-二甲基丙醯胺、3-丁氧基-N,N-二甲基丙醯胺、N,N-二甲基甲醯胺、乙二醇、丙二醇、甘油、二甲基卡必醇、丁基二卡必醇、丁基賽珞蘇、1,4-丁二醇、二乙二醇、三乙二醇、四乙二醇等。又,該等水溶性溶劑可使用1種或將2種以上者混合而使用。上述水溶性溶劑較佳為高沸點有機溶劑,其中,就分散穩定性、安全性之方面而言,更佳為二醇系溶劑。
上述水溶性溶劑之摻合量較佳為全部水量之0.5~50質量%,更佳為1~30質量%。於低沸點有機溶劑之情形時,當摻合量過少時,會容易發生起泡等情況,當過多時,組成物整體具有易燃性,會損害水性分散組成物之優點。於中沸點有機溶劑之情形時,當摻合量過多時,有時亦於燒成後在被覆膜中殘留而造成不良影響,當過少時,於塗布後進行乾燥時氟樹脂會變回粉末而無法燒成。於高沸點有機溶劑之情形時,當摻合量過多時,有時亦於燒成後在被覆膜中殘留而造成不良影響。上述水溶性溶劑較佳為藉由選擇具有易揮發之性質者或調整摻合量等,從而在上述氟樹脂粒子(A)之燒成後亦不會殘留於被覆膜中。再者,二醇系溶劑於氟樹脂粒子(A)之燒成後未殘留可藉由削掉燒成後之塗膜,利用TG/DTA測定來檢測二醇系溶劑之沸點附近無重量減少來確認。
為了提高電特性、強度、耐熱性等,本發明之水性塗料組成物較佳為進而含有無機填料(F)。無機填料(F)並無特別限定,例如可例舉:二氧化矽(更具體而言為晶質二氧化矽、熔融二氧化矽、球狀熔融二氧化矽等)、氧化鈦、氧化鋯、氧化鋅、氧化錫、氮化矽、碳化矽、氮化硼、碳酸鈣、矽酸鈣、鈦酸鉀、氮化鋁、氧化銦、氧化鋁、氧化銻、氧化鈰、氧化鎂、氧化鐵、摻錫氧化銦(ITO)等無機化合物。又,可例舉蒙脫石、滑石、雲母、軟水鋁石、高嶺土、膨潤石、硬矽鈣石、蛭石、絹雲母等礦物。作為其他填料,亦可例舉:碳黑、乙炔黑、科琴黑(Ketjenblack)、奈米碳管等碳化合物;氫氧化鋁、氫氧化鎂等金屬氫氧化物;玻璃珠、玻璃薄片、玻璃中空球等各種玻璃等。
上述無機填料(F)可使用一種或兩種以上之無機填料。
又,無機填料(F)可直接使用粉體,亦可使用分散於樹脂中者。
上述無機填料(F)較佳為二氧化矽、氧化鋁、氧化鈦等,特佳為低比重且低介電常數之二氧化矽。藉由含有二氧化矽,可將塗膜之熱膨脹係數抑制得較低。又,藉由該作用,可抑制基板之翹曲,因此較佳。進而,亦可提高被覆層之剝離強度。
無機填料之形狀並無特別限定,例如可使用粒狀、球狀、鱗片狀、針狀、柱狀、錘狀、錐狀、多面體狀、中空狀等。尤其是球狀、立方體、缽狀、圓盤狀、八面體狀、鱗片狀、棒狀、板狀、桿狀、四角狀(tetrapod)、中空狀較佳,更佳為球狀、立方狀、八面體狀、板狀、中空狀。藉由設為鱗片狀或針狀之形狀,而使具有各向異性之填料排列,藉此可獲得更高之密接性。球狀填料因表面積較小,故可減小對氟樹脂特性之影響,又,摻合於液狀物之情形時增黏程度較小,就該方面而言較佳。
上述無機填料(F)之平均粒徑較佳為0.1~20 μm。當平均粒徑處於上述範圍內時,凝聚較少,可獲得良好之表面粗度。上述平均粒徑之下限更佳為0.1 μm,進而較佳為0.3 μm。上述平均粒徑之上限更佳為5 μm,進而較佳為2 μm。
上述平均粒徑係藉由雷射繞射散射法所測得之值。
上述無機填料(F)之最大粒徑較佳為10 μm以下。當最大粒徑為10 μm以下時,凝聚較少,分散狀態良好。進而,可使所得之塗膜之表面粗度變小。上述最大粒徑更佳為5 μm以下。最大粒徑係拍攝SEM(掃描式電子顯微鏡)照片,使用SEM用圖像解析軟體,根據隨機選擇之200個粒子之圖像資料而求出。
上述無機填料(F)亦可為進行表面處理而得者,例如可為利用聚矽氧化合物進行表面處理而得者。藉由利用上述聚矽氧化合物進行表面處理,可降低無機填料(F)之介電常數。
上述聚矽氧化合物並無特別限定,可使用先前公知之聚矽氧化合物。例如,較佳為包含選自由矽烷偶合劑及有機矽氮烷所組成之群中之至少一種。
至於上述聚矽氧化合物之表面處理量,表面處理劑對於無機填料表面之反應量較佳為每單位表面積(nm
2)為0.1~10個,更佳為0.3~7個。
上述無機填料(F)之水分散性較佳為30質量%以上。當未達30質量%時,有分散性變得不充分,水性塗料組成物之穩定性降低之虞。
上述水分散性係藉由以下方式確認,即,秤量無機填料、水置於容器,充分施加剪切使其等分散後,於停止攪拌時無機填料表面潤濕,數分鐘內不產生沉澱。
例如,上述無機填料(F)之利用BET法所測得之比表面積較佳為1.0~25.0 m
2/g,更佳為1.0~10.0 m
2/g,進而較佳為2.0~6.4 m
2/g。藉由使比表面積處於上述範圍內,膜中之無機填料之凝聚較少,塗膜面平滑,因此較佳。
上述無機填料(F)之摻合量相對於與上述氟樹脂粒子(A)之合計量100質量%,較佳為10~90質量%,更佳為30~70質量%。進而較佳為40~60質量%。
於上述水性塗料組成物中,除了上述各成分以外,亦可進而摻合例如著色顏料、穩定劑、增黏劑、分解促進劑、防鏽劑、防腐劑、消泡劑等通常添加至氟樹脂組成物中之各種添加劑。
上述水性塗料組成物可為不含著色顏料之透明塗料,視需要亦可為包含著色顏料之著色塗料。
以具有藉由塗裝上述水性塗料組成物而形成之被覆層為特徵之塗裝物品亦為本發明之一。
上述水性塗料組成物可利用通常之塗料所使用之塗裝方法進行塗裝,作為上述塗裝方法,可例舉:噴霧塗裝、輥塗裝、利用刮刀之塗裝、浸漬(浸)塗裝、含浸塗裝、旋流塗裝、淋幕平面塗裝(curtain flow coating)、利用棒式塗布機之塗布、凹版塗布法、微凹版塗布法等。
於上述塗裝之後,藉由乾燥、燒成,能夠製成本發明之塗裝物品。作為上述乾燥,只要為能夠去除水性介質之方法則無特別限定,例如可例舉視需要進行加熱,於室溫~130℃加熱5~30分鐘之方法等。上述燒成係於氟樹脂粒子之熔融溫度以上進行者,通常較佳為於200~400℃之範圍進行10~60分鐘。為了防止所塗布之金屬箔發生氧化,較佳為於不活性氣體下進行乾燥、燒成。
作為本發明之塗裝物品中之物品基材,可使用:鐵、不鏽鋼、銅、鋁、黃銅等金屬類;玻璃板、玻璃纖維之織布及不織布等玻璃製品;聚丙烯、聚甲醛、聚醯亞胺、修飾聚醯亞胺、聚醯胺醯亞胺、聚碸、聚醚碸、聚醚醚酮、液晶聚合物等通用及耐熱性樹脂之成形品以及被覆物;SBR、丁基橡膠、NBR、EPDM等通用橡膠、聚矽氧橡膠、氟橡膠等耐熱性橡膠之成形品及被覆物;天然纖維及合成纖維之織布及不織布;或將該等加以組合所形成之積層基材等。
上述物品基材亦可為經表面加工者。作為上述表面加工,可例舉:使用噴砂進行表面粗化直至達到所需粗度者、使粒子附著而進行表面粗化者、實施了金屬抗氧化處理者。
本發明之塗裝物品可於要求耐熱性、耐溶劑性、潤滑性、非黏著性等之領域中使用,可用於膜、纖維強化膜、預浸體、附樹脂金屬箔、覆金屬積層板、印刷基板、基板用介電材料、積層電路基板等。
本發明之塗裝物品特佳為於銅箔上具有藉由本發明之水性塗料組成物而形成之被覆層者。近年來,於各種領域中,高頻區域內之通訊盛行。為了減少於高頻區域使用時之傳輸損耗,正在使用積層有含有氟聚合物之介電體層與銅箔而成者。於此種用途中,本發明之水性塗料組成物可特佳地使用。
[實施例]
以下,藉由實施例對本發明進行說明。實施例中,摻合比例中之%、份只要不特別說明則意指質量%、質量份。本發明並不限定於以下所記載之實施例。
實施例1
步驟1.預粉碎(乾式粉碎)
藉由懸浮聚合製造四氟乙烯(TFE)/全氟乙烯醚(PFVE)共聚物(PFA:熔點=300℃、MFR=25 g/10分鐘),將所得之乾燥粉末直接利用空氣噴流研磨裝置(I.M.MATERIAL公司製造)進行粉碎,獲得平均粒徑10 μm之微粉末。
步驟2.預混合(預分散)
將相對於由步驟1.獲得之PFA微粉末100質量份為10質量份之乙炔二醇系分散劑(Surfynol 440,Air Products Japan公司製造)、10質量份之聚矽氧系界面活性劑(KP-106,信越化學工業公司製造)及280質量份之離子交換水與PFA微粉末充分攪拌、混合,獲得PFA分散液。
步驟3.濕式粉碎
於將由步驟2.獲得之PFA分散液利用100目金屬網過濾後,使其通過高壓乳化機(Nanomizer NMII,吉田機械興業公司製造,粉碎壓力=200 MPa),獲得平均粒徑0.20 μm(利用堀場製作所公司製造之CAPA700測得)之PFA微粉末分散液(氟樹脂粒子(A-1)分散液)。
所得之PFA微粉末之體積基準累積50%粒徑為0.20 μm。
步驟4.塗料化
相對於由步驟3.獲得之PFA微粉末分散液100質量份,添加2.5質量份之聚矽氧系界面活性劑(KP-106,信越化學工業公司製造),以聚乙烯醇成為2.7質量份之方式添加作為黏合劑樹脂之聚乙烯醇(PVA,FUJIFILM Wako Pure Chemical股份有限公司製造)10 wt%水溶液,進而,添加20質量份之離子交換水,進行塗料化。
上述聚乙烯醇之在400℃之重量減少為75.6%。又,水中之溶解性為10質量%以上。
實施例2~6
除了將各摻合成分如表1所示般進行變更以外,以與實施例1相同之方式進行塗料化。
實施例7
除了使用平均粒徑25.0 μm之PFA微粉末,省略濕式粉碎以外,以與實施例1相同之方式進行塗料化(氟樹脂粒子(A-2)分散液)。
所得之PFA微粉末之體積基準累積50%粒徑為22.9 μm。
實施例8~12
除了將各摻合成分如表1所示般進行變更以外,以與實施例1相同之方式進行塗料化。
實施例13~30、比較例1~6
除了將各摻合成分如表2、3、4所示般進行變更以外,以與實施例1相同之方式進行塗料化。再者,於摻合二氧化矽之情形時,其摻合量設為與氟樹脂質量相同之量。
除了藉由懸浮聚合來製造四氟乙烯[TFE]/六氟丙烯[HFP]共聚物(FEP)以外,以與上述PFA微粉末分散液(氟樹脂粒子(A-1)分散液)相同之方式進行操作,而獲得平均粒徑0.2 μm(利用堀場製作所公司製造之CAPA700測得)之FEP微粉末分散液(氟樹脂粒子(A-3)分散液)。
所得之FEP微粉末之體積基準累積50%粒徑為0.23 μm。
實施例31~33
除了將各摻合成分如表3所示般進行變更以外,以與實施例1相同之方式進行塗料化。再者,於摻合二氧化矽之情形時,其摻合量設為與氟樹脂質量相同之量。
以下示出所使用之成分。
MC400:FUJIFILM Wako Pure Chemical製造之甲基纖維素400
在400℃之重量減少為87.3%。又,水中之溶解性為2質量%。
GM14L:三菱化學製造之Gosenol
TM在400℃之重量減少為77.7%。又,水中之溶解性為10質量%以上。
聚丙烯酸:FUJIFILM Wako Pure Chemical製造之聚丙烯酸250,000
在400℃之重量減少為53.1%。又,水中之溶解性為10質量%以上。
二氧化矽:Admatechs製造之Admafine SC2500-SQ,平均粒徑0.5 μm,比表面積6.1 m
2/g,最大粒徑1.7 μm
針對所得之塗料組成物,基於以下基準進行評價。
按照以下方法獲得樹脂被覆層。
使用棒式塗布機(No.40)於銅箔(福田金屬箔粉工業製造之CF-V9S-SV-18)上塗布塗料。使塗布後之銅箔於130℃乾燥15分鐘,對落粉進行評價。進而,於氮氣環境、350℃燒成15分鐘,獲得塗膜。塗布厚度為30±5 μm。燒成後之塗膜並未殘留乙二醇。
(落粉)
藉由目視確認用手指撫摸之情形及用手指按壓之情形時之氟樹脂粉末之脫落。
×:發現粉末脫落。
△:發現手指上有粉末附著。
〇:未發現手指上有附著。
(不均)
藉由目視確認有無不均,以此作為表面粗度之評價。
×:有不均。
〇:無不均。
(著色)
藉由目視確認被覆層有無著色。
×:有著色。
△:有若干變色。
〇:無著色(透明或白色)。
(覆銅積層板之翹曲)
針對所得之覆銅積層體,藉由目視確認有無翹曲。
×:發現翹起。
〇:未發現翹起。
[表1]
實施例1 | 實施例2 | 實施例3 | 實施例4 | 實施例5 | 實施例6 | 實施例7 | 實施例8 | 實施例9 | 實施例10 | 實施例11 | 實施例12 | ||
A-1 | A-1 | A-1 | A-1 | A-1 | A-1 | A-2 | A-2 | A-2 | A-2 | A-2 | A-2 | ||
二氧化矽 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | 無 | |
黏合劑 | 種類 | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA |
濃度 | 10 | 5 | 2 | 1 | 0.5 | 0.3 | 10 | 5 | 2 | 1 | 0.5 | 0.3 | |
落粉 | 撫摸 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 |
用手指按壓 | 〇 | 〇 | 〇 | 〇 | 〇 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | △ | |
不均 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | |
燒成後著色 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | |
覆銅積層板之翹曲 | × | × | × | × | × | × | × | × | × | × | × | × |
[表2]
實施例13 | 實施例14 | 實施例15 | 實施例16 | 實施例17 | 實施例18 | 實施例19 | 實施例20 | 實施例21 | 實施例22 | 實施例23 | 實施例24 | ||
A-1 | A-1 | A-1 | A-1 | A-1 | A-1 | A-2 | A-2 | A-2 | A-2 | A-2 | A-2 | ||
二氧化矽 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |
黏合劑 | 種類 | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA | PVA |
濃度 | 10 | 5 | 2 | 1 | 0.5 | 0.3 | 10 | 5 | 2 | 1 | 0.5 | 0.3 | |
落粉 | 撫摸 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 |
用手指按壓 | 〇 | 〇 | 〇 | 〇 | △ | △ | 〇 | 〇 | 〇 | 〇 | △ | △ | |
不均 | 〇 | 〇 | 〇 | 〇 | 〇 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | △ | |
燒成後著色 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | △ | 〇 | 〇 | 〇 | 〇 | 〇 | |
覆銅積層板之翹曲 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 |
[表3]
實施例25 | 實施例26 | 實施例27 | 實施例28 | 實施例29 | 實施例30 | 實施例31 | 實施例32 | 實施例33 | ||
A-2 | A-2 | A-2 | A-2 | A-2 | A-2 | A-3 | A-3 | A-3 | ||
二氧化矽 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |
黏合劑 | 種類 | MC400 | MC400 | MC400 | GM14L | GM14L | GM14L | PVA | PVA | PVA |
濃度 | 1 | 0.5 | 0.3 | 1 | 0.5 | 0.3 | 1 | 0.5 | 0.3 | |
落粉 | 撫摸 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 |
用手指按壓 | 〇 | △ | △ | 〇 | 〇 | 〇 | 〇 | △ | △ | |
不均 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | △ | |
燒成後著色 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | |
覆銅積層板之翹曲 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 | 〇 |
[表4]
比較例1 | 比較例2 | 比較例3 | 比較例4 | 比較例5 | 比較例6 | ||
A-1 | A-1 | A-1 | A-1 | A-2 | A-2 | ||
二氧化矽 | 無 | 有 | 無 | 有 | 無 | 有 | |
黏合劑 | 種類 | 不摻合 | 不摻合 | 聚丙烯酸 | 聚丙烯酸 | PVA | PVA |
濃度 | 0 | 0 | 3 | 3 | 15 | 15 | |
落粉 | 撫摸 | × | × | 〇 | 〇 | 〇 | 〇 |
用手指按壓 | × | × | 〇 | 〇 | 〇 | 〇 | |
不均 | × | × | 〇 | 〇 | 〇 | 〇 | |
燒成後著色 | 〇 | 〇 | × | × | × | × | |
覆銅積層板之翹曲 | × | 〇 | × | 〇 | × | 〇 |
由表1~4之結果可知,本發明之水性塗料組成物可抑制落粉,形成無不均或無著色之良好之氟樹脂被覆層。
再者,於未摻合有二氧化矽之實施例中,在覆銅積層板之翹曲方面評價為×,但在落粉、不均、燒成後著色等性能上獲得了較佳之結果。因此,於翹曲之抑制並非特別重要之領域中,可較佳地使用不摻合二氧化矽之水性塗料組成物。另一方面,二氧化矽之摻合在進一步改善覆銅積層板之翹曲之抑制方面較佳。
[產業上之可利用性]
根據本發明,可獲得一種水性塗料組成物,其可抑制落粉,並且形成電物性及表面物性優異之被覆層。上述水性塗料組成物可較佳地用於印刷基板、基板用介電材料、積層電路基板等之塗裝。
無
無
Claims (17)
- 一種水性塗料組成物,其係含有能夠熔融成型之氟樹脂粒子(A)者,且特徵在於: 進而含有黏合劑樹脂(B)、非氟系界面活性劑(C)及水(D), 上述黏合劑樹脂(B)於N 2下、10℃/分鐘之條件測得之在400℃之重量減少為55%以上,並且,該水性塗料組成物以相對於塗料組成物之固形物總量為10質量%以下之比例包含上述黏合劑樹脂(B)。
- 如請求項1之水性塗料組成物,其中,氟樹脂粒子(A)之平均粒徑為0.05~1000 μm。
- 如請求項1或2之水性塗料組成物,其中,氟樹脂粒子(A)之體積基準累積50%粒徑為0.05~40 μm。
- 如請求項1至3中任一項之水性塗料組成物,其中,黏合劑樹脂(B)於水中之溶解性為2質量%以上。
- 如請求項1至4中任一項之水性塗料組成物,其中,非氟系界面活性劑(C)為聚矽氧系界面活性劑。
- 如請求項1至5中任一項之水性塗料組成物,其進而含有二醇系溶劑(E)。
- 如請求項6之水性塗料組成物,其中,二醇系溶劑(E)於氟樹脂粒子(A)之燒成後不會殘留。
- 如請求項1至7中任一項之水性塗料組成物,其進而含有無機填料(F)。
- 如請求項8之水性塗料組成物,其中,無機填料(F)為二氧化矽(silica)。
- 如請求項8或9之水性塗料組成物,其中,上述無機填料(F)之平均粒徑為0.1~20 μm。
- 如請求項8至10中任一項之水性塗料組成物,其中,上述無機填料(F)之最大粒徑為10 μm以下。
- 如請求項8至11中任一項之水性塗料組成物,其中,無機填料(F)係利用聚矽氧化合物進行表面處理而得者。
- 如請求項12之水性塗料組成物,其中,聚矽氧化合物包含選自由矽烷偶合劑及有機矽氮烷所組成之群中之至少一種。
- 如請求項8至13中任一項之水性塗料組成物,其中,上述無機填料(F)之水分散性為30質量%以上。
- 一種塗裝物品,其特徵在於:具有藉由塗裝請求項1至14中任一項之水性塗料組成物而形成之被覆層。
- 如請求項15之塗裝物品,其於金屬基材上具有藉由塗裝請求項1至14中任一項之水性塗料組成物而形成之被覆層。
- 如請求項15或16之塗裝物品,其係印刷基板、基板用介電材料或積層電路基板。
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