TW202402974A - 塗料組成物、絕緣材料及積層體 - Google Patents
塗料組成物、絕緣材料及積層體 Download PDFInfo
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- TW202402974A TW202402974A TW112113310A TW112113310A TW202402974A TW 202402974 A TW202402974 A TW 202402974A TW 112113310 A TW112113310 A TW 112113310A TW 112113310 A TW112113310 A TW 112113310A TW 202402974 A TW202402974 A TW 202402974A
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- 230000005484 gravity Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
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- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 239000010452 phosphate Substances 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229940080117 triethanolamine sulfate Drugs 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
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- 230000004580 weight loss Effects 0.000 description 1
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- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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Abstract
本發明提供一種塗料組成物,其為低介電且線膨脹係數較小,即便對接材之表面平滑亦具有優異之接著性,能夠形成龜裂或孔等塗膜缺陷較少之塗膜層。
本發明係一種塗料組成物,其由兩種以上氟樹脂乳劑構成,且特徵在於:
至少一種氟樹脂係每10
6個主鏈碳數之官能基數為30~1000個之氟樹脂(I),上述塗料組成物進而含有各向異性填料、界面活性劑、及液體介質。
Description
本發明係關於一種塗料組成物、絕緣材料及積層體。
電路基板中,廣泛使用環氧樹脂或聚醯亞胺樹脂作為絕緣層。近年來,關於數十吉赫等級之高頻範圍之用途中所使用之高頻電路基板,基於介電特性或吸濕性之觀點,提出有數個於銅箔上形成氟樹脂之絕緣層之構成。
專利文獻1中揭示有一種分散液,其包含:含有基於全氟(烷基乙烯基醚)之單元或基於六氟丙烯之單元之四氟乙烯系聚合物之粉末、莫氏硬度為4以下之各向異性填料、及液態分散介質。
專利文獻2中記載有一種液態組成物,其特徵在於包含液體介質及分散於該液體介質之具有特定粒徑之樹脂粉末,且包含聚四氟乙烯之粉末、或無機質填料。
專利文獻3中揭示有一種氟樹脂組成物,其含有能夠熔融成形之氟樹脂、及球狀二氧化矽。
專利文獻4中揭示有一種介電體用樹脂組成物,其包含「分散於熱塑性樹脂及/或熱固性樹脂中之無機物質」,上述無機物質包含板狀無機粒子,該無機粒子具有選自由六方晶氮化硼、氧化鋁、滑石、及雲母所組成之群中之材料。
[先前技術文獻]
[專利文獻]
專利文獻1:國際公開第2021/112164號
專利文獻2:日本特開2021-121675號公報
專利文獻3:國際公開第2020/145133號
專利文獻4:日本特開2015-40296號公報
[發明所欲解決之課題]
本發明之目的在於提供一種塗料組成物,其為低介電且線膨脹係數較小,即便對接材之表面平滑亦具有優異之接著性,且能夠形成龜裂或孔等塗膜缺陷較少之塗膜層。
[解決課題之技術手段]
本發明係關於一種塗料組成物,其由兩種以上氟樹脂分散體構成者,其特徵在於:
至少一種氟樹脂係每10
6個主鏈碳數之官能基數為30~1000個之氟樹脂(I),且
上述塗料組成物進而含有各向異性填料、界面活性劑、及液體介質。
上述氟樹脂(I)中所含之官能基較佳為含羰基之基。
上述含羰基之基較佳為選自由羰基醯胺基、羧基、氟化醯基、及甲氧基羰基所組成之群中之至少一種基。
上述氟樹脂(I)中所含之官能基較佳為位於聚合物主鏈之末端。
上述氟樹脂(I)較佳為四氟乙烯-六氟丙烯共聚物(FEP)或四氟乙烯-全氟烷基乙烯基醚共聚物(PFA)。
於上述塗料組成物中,至少一種氟樹脂較佳為每10
6個主鏈碳數之官能基未達30個之氟樹脂(II)。
上述氟樹脂(II)較佳為PTFE。
上述PTFE之平均粒徑較佳為0.1~0.5 μm。
於上述塗料組成物中,上述PTFE之含量較佳為相對於氟樹脂總量為50質量%以上。
上述氟樹脂之平均粒徑較佳為各向異性填料之平均粒徑的1/5以下。
上述氟樹脂之平均粒徑較佳為未達0.3 μm。
上述各向異性填料較佳為氮化硼或滑石。
上述各向異性填料之長寬比較佳為15以上。
於上述塗料組成物中,上述各向異性填料與氟樹脂之合計量之質量比較佳為5:95~60:40。
上述界面活性劑較佳為非氟系界面活性劑。
上述液體介質較佳為包含水。
本發明亦為一種電路基板之絕緣材料,其由上述塗料組成物構成。
本發明亦為一種積層體,其特徵在於:具有藉由將上述塗料組成物塗裝於基材上所形成之塗膜層。
上述基材可為金屬材料。
上述金屬材料之塗膜層側之面的表面粗糙度Rz可為2.0 μm以下。
上述金屬較佳為銅。
上述積層體較佳為印刷基板、基板用介電材料、或積層電路基板。
[發明之效果]
本發明之塗料組成物由於為低介電且線膨脹係數較低,即便對接材之表面平滑亦具有優異之接著性,進而亦可獲得與Rz為2.0 μm以下之銅箔之良好之接著性,亦可降低導體損耗,故而可提供低傳輸損耗之電路基板。
以下對本發明進行說明。
本發明之塗料組成物係下述塗料組成物,即,由兩種以上氟樹脂分散體構成,且至少一種氟樹脂係每10
6個主鏈碳數之官能基數為30~1000個之氟樹脂(I),上述塗料組成物進而含有各向異性填料、界面活性劑、及液體介質。
例如,專利文獻1及2中所例舉之習知之含氟塗料組成物係將乾燥而製成粉末狀之氟樹脂分散於液體介質中,進而摻合填料及界面活性劑而成者。
另一方面,本發明係以聚合結束時之乳劑之形式、或以濃縮了聚合結束時之乳劑之形式使用氟樹脂。即,本發明之特徵在於:並非以粉體之形式自聚合結束時之乳劑取出氟樹脂,而是以分散狀態直接加以使用。本發明係作為液體之氟樹脂成為微粒並分散、懸浮於作為液體之分散介質中。
藉由以如上述之乳劑之形式使用氟樹脂,可穩定地摻合尤其是粒徑較小之氟樹脂微粒子。因此,可獲得能夠緻密地含有氟樹脂粒子,且於線膨脹性、介電特性等方面具有良好性質之含氟樹脂之塗料組成物。
進而,藉由塗裝該塗料組成物所形成之塗膜層顯示出塗膜缺陷較少之良好表面外觀。
又,由於不需要將氟樹脂進行乾燥而製成粉末狀之步驟,故基於減少步驟數之觀點而言亦較佳。上述氟樹脂之聚合並無特別限定,可例舉:溶液聚合、懸濁聚合、乳化聚合等。
(氟樹脂(I))
上述塗料組成物含有兩種以上包含氟樹脂之乳劑。上述氟樹脂中,至少一種氟樹脂係每10
6個主鏈碳數之官能基數為30~1000個之氟樹脂(I)。
再者,此處之官能基係指與被接著物表面之間產生相互作用,而有助於提高接著性之官能基。具體而言,較佳為下述表1所示之官能基。
上述官能基數之下限更佳為50個,進而較佳為100個。又,上述官能基數之上限更佳為800個,進而較佳為500個。
上述官能基之種類之鑑定及官能基數之測定可使用紅外分光分析法進行。
上述官能基數可根據單獨氟樹脂之水性分散液進行分析,亦可將作為目標之氟樹脂自塗料中單離來進行分析。
官能基數具體而言,藉由以下方法進行測定。首先,使用上述氟樹脂粉末及KBr製作錠劑,藉由傅立葉變換紅外分光分析對該錠劑進行分析,獲得上述氟樹脂之紅外吸收光譜,從而獲得與完全氟化而不存在官能基之基礎光譜之差光譜。根據該差光譜中出現之特定之官能基之吸收峰,按照下述式(A)而算出上述氟樹脂中每1×10
6個碳原子之官能基數N。
N=I×K/t (A)
I:吸光度
K:修正係數
t:膜之厚度(mm)
作為參考,針對本發明中之官能基,將吸收頻率、莫耳吸光係數、及修正係數於表1示出。又,莫耳吸光係數係根據低分子模型化合物之FT-IR測定資料而確定者。
[表1]
官能基 | 吸收頻率 (cm -1) | 莫耳吸光係數 (l/cm/mol) | 修正係數 | 模型化合物 |
-COF | 1883 | 600 | 388 | C 7F 15COF |
-COOH游離(free) | 1815 | 530 | 439 | H(CF 2) 6COOH |
-COOH鍵(bonded) | 1779 | 530 | 439 | H(CF 2) 6COOH |
-COOCH 3 | 1795 | 680 | 342 | C 7F 15COOCH 3 |
-CONH 2 | 3436 | 506 | 460 | C 7H 15CONH 2 |
-CH 2OH、-OH | 3648 | 104 | 2236 | C 7H 15CH 2OH |
-CF 2H | 3020 | 8.8 | 26485 | H(CF 2CF 2) 3CH 2OH |
-CF=CF 2 | 1795 | 635 | 366 | CF 2=CF 2 |
再者,-CH
2CF
2H、-CH
2COF、-CH
2COOH、CH
2COOCH
3、及-CH
2CONH
2之吸收頻率分別較表中所示之-CF
2H、-COF、-COOH游離(free)與-COOH鍵(bonded)、-COOCH
3、-CONH
2之吸收頻率低數十k數(kayser,cm
-1)。
因此,例如,-COF之官能基數係根據由來自-CF
2COF之吸收頻率1883 cm
-1之吸收峰求出之官能基數、及由來自-CH
2COF之吸收頻率1840 cm
-1之吸收峰所求出之官能基數的合計。
上述官能基係存在於氟樹脂(I)之主鏈末端或側鏈末端之官能基、及存在於主鏈中或側鏈中之官能基。於本發明中,上述官能基較佳為位於聚合物主鏈之末端。藉由使聚合物末端具有官能基,可高效率地提高接著性。
上述官能基數可為-CF=CF
2、-CF
2H、-COF、-COOH、-COOCH
3、-CONH
2、及CH
2OH之合計數。
於本發明中,上述官能基較佳為含羰基之基,其中更佳為選自由羰基醯胺基、羧基、氟化醯基、及甲氧基羰基所組成之群中之至少一種基。基於賦予接著性之觀點而言,尤佳為羧基、羰基醯胺基。
上述官能基例如藉由製造氟樹脂時所使用之鏈轉移劑或聚合起始劑而導入至氟樹脂中。例如,於使用醇作為鏈轉移劑,或使用具有-CH
2OH結構之過氧化物作為聚合起始劑之情形時,-CH
2OH被導入氟樹脂之主鏈末端。又,亦可藉由使具有官能基之單體聚合而將上述官能基導入至氟樹脂中。
上述官能基較佳為藉由製造氟樹脂時所使用之鏈轉移劑或聚合起始劑而被導入至氟樹脂末端。當設為此種結構時,接著性變得更為良好,就該方面而言較佳。
關於上述官能基,亦可為使藉由製造氟樹脂時所使用之鏈轉移劑或聚合起始劑而導入至氟樹脂末端之官能基進而進行反應而轉化為其他結構者。又,有對氟樹脂之粉末實施電暈處理,而於主鏈末端生成官能基之方法。
上述氟樹脂(I)之熔點較佳為190~350℃。上述熔點更佳為200℃以上,進而較佳為220℃以上,尤佳為280℃以上,且更佳為330℃以下。上述熔點係使用示差掃描熱量計[DSC]以10℃/分鐘之速度升溫時之熔解熱曲線中與極大值對應之溫度。
作為上述氟樹脂(I),較佳為熔融加工性之氟樹脂。又,就可獲得優異之電特性而言,更佳為選自由含有四氟乙烯單元(TFE單元)及氟烷基烯丙醚或(全)氟(烷基乙烯基醚)單元(PAVE單元)之共聚物(以下稱為TFE/氟烷基烯丙醚或PAVE共聚物(或PFA))、及含有TFE單元及六氟丙烯單元(HFP單元)之共聚物(以下稱為TFE/HFP共聚物(或FEP))所組成之群中之至少一種共聚物。其中,就能夠賦予更優異之接著性之方面而言,尤佳為包含TFE/HFP共聚物(FEP)。
作為上述氟樹脂(I),亦可併用兩種以上氟樹脂。
(全)氟(烷基乙烯基醚)(PAVE)可為氟烷基乙烯基醚,亦可為全氟(烷基乙烯基醚)。於本發明中,「全氟(烷基乙烯基醚)」係指不含C-H鍵之烷基乙烯基醚。
作為構成上述PAVE單元之PAVE,可例舉選自由下述通式(1)所表示之單體及下述通式(2)所表示之單體所組成之群中之至少一種:
CF
2=CFO(CF
2CFY
1O)
p-(CF
2CF
2CF
2O)
q-R
f(1)
(式中,Y
1表示F或CF
3,R
f表示碳數1~5之全氟烷基;p表示0~5之整數,q表示0~5之整數)
CFX=CXOCF
2OR
1(2)
(式中,X相同或不同,表示H、F、或CF
3,R
1表示直鏈或支鏈之可包含1~2個選自由H、Cl、Br、及I所組成之群中之至少一種原子之碳數為1~6之氟烷基、或者可包含1~2個選自由H、Cl、Br及I所組成之群中之至少一種原子之碳數為5或6之環狀氟烷基)。
其中,上述PAVE較佳為通式(1)所表示之單體,更佳為選自由全氟(甲基乙烯基醚)、全氟(乙基乙烯基醚)、及全氟(丙基乙烯基醚)(PPVE)所組成之群中之至少一種,進而較佳為PPVE。
上述TFE/PAVE共聚物中之PAVE單元之含量相對於所有單體單元,較佳為1.0~10質量%,更佳為2.0質量%以上,進而較佳為3.5質量%以上,尤佳為4.0質量%以上,最佳為5.0質量%以上,且更佳為8.0質量%以下,進而較佳為7.0質量%以下,尤佳為6.5質量%以下,最佳為6.0質量%以下。再者,上述PAVE單元之量係藉由
19F-NMR法進行測定。上述TFE/PAVE共聚物可為僅由TFE單元及PAVE單元構成之共聚物。
於上述氟聚合物(I)為TFE/PAVE共聚物之情形時,熔點較佳為280~322℃,更佳為290℃以上,更佳為315℃以下。
於上述氟聚合物(I)為TFE/PAVE共聚物之情形時,玻璃轉移溫度(Tg)較佳為70~110℃,更佳為80℃以上,更佳為100℃以下。上述玻璃轉移溫度係藉由動態黏彈性測定進行測定所獲得之值。
上述TFE/HFP共聚物含有TFE單元及HFP單元。上述TFE/HFP共聚物中之TFE單元之含量相對於所有單體單元,較佳為70質量%以上,更佳為85質量%以上,較佳為99.8質量%以下,更佳為99質量%以下,進而較佳為98質量%以下。
上述TFE/HFP共聚物較佳為TFE單元與HFP單元之質量比(TFE/HFP)為70~99/1~30(質量%)。上述質量比(TFE/HFP)更佳為85~95/5~15(質量%)。
上述TFE/HFP共聚物可進而含有(全)氟(烷基乙烯基醚)(PAVE)單元。作為上述TFE/HFP共聚物中所含之PAVE單元,可例舉與上述PAVE單元相同者。上述TFE/PAVE共聚物不含HFP單元,因此於該方面與TFE/HFP/PAVE共聚物不同。
於上述TFE/HFP共聚物為包含TFE單元、HFP單元、及PAVE單元之共聚物之情形時(以下亦稱為「TFE/HFP/PAVE共聚物」),質量比(TFE/HFP/PAVE)較佳為70~99.8/0.1~25/0.1~25(質量%)。上述質量比(TFE/HFP/PAVE)更佳為75~98/1.0~15/1.0~10(質量%)。上述TFE/HFP/PAVE共聚物相對於所有單體單元,較佳為合計包含1質量%以上之HFP單元及PAVE單元。
上述TFE/HFP/PAVE共聚物較佳為HFP單元為所有單體單元之25質量%以下。HFP單元之含量更佳為20質量%以下,進而較佳為18質量%以下,尤佳為15質量%以下。又,HFP單元之含量較佳為0.1質量%以上,更佳為1質量%以上,尤佳為2質量%以上。再者,HFP單元之含量可藉由
19F-NMR法進行測定。
PAVE單元之含量更佳為20質量%以下,進而較佳為10質量%以下,尤佳為3質量%以下。又,PAVE單元之含量較佳為0.1質量%以上,更佳為1質量%以上。再者,PAVE單元之含量可藉由
19F-NMR法進行測定。
上述TFE/PAVE共聚物及上述TFE/HFP共聚物亦可進而含有其他乙烯性單體(α)單元。其他乙烯性單體(α)單元並無特別限定,只要為能夠與TFE、HFP、及PAVE共聚之單體單元即可,例如可例舉:氟乙烯(VF)、偏二氟乙烯(VdF)、三氟乙烯(TrFE)、三氟氯乙烯(CTFE)等含氟乙烯性單體;或乙烯、丙烯、烷基乙烯基醚等非氟化乙烯性單體等。其他乙烯性單體(α)單元之含量較佳為0~25質量%,更佳為0.1~25質量%。
於上述共聚物為TFE/HFP/PAVE/其他乙烯性單體(α)共聚物之情形時,質量比(TFE/HFP/PAVE/其他乙烯性單體(α))較佳為70~98/0.1~25/0.1~25/0.1~25(質量%)。上述TFE/HFP/PAVE/其他乙烯性單體(α)共聚物較佳為合計包含1質量%以上之除TFE單元以外之單體單元。
上述TFE/HFP共聚物之熔點較佳為200~322℃,更佳為超過200℃,進而較佳為220℃以上,更佳為300℃以下,進而較佳為280℃以下。
上述TFE/HFP共聚物之玻璃轉移溫度(Tg)較佳為60~110℃,更佳為65℃以上,更佳為100℃以下。上述玻璃轉移溫度係藉由動態黏彈性測定進行測定所獲得之值。
上述氟樹脂(I)例如可藉由適當混合成為其結構單元之單體或聚合起始劑等添加劑,進行乳化聚合、懸濁聚合等以往公知之方法而製造。其中,更佳為藉由乳化聚合所獲得者。
上述氟樹脂(I)較佳為於372℃、5 kg負載下測得之MFR之值處於0.5~100之範圍內。藉由設為此種範圍,而容易利用末端官能基獲得如上述之官能基量,就該方面而言較佳。
本發明之塗料組成物係併用地含有上述氟樹脂(I)及其他氟樹脂(II)者。
上述氟樹脂(II)並無特別限定,較佳為每10
6個主鏈碳數之官能基數未達30個。即,較佳為在官能基數方面上與上述氟樹脂(I)不同者。
官能基數較多之氟樹脂於密接性方面上顯示出優異性能,但另一方面,電特性、耐熱性容易變得不充分。因此,作為氟樹脂(II),較佳為組合使用電特性、耐熱性優異之氟樹脂。藉此,可形成電特性、耐熱性等塗膜物性亦優異之被覆層。
上述氟樹脂(II)並無特別限定,只要為含氟樹脂即可,可例舉聚四氟乙烯樹脂(PTFE)、PFA、FEP等。其中,尤其是PTFE尤佳。進而,PTFE為佳之原因在於:TFE之均聚物之粒子柔軟且容易貼附,故而不易產生龜裂。柔軟度之指標並無特別限定,蕭氏硬度(D標度)較佳為D65以下,更佳為D60以下,尤佳為D55以下。
又,上述PTFE較佳為平均粒徑為0.1~0.5 μm。
上述PTFE之平均粒徑係下述值,即,用水將PTFE乳劑稀釋至1000倍,將稀釋後之液1滴置於鋁箔上並使其自然乾燥,對自然乾燥後所得者拍攝SEM(掃描式電子顯微鏡)照片,使用SEM用影像分析軟體,根據隨機選擇之50個粒子之影像資料測量粒徑,算出平均而得之值。
上述PTFE之含量相對於氟樹脂總量,較佳為50質量%以上。若為50質量%以上,則賦予充分之耐熱性,且亦可獲得抑制塗膜龜裂之效果,故而較佳。上述PTFE之含量更佳為70質量%以上,較佳為95質量%以下。
作為PFA及FEP,較佳為使用具有與上述氟樹脂(I)相同之樹脂組成、且官能基數與氟樹脂(I)不同者。
上述氟樹脂(II)之聚合方法並無特別限制,可例舉:塊狀聚合、懸濁聚合、溶液聚合、乳化聚合等。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而適當設定。
上述氟樹脂(II)亦可為藉由氟化處理而製成具有上述範圍內之官能基數之上述氟樹脂。
上述氟化處理可藉由使未經氟化處理之氟樹脂與含氟化合物接觸來進行。
上述含氟化合物並無特別限定,可例舉於氟化處理條件下產生氟自由基之氟自由基源。作為上述氟自由基源,可例舉:氟(F
2)氣、CoF
3、AgF
2、UF
6、OF
2、N
2F
2、CF
3OF、氟化鹵素(例如IF
5、ClF
3)等。
上述氟氣(F
2)等氟自由基源可為濃度100%者,就操作性之方面而言,較佳為與非活性氣體混合而稀釋至5~50質量%來使用,更佳為稀釋至15~30質量%來使用。作為上述非活性氣體,可例舉氮氣、氦氣、氬氣等,就經濟性方面而言,較佳為氮氣。
上述氟化處理之條件並無特別限定,亦可使熔融狀態之氟樹脂與含氟化合物接觸,通常可於氟樹脂之熔點以下,較佳為20~220℃、更佳為100~200℃之溫度下進行。上述氟化處理一般進行1~30小時,較佳為進行5~25小時。上述氟化處理較佳為使未經氟化處理之氟樹脂與氟氣(F
2gas)接觸。
本發明之塗料組成物中所含之氟樹脂之合計含量相對於整個組成物,較佳為30~80質量%,更佳為40~70質量%。
關於本發明之塗料組成物中所含之氟樹脂之平均粒徑,由於本發明之塗料組成物中所含之氟樹脂係以聚合時之乳劑之形式摻合,故而平均粒徑小於以往之塗料組成物中所使用之粉末狀氟樹脂。具體而言,上述平均粒徑較佳為未達0.3 μm。此處,上述平均粒徑並不限定於氟樹脂(I)或氟樹脂(II),係由自塗料組成物中所含之氟樹脂粒子中隨機選擇之粒子進行測量所算出的值。
具體而言,為下述之值:用水將塗料組成物稀釋至1000倍,將稀釋後之液1滴置於鋁箔上並使其自然乾燥,對自然乾燥後所得者拍攝SEM(掃描式電子顯微鏡)照片,使用SEM用影像分析軟體,根據隨機選擇之100個粒子之影像資料測量粒徑,算出平均所得之值。
上述平均粒徑較佳為下限為0.05 μm,更佳為0.07 μm,進而較佳為0.1 μm。
又,上述氟樹脂之平均粒徑較佳為後述之各向異性填料之平均粒徑之1/5以下,更佳為1/10以下。若上述平均粒徑為1/5以下,則可緻密地填充各向異性填料之間隙,故而較佳。
(各向異性填料)
本發明之塗料組成物係含有各向異性填料者。上述各向異性填料藉由以平行於基材表面之方式配向,而即便添加量相對較少,亦容易高度地表現出各向異性填料之物性,就該方面而言較佳。進而,上述氟樹脂乳劑中所含之氟樹脂微粒子由於可緻密地填充各向異性填料之間隙,故而可獲得為低介電且線膨脹係數較低之塗料組成物。
作為上述各向異性填料,可例舉:碳填料、氮化物填料、雲母填料、黏土填料、滑石填料,較佳為包含氮化硼或滑石之填料,更佳為包含滑石之填料。
上述各向異性填料可使用一種,亦可使用平均粒徑等物性或種類不同之兩種以上。
上述各向異性填料之形狀可為粒狀、針狀(纖維狀)、板狀中之任一者。作為各向異性填料之具體形狀,可例舉:鱗片狀、層狀、單片狀、杏仁狀、柱狀、雞冠狀、等軸狀、葉狀、雲母狀、塊狀、平板狀、楔狀、玫瑰花狀、網狀、角柱狀。其中,各向異性填料之形狀較佳為鱗片狀或板狀。
當使用鱗片狀或板狀之各向異性填料時,其形成片架結構,不僅容易提高塗料組成物之液體物性(黏度、分散穩定性等),亦容易提高塗膜層中之填料之配向性,容易提高其功能(機械強度、導熱性、電特性等)。
上述各向異性填料之平均粒徑較佳為1 μm以上、20 μm以下。若平均粒徑為上述範圍內,則塗料組成物中之分散穩定性更為良好。上述平均粒徑更佳為3~10 μm。
於本發明中,各向異性填料之平均粒徑係使用粒徑分佈測定裝置HELOS&RODOS(SYMPATEC公司製造),藉由乾式雷射法所測得者。
於本說明書中,上述各向異性填料係指長寬比並非1之填料。作為本發明中使用之各向異性填料,較佳為長寬比為15以上之填料。若長寬比為15以上,則容易進一步提高塗膜層中之填料之配向性,而容易提高其功能。具體而言,不僅容易使分散液中之各向異性填料之分散狀態穩定,而且由塗料組成物成形塗膜層時之各向異性填料之配向性亦進一步提高,從而容易獲得高度具備氟樹脂之物性及各向異性填料之物性的積層體。
上述長寬比更佳為20以上,進而較佳為30以上。作為上限,較佳為100。
再者,於本說明書中,長寬比係指任意1個粒子之長徑(d
L)與短徑(d
S)之比(d
L/d
S),該長徑(d
L)係連接粒子表面上之任意兩點之直線中長度最長直線之長度,該短徑(d
S)係與該最長直線垂直之直線中長度最短直線之長度。於本說明書中,長寬比係藉由影像處理所獲得之值。
上述各向異性填料可為經表面處理所得者。藉由預先實施表面處理,可抑制各向異性填料之凝集,可使各向異性填料良好地分散於樹脂組成物中。
上述表面處理並無特別限定,可使用公知之任意者。具體而言,例如可例舉:藉由具有反應性官能基之環氧矽烷、胺基矽烷、乙烯基矽烷、丙烯基矽烷、疏水性之烷基矽烷、苯基矽烷、氟化烷基矽烷等矽烷偶合劑進行之處理、電漿處理、氟化處理等。
作為上述表面處理,較佳為藉由矽烷偶合劑進行之處理,作為矽烷偶合劑之反應性官能基,基於與樹脂基材之接著性之觀點而言,較佳為於末端具有選自胺基、(甲基)丙烯酸基、巰基、及環氧基中之至少一種。
上述各向異性填料之摻合量相對於整個組成物,較佳為0.3~5質量%,更佳為1~3質量%。
於本發明之塗料組成物中,上述各向異性填料與氟樹脂之合計量之質量比較佳為5:95~60:40,更佳為20:80~35:65。藉由使質量比處於上述範圍內,可取得線膨脹係數與成形性之平衡,就容易製成兼具該等兩者之性質之氟樹脂組成物之方面而言較佳。
本發明之塗料組成物亦可進而含有其他填料。作為上述其他填料,較佳為二氧化矽、黏土、滑石、碳酸鈣、雲母、矽藻土、氧化鋁、氧化鋅、氧化鈦、氧化鈣、氧化鎂、氧化鐵、氧化錫、氧化銻、氫氧化鈣、氫氧化鎂、氫氧化鋁、鹼性碳酸鎂、碳酸鎂、碳酸鋅、碳酸鋇、碳鈉鋁石、鋁碳酸鎂、硫酸鈣、硫酸鋇、矽酸鈣、蒙脫石、膨潤土、活性白土、海泡石、絲狀鋁英石、絹雲母、玻璃纖維、玻璃珠、矽土系氣球、碳黑、奈米碳管、奈米碳角、石墨、碳纖維、玻璃中空球、碳中空球、木粉、及硼酸鋅等。
(界面活性劑)
本發明之塗料組成物係進而含有界面活性劑者。藉由含有上述界面活性劑,從而塗料組成物之分散穩定性得到提高,且可抑制塗膜龜裂之產生。上述界面活性劑並無特別限定,就成本或穩定性之方面而言,較佳為非氟系界面活性劑。
上述非氟系界面活性劑並無特別限定,只要能夠使氟樹脂穩定地分散於組成物中即可,亦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:硫酸烷基鈉、烷基醚硫酸鈉、三乙醇胺硫酸烷基酯、三乙醇胺烷基醚硫酸鹽、硫酸烷基銨、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。尤佳之界面活性劑係熱分解殘量較少之具有氧乙烯鏈之非離子性界面活性劑。
作為上述非離子性界面活性劑之市售品,例如可例舉:以Genapol X080(製品名,Clariant公司製造)、Noigen TDS-80(商品名)、及Noigen TDS-100(商品名)為例之Noigen TDS系列(第一工業製藥公司製造);以LEOCOL TD-90(商品名)為例之LEOCOL TD系列(LION公司製造)、LIONOL(註冊商標)TD系列(LION公司製造);以T-Det A138(商品名)為例之T-Det A系列(Harcros Chemicals公司製造)、TERGITOL(註冊商標)15S系列(Dow公司製造)、DISPANOL TOC(商品名,日本油脂公司製造)等。
作為上述非氟系界面活性劑,又,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,該等非氟系界面活性劑中,可組合一種或兩種以上使用。再者,較佳為不使用壬基苯酚系界面活性劑。
上述非氟系界面活性劑之摻合量相對於上述氟樹脂之合計量100質量%,較佳為0.01~50質量%,更佳為0.1~30質量%,進而較佳為0.2~20質量%。若界面活性劑之添加量過少,則可能氟樹脂之分散會變得不均,一部分氟樹脂浮起。另一方面,若界面活性劑之添加量過多,則因焙燒產生之界面活性劑之分解殘渣增多而引起著色,此外被覆膜之耐熱性、非黏著性等降低。
(液體介質)
本發明之塗料組成物進而含有液體介質。上述液體介質並無特別限定,較佳為包含水。
進而,本發明之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潤濕上述氟樹脂之作用,進而,具有高沸點者於塗裝後之乾燥時將樹脂彼此黏合,而作為防止龜裂產生之乾燥延遲劑而發揮功能。即便係高沸點溶劑,亦會於氟樹脂之焙燒溫度下蒸發,因此不會對被覆膜產生不利影響。
作為上述水溶性溶劑之具體例,可例舉:作為沸點至多100℃之低沸點有機溶劑之甲醇、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℃之中沸點有機溶劑之甲基賽珞蘇、乙基賽珞蘇等;作為沸點為150℃以上之高沸點有機溶劑之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、二乙二醇單甲醚等。又,該等水溶性溶劑亦可混合一種或兩種以上之水溶性溶劑來使用。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、操作性之方面而言,更佳為二醇系溶劑。
作為上述二醇系溶劑,較佳為包含選自由乙二醇、二乙二醇單甲醚、甘油、及丁基卡必醇所組成之群中之至少一種。
上述水溶性溶劑之摻合量較佳為總水量之0.5~50質量%,更佳為1~30質量%。於低沸點有機溶劑之情形時,若摻合量過少,則容易引起氣泡之混入等,若過多,則使得整個組成物具有易燃性,會損害水性分散組成物之優勢。於中沸點有機溶劑之情形時,若摻合量過多,則可能於焙燒後亦會殘留於被覆膜中,而產生不良影響,若過少,則於塗佈後之乾燥時,氟樹脂會恢復成粉末,而無法焙燒。於高沸點有機溶劑之情形時,若摻合量過多,則可能於焙燒後亦殘留於被覆膜中而產生不良影響。上述水溶性溶劑較佳為藉由選擇具有易揮發性質者,或者調整摻合量等,從而即便於上述氟樹脂之焙燒後亦不會殘留於被覆膜中。再者,於氟樹脂之焙燒後不殘留二醇系溶劑之情況可藉由下述情況確認,即,刮取焙燒後之塗膜,於TG/DTA測定中,在二醇系溶劑之沸點附近不存在重量減少。
可將通常添加於氟樹脂組成物中之各種添加劑,例如穩定劑、增黏劑、分解促進劑、防銹劑、防腐劑、消泡劑等摻合於上述塗料組成物中。
上述增黏劑並無特別限定,只要增加塗料之黏度且不影響塗膜性狀即可,較佳為高級脂肪酸之非離子乳劑,因為其與氟樹脂粒子形成三維網狀結構,而使得視黏度得到提高,亦防止塗膜之龜裂。尤佳為油酸乳劑、辛酸乳劑。
本發明之一亦為一種積層體,其特徵在於,具有藉由塗裝上述塗料組成物所形成之塗膜層。
上述塗料組成物可藉由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(dip)塗裝、含浸塗裝、旋轉流塗裝、淋幕式平面塗裝、利用棒式塗佈機之塗佈、凹版塗佈法、微凹版塗佈法、模具塗佈等。
可於上述塗裝後,進行乾燥、焙燒,藉此製成本發明之積層體。上述乾燥並無特別限定,只要為能夠去除液體介質之方法即可,例如可例舉視需要進行加熱,於室溫~130℃進行5~30分鐘之方法等。上述焙燒係於氟樹脂之熔融溫度以上進行,通常較佳為於200~400℃之範圍進行10~60分鐘。為了防止塗佈後之金屬箔氧化,較佳為於非活性氣體下進行乾燥、焙燒。
使用本發明之塗料組成物所形成之塗膜之乾燥、焙燒後之厚度較佳為2~40 μm。藉由製成此種範圍內之塗膜,可容易地形成不產生塗膜狀態之問題之良好之塗膜,進而可充分發揮作為塗膜所要求之物性。上述下限更佳為3 μm,進而較佳為5 μm。上述上限更佳為35 μm,進而較佳為30 μm。
作為本發明之積層體中之物品基材,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、改良型聚醯亞胺、聚醯胺醯亞胺、聚碸、聚醚碸、聚醚醚酮、液晶聚合物等通用樹脂及耐熱性樹脂之成形品及被覆物;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;或將其等組合所形成之積層基材等。
上述物品基材可為經表面加工者。作為上述表面加工,可例舉:使用噴砂進行表面粗糙化至所需粗糙度者、使粒子附著以進行表面粗糙化者、實施金屬抗氧化處理者。
本發明之塗料組成物可提高與基材之接著性。具體而言,藉由塗裝本發明之塗料組成物所形成之塗膜層與物品基材之接著強度可設為3 N/cm以上。
上述接著強度係下述值,即,將由塗膜層及基材構成之積層體以塗膜層密接於銅箔之方式重疊,於真空下加熱溫度:320℃並以壓力:3 MPa加壓5分鐘,藉此獲得積層有由塗膜層及基材構成之積層體及銅箔之接合體,之後將接合體切割成寬度10 mm×長度40 mm×3組之短條狀,而製作試片,針對該試片,使用自動立體測圖儀(島津製作所(股)製造之AGS-J 5kN),依據JIS C 6481-1996,於25℃以50 mm/分鐘之拉伸速度進行90度剝離試驗,觀察剝離模式進行測定,將所測得之值作為接著強度。
上述接著強度更佳為5 N/cm以上。
再者,即便所使用之塗料組成物相同,上述接著強度亦會根據基材之種類產生變化,但本發明之塗料組成物即便於使用通常難以獲得剝離強度之基材之情形時,亦可獲得如上述之優異之剝離強度,就該方面而言尤佳。
更具體而言,即便物品基材為表面粗糙度較小之金屬基材,亦可獲得上述範圍之接著強度。例如於以表面粗糙度(Rz)為2.0 μm以下之銅箔作為基材之情形時,以往之含氟塗料組成物無法獲得充分之接著性,但由本發明之塗料組成物構成之塗膜層可顯示出3 N/cm以上之接著強度。
上述表面粗糙度(Rz)係JIS-B0601所規定之十點平均粗糙度。於本說明書中,上述Rz係將測定長度設為4 mm,並使用表面粗糙度計(商品名:Surfcom 470A,東京精機公司製造)所測得之值。
本發明之積層體可用於要求耐熱性、耐溶劑性、潤滑性、非黏著性等之領域,可用於膜、纖維強化膜、預浸體、附樹脂之金屬箔、金屬箔積層板、印刷基板、基板用介電材料、積層電路基板等。
本發明之積層體尤佳為於銅箔上具有藉由本發明之塗料組成物形成之塗膜層者。近年來,於各種領域中,正在流行高頻區域內之通信。為了減少於高頻區域使用時之傳輸損耗,使用使含有含氟聚合物之介電層與銅箔積層所得者。於此種用途中,本發明之塗料組成物尤其適宜使用。
[實施例]
以下,藉由實施例對本發明進行說明。於實施例中,關於摻合比率,除非另有說明,%、份係指質量%、質量份。本發明並不限定於以下所記載之實施例。
製造例1
(PTFE乳劑)
使用下述之PTFE乳劑,即,聚合物固形物成分濃度為64質量%,非離子界面活性劑濃度相對於聚四氟乙烯固形物成分為2.7質量%,平均粒徑為312 nm,標準比重為1.57,藉由上述方法測得之每10
6個主鏈碳數之官能基數為10個以下。
製造例2
(PFA-1之製備)
藉由日本專利4306072號之實施例4中所記載之方法獲得PFA之水分散體。所獲得之PFA粒子之平均粒徑為194 nm,每10
6個主鏈碳數之官能基數為143個。
製造例3
(FEP-1之製備)
藉由日本專利4306072號之實施例1中所記載之方法獲得FEP之水分散體。於FEP粒子中,於末端基包含源自起始劑之羧酸,所獲得之含官能基之FEP粒子之平均粒徑為65 nm,藉由上述方法測定官能基數,結果每10
6個主鏈碳數之官能基數為207個。
製造例4
(PFA-2之調整)
藉由懸濁聚合製造四氟乙烯(TFE)/全氟乙烯醚(PFVE)共聚物(PFA:熔點=300℃,MFR=25 g/10 min),利用空氣噴射研磨裝置(I.M. Material公司製造)將所獲得之乾燥粉末直接粉碎,從而獲得平均粒徑2.5 μm之微粉末。對於PFA微粉末100質量份,將乙炔二醇系分散劑(Surfynol 440,Air Products Japan公司製造)10質量份、非離子界面活性劑(Noigen TDS-80,第一工業製藥公司製造)10質量份、及離子交換水280質量份與PFA微粉末充分攪拌、混合,而獲得PFA分散液。所獲得之PFA粒子之每10
6個主鏈碳數之官能基數為10個以下。
製造例5
(FEP-2之製備)
對於TFE及HFP,使用聚合起始劑(二(ω-氫全氟己醯基)過氧化物),藉由懸濁聚合製造FEP(TFE/HFP=90/10莫耳比),利用空氣噴射研磨裝置(I.M. Material公司製造)將所獲得之乾燥粉末直接粉碎,從而獲得平均粒徑10 μm之微粉末。相對於所獲得之FEP微粉末100質量份,將乙炔二醇系分散劑(Surfynol 440,Air Products Japan公司製造)10質量份、聚矽氧系界面活性劑(KP-106,信越化學工業公司製造)10質量份、及離子交換水280質量份與FEP微粉末充分攪拌、混合,從而獲得FEP分散液。藉由上述方法測定所獲得之FEP粒子之官能基數,結果每10
6個主鏈碳數之官能基數為20個。
製造例6
(各向異性填料分散液之製作)
製作各向異性填料分散液,其係將各向異性填料、水、界面活性劑(LEOCOL TD-90D,烴系非離子性界面活性劑,LION SPECIALTY CHEMICALS股份有限公司製造)混合之後,使用Star Burst Labo(SUGINO MACHINE製造)使各向異性填料分散於水中而獲得。
再者,所使用之各向異性填料如下所述。滑石均為NIPPON TALC製造。氮化硼為DENKA股份有限公司製造。
又,作為比較例,使用球狀二氧化矽分散液5SQ-CW(Admatechs製造)。
[表2]
商品號 | 平均粒徑(μm) | 長寬比 | |
滑石1 | PAOG-2 | 7.0 | 45 |
滑石2 | PAOG-3 | 5.0 | 40 |
滑石3 | P-4 | 4.5 | 30 |
滑石4 | P-3 | 5.0 | 30 |
滑石5 | P-2 | 7.0 | 30 |
滑石6 | PAOG-2/P-3=50/50 | 6.0 | 30 |
滑石7 | PAOG-3/P-2=50/50 | 6.0 | 30 |
BN1 | DENKA股份有限公司 SP-3 | 4.0 | 20 |
實施例1~16、比較例1~6
以達到表3~5所示之摻合量之方式混合所獲得之各氟樹脂乳劑、各向異性填料分散液,而獲得塗料組成物。
藉由上述方法測定所獲得之塗料組成物中所含之氟樹脂之平均粒徑。再者,比較例2之塗料組成物中所含之氟樹脂之平均粒徑與所組合之氟樹脂之平均粒徑相差較大,難以於同一個畫面測定。
按照以下方法獲得塗膜層。
使用棒式塗佈機(No.30),將塗料塗佈於銅箔(福田金屬箔粉工業製造之CF-V9S-SV-18,表面粗糙度0.8 μm(Rz))上。將塗佈後之銅箔於130℃乾燥15分鐘。進而,於氮氣氛圍下以350℃焙燒15分鐘,製作膜厚25 μm之塗膜。
進而,針對所獲得之塗膜,基於以下基準進行評價。
(塗膜層之線膨脹率)
對銅箔進行蝕刻,僅取出塗膜層,藉由熱機械分析裝置(TMA/TMA7100E;Hitachi High-Tech Science股份有限公司製造)測定塗膜層之線膨脹率。再者,塗膜層之線膨脹率係於-55℃-280℃之溫度範圍內測得之值。X/Y軸方向係於拉伸模式下測定,Z軸方向係於壓縮模式下測定。
(塗膜缺陷:乾燥時之龜裂)
使用雷射顯微鏡(基恩斯公司製造),藉由5倍之物鏡觀察乾燥後之塗膜,觀察塗膜有無裂紋。
無:○
部分存在:△
整面存在:×
(塗膜缺陷:焙燒後之孔)
使用雷射顯微鏡(基恩斯公司製造),藉由5倍之物鏡觀察焙燒後之塗膜,觀察塗膜有無孔狀缺陷。
無:○
有:×
(銅箔與塗膜層間之接著強度)
關於接著強度,將由塗膜層及基材構成之積層體以塗膜層密接於銅箔之方式重疊,於加熱溫度:320℃並以壓力:3 MPa加壓5分鐘,藉此獲得積層有由塗膜層及基材構成之積層體及銅箔之接合體,之後將接合體切割成寬度10 mm×長度40 mm×3組之短條狀,製作試片,針對該試片,使用自動立體測圖儀(島津製作所(股)製造之AGS-J 5kN),依據JIS C 6481-1996,於25℃以50 mm/分鐘之拉伸速度進行剝離試驗,觀察剝離模式而測定。
3 N/cm以上:○
未達3 N/cm:×
(相對介電常數、介電損耗正切)
藉由空洞共振器(關東電子應用開發股份有限公司製造),以10 GHz進行測定,藉由Network analyzer(安捷倫科技股份有限公司製造)進行分析。
按照以下基準對介電率進行評價。
3.5以下:○
大於3.5:×
進而,按照以下基準對介電損耗正切進行評價。
0.0015以下:○
大於0.0015:×
[表3]
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 | ||
氟樹脂比率 | PTFE | 65 | 65 | 65 | 65 | 65 | 65 | 65 | 65 | 65 | 65 | 65 |
PFA-1 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 35 | 35 | |
FEP-1 | 35 | 35 | 35 | 35 | 35 | 35 | 35 | 35 | 35 | 0 | 0 | |
氟樹脂:填料 | 60:40 | 60:40 | 70:30 | 60:40 | 60:40 | 60:40 | 60:40 | 60:40 | 60:40 | 70:30 | 60:40 | |
填料種類 | 滑石1 | 滑石1 | 滑石2 | 滑石2 | 滑石3 | 滑石4 | 滑石5 | 滑石6 | 滑石7 | 滑石2 | BN1 | |
氟樹脂之平均粒徑(μm) | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.28 | 0.28 | |
線膨脹係數 | 87.7 | 82.2 | 90.0 | 63.6 | 77.6 | 70 | 72.8 | 81.6 | 86.3 | 88.2 | 95.2 | |
塗膜缺陷(乾燥時之龜裂) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |
塗膜缺陷(焙燒後之孔) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |
與銅箔之接著 | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |
介電率 | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |
介電損耗正切 | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ |
[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 | ||
氟樹脂比率 | PTFE | 65 | 65 | 65 | 100 | 0 | 0 |
FEP-1 | 35 | 0 | 0 | 0 | 100 | 0 | |
FEP-2 | 0 | 35 | 0 | 0 | 0 | 0 | |
PFA-2 | 0 | 0 | 35 | 0 | 0 | 100 | |
氟樹脂:填料 | 60:40 | 60:40 | 60:40 | 60:40 | 60:40 | 60:40 | |
填料種類 | 球狀二氧化矽 | 滑石1 | 滑石1 | 滑石1 | 滑石1 | 滑石1 | |
氟樹脂之平均粒徑(μm) | 0.20 | 無法測定 | 1.20 | 0.27 | 0.10 | 2.50 | |
線膨脹係數 | 180 | 95 | 110 | 95 | 無法測定 | 無法測定 | |
塗膜缺陷(乾燥時之龜裂) | ○ | ○ | ○ | ○ | × | × | |
塗膜缺陷(焙燒後之孔) | ○ | ○ | × | ○ | × | × | |
與銅箔之接著 | ○ | × | × | × | ○ | ○ | |
介電率 | ○ | ○ | ○ | ○ | 未測定 | ○ | |
介電損耗正切 | ○ | ○ | ○ | ○ | × | × |
本發明之塗料組成物表現出不產生塗膜缺陷且具有足以作為絕緣材料之性能者。
[產業上之可利用性]
本發明之塗料組成物可適宜地用作電路基板之絕緣材料。
無
無
Claims (22)
- 一種塗料組成物,其由兩種以上氟樹脂乳劑構成,且特徵在於: 至少一種氟樹脂係每10 6個主鏈碳數之官能基數為30~1000個之氟樹脂(I), 上述塗料組成物進而含有各向異性填料、界面活性劑、及液體介質。
- 如請求項1之塗料組成物,其中,氟樹脂(I)中所含之官能基為含羰基之基。
- 如請求項2之塗料組成物,其中,含羰基之基係選自由羰基醯胺基、羧基、氟化醯基、及甲氧羰基所組成之群中之至少一種基。
- 如請求項1至3中任一項之塗料組成物,其中,氟樹脂(I)中所含之官能基位於聚合物主鏈之末端。
- 如請求項1至4中任一項之塗料組成物,其中,氟樹脂(I)為四氟乙烯-六氟丙烯共聚物(FEP)或四氟乙烯-全氟烷基乙烯基醚共聚物(PFA)。
- 如請求項1至5中任一項之塗料組成物,其中,至少一種氟樹脂係每10 6個主鏈碳數之官能基數未達30個之氟樹脂(II)。
- 如請求項6之塗料組成物,其中,氟樹脂(II)為PTFE。
- 如請求項7之塗料組成物,其中,PTFE之平均粒徑為0.1~0.5 μm。
- 如請求項7或8之塗料組成物,其中,PTFE之含量相對於氟樹脂總量為50質量%以上。
- 如請求項1至9中任一項之塗料組成物,其中,氟樹脂之平均粒徑為各向異性填料之平均粒徑的1/5以下。
- 如請求項1至10中任一項之塗料組成物,其中,氟樹脂之平均粒徑未達0.3 μm。
- 如請求項1至11中任一項之塗料組成物,其中,各向異性填料為氮化硼或滑石。
- 如請求項1至12中任一項之塗料組成物,其中,各向異性填料之長寬比為15以上。
- 如請求項1至13中任一項之塗料組成物,其中,各向異性填料與氟樹脂之合計量之質量比為5:95~60:40。
- 如請求項1至14中任一項之塗料組成物,其中,界面活性劑為非氟系界面活性劑。
- 如請求項1至15中任一項之塗料組成物,其中,液體介質包含水。
- 一種電路基板之絕緣材料,其由請求項1至16中任一項之塗料組成物構成。
- 一種積層體,其特徵在於:具有藉由將請求項1至16中任一項之塗料組成物塗裝於基材上所形成之塗膜層。
- 如請求項18之積層體,其中,基材為金屬材料。
- 如請求項19之積層體,其中,金屬材料之塗膜層側之面的表面粗糙度Rz為2.0 μm以下。
- 如請求項19或20之積層體,其中,金屬為銅。
- 如請求項18至21中任一項之積層體,其係印刷基板、基板用介電材料、或積層電路基板。
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TW112113310A TW202402974A (zh) | 2022-04-11 | 2023-04-10 | 塗料組成物、絕緣材料及積層體 |
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JP (2) | JP7323856B1 (zh) |
TW (1) | TW202402974A (zh) |
WO (1) | WO2023199809A1 (zh) |
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JP4306072B2 (ja) * | 2000-01-28 | 2009-07-29 | ダイキン工業株式会社 | 溶融加工可能な含フッ素重合体水性分散液 |
EP1561784B1 (en) * | 2002-10-29 | 2012-11-28 | Daikin Industries, Ltd. | Fluororesin composition, molded fluororesin articles, fluororesin laminates and use of the laminates |
JP2016087799A (ja) * | 2014-10-29 | 2016-05-23 | 東レ・デュポン株式会社 | 高周波回路基板用の長尺状積層体及びその製造方法 |
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- 2023-04-05 WO PCT/JP2023/014045 patent/WO2023199809A1/ja unknown
- 2023-04-05 JP JP2023061086A patent/JP7323856B1/ja active Active
- 2023-04-10 TW TW112113310A patent/TW202402974A/zh unknown
- 2023-07-24 JP JP2023119778A patent/JP2023155916A/ja active Pending
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JP7323856B1 (ja) | 2023-08-09 |
WO2023199809A1 (ja) | 2023-10-19 |
JP2023155897A (ja) | 2023-10-23 |
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