CN116390993A - 水性涂料组合物及涂装物品 - Google Patents
水性涂料组合物及涂装物品 Download PDFInfo
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- CN116390993A CN116390993A CN202180074931.4A CN202180074931A CN116390993A CN 116390993 A CN116390993 A CN 116390993A CN 202180074931 A CN202180074931 A CN 202180074931A CN 116390993 A CN116390993 A CN 116390993A
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- aqueous coating
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- fluororesin
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- 239000008199 coating composition Substances 0.000 title claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 80
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- 238000000576 coating method Methods 0.000 claims abstract description 41
- 239000011248 coating agent Substances 0.000 claims abstract description 38
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- 238000002156 mixing Methods 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-DYCDLGHISA-N deuterium hydrogen oxide Chemical compound [2H]O XLYOFNOQVPJJNP-DYCDLGHISA-N 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 28
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 20
- 239000011737 fluorine Substances 0.000 claims description 20
- 239000011247 coating layer Substances 0.000 claims description 16
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- 125000001309 chloro group Chemical group Cl* 0.000 description 2
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- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 2
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- ODYWKGZHVSUTKO-UHFFFAOYSA-N 2-ethylhexan-1-ol;oxirane Chemical compound C1CO1.CCCCC(CC)CO ODYWKGZHVSUTKO-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- LVYXPOCADCXMLP-UHFFFAOYSA-N 3-butoxy-n,n-dimethylpropanamide Chemical compound CCCCOCCC(=O)N(C)C LVYXPOCADCXMLP-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
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- 229920001214 Polysorbate 60 Polymers 0.000 description 1
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- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
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- 125000004183 alkoxy alkyl group Chemical group 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
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- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
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- 125000005008 perfluoropentyl group Chemical group FC(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)* 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
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Abstract
本发明提供一种水性涂料组合物,其为显示低线膨胀系数的水性涂料组合物,通过涂布于铜箔等金属基材,能够抑制基材的翘曲。一种水性涂料组合物,其为含有能够熔融成型的氟树脂颗粒(A)的水性涂料组合物,其特征在于,上述水性涂料组合物还含有二氧化硅颗粒(B)、非氟系表面活性剂(C)及水(D),上述氟树脂颗粒(A)的平均粒径为0.05μm~1000μm,上述二氧化硅颗粒(B)的平均粒径为0.1μm~20μm,上述氟树脂颗粒(A)与上述二氧化硅颗粒(B)的混配比为氟树脂颗粒(A):二氧化硅颗粒(B)=10:90~90:10(质量比),相对于涂料固体成分100质量%,含有15质量%~80质量%的上述氟树脂颗粒(A)。
Description
技术领域
本公开涉及水性涂料组合物及涂装物品。
背景技术
氟树脂利用其优异的耐热性、耐候性、耐油性、耐溶剂性、耐化学药品性及非粘合性,已知有各种用途和粉末、膜等各种使用形态。
在数十千兆赫水平的高频区域的用途中使用的印刷布线基板中,从介电特性、吸湿性的观点出发,也主要使用形成有氟树脂的绝缘层的层积体。
专利文献1中公开了一种用于在金属基材上形成由氟树脂形成的被覆层的水性涂料组合物。
专利文献2中公开了一种用于在金属基材上形成由氟树脂形成的被覆层的涂料组合物,还公开了进一步混配二氧化硅。
专利文献3~5中公开了含有氟树脂颗粒的水性涂料组合物。
现有技术文献
专利文献
专利文献1:国际公开1994/05729
专利文献2:日本特开2009-1767号公报
专利文献3:日本特开平5-301974号公报
专利文献4:国际公开2020/071382
专利文献5:国际公开2018/016644
发明内容
发明所要解决的课题
本公开的目的在于提供一种通过涂布于铜箔等金属基材而能够抑制基材的翘曲的水性涂料组合物。
用于解决课题的手段
本公开涉及一种水性涂料组合物,其为含有能够熔融成型的氟树脂颗粒(A)的水性涂料组合物,其特征在于,
该水性涂料组合物还含有二氧化硅颗粒(B)、非氟系表面活性剂(C)及水(D),
上述氟树脂颗粒(A)的平均粒径为0.05μm~1000μm,
上述二氧化硅颗粒(B)的平均粒径为0.1μm~20μm,
上述氟树脂颗粒(A)与上述二氧化硅颗粒(B)的混配比为氟树脂颗粒(A):二氧化硅颗粒(B)=10:90~90:10(质量比),
相对于涂料固体成分100质量%,含有15质量%~80质量%的上述氟树脂颗粒(A)。
上述水性涂料组合物优选还含有二醇系溶剂(E)。
上述二醇系溶剂(E)优选在氟树脂颗粒(A)的烧成后不残留。
上述二氧化硅颗粒(B)的最大粒径优选为10μm以下。
上述二氧化硅颗粒(B)的水分散性优选为30质量%以上。
上述氟树脂颗粒(A)的平均粒径优选为0.1~100。
上述氟树脂颗粒(A)的体积基准累积50%直径优选为0.05μm~40μm。
上述非氟系表面活性剂(C)优选为有机硅系表面活性剂。
本公开也涉及一种涂装物品,其特征在于,具有通过涂装上述水性涂料组合物而形成的被覆层。
上述涂装物品可以是在金属基材上具有通过涂装上述水性涂料组合物而形成的被覆层的涂装物品。
上述涂装物品可以是印刷基板、基板用介电材料或层积电路基板。
发明效果
根据本公开,能够不使用氟系表面活性剂而得到能够形成电物性和表面物性优异、且抑制了翘曲的产生的氟树脂被覆层的水性涂料组合物。
具体实施方式
若想要层积氟树脂和金属导体来制作氟树脂基板,则在260℃左右的温度下进行的回流焊处理中会产生翘曲。并且,产生了这种翘曲的氟树脂基板无法用作高频电路基板。
二氧化硅即使在260℃以上的回流焊温度下,氟耐腐蚀性也优异,并且与氟树脂相比,热膨胀系数小。通过形成混配有上述二氧化硅的氟树脂被覆层,被覆层的热膨胀系数与金属基材的热膨胀系数之差变小,能够抑制回流焊时的翘曲的产生。进而,在本公开的水性涂料组合物中,通过与非氟系表面活性剂组合使用,能够抑制由回流焊时产生的氢氟酸导致的分解,能够有效地得到由混配二氧化硅带来的效果。
上述二氧化硅颗粒(B)例如基于BET法的比表面积优选为1.0m2/g~25.0m2/g,更优选为1.0m2/g~10.0m2/g,进一步优选为2.0m2/g~6.4m2/g。通过使比表面积为上述范围内,膜中的二氧化硅的凝聚少,涂膜面平滑,因此优选。
上述二氧化硅颗粒(B)的平均粒径为0.1μm~20μm。若平均粒径为上述范围内,则凝聚少,能够得到良好的表面粗糙度。上述平均粒径的下限优选为0.1μm,更优选为0.3μm。上述平均粒径的上限优选为5μm,更优选为2μm。上述平均粒径是通过激光衍射/散射法测定的值。
上述二氧化硅颗粒(B)的最大粒径优选为10μm以下。若最大粒径为10μm以下,则凝聚少,分散状态良好。进而,可以使得到的涂膜的表面粗糙度小。上述最大粒径更优选为5μm以下。对于最大粒径,拍摄SEM(扫描型电子显微镜)照片,使用SEM用图像分析软件,由随机选择的200个颗粒的图像数据求出。
上述二氧化硅颗粒(B)的形状没有特别限定,可以使用球状、柱状、锥状、截锥状、多面体状、中空状等。特别优选为球状、立方体、盆状、圆盘状、八面体状、鳞片状、棒状、板状、杆状、四角砌块状、中空状,更优选为球状、立方状、八面体状、板状、中空状。
上述二氧化硅颗粒(B)的水分散性优选为30质量%以上。若低于30质量%,则分散性变得不充分,水性涂料组合物的稳定性有可能降低。
关于上述水分散性,在容器中称量二氧化硅、水,充分施加剪切使其分散后,停止搅拌时二氧化硅表面润湿,确认数分钟不产生沉淀。
上述二氧化硅颗粒(B)可以是进行了表面处理的二氧化硅颗粒,例如可以是用有机硅化合物进行了表面处理的二氧化硅颗粒。通过用上述有机硅化合物进行表面处理,能够降低二氧化硅颗粒(B)的介电常数。
作为上述有机硅化合物,没有特别限定,可以使用以往公知的有机硅化合物。例如,优选包含选自由硅烷偶联剂和有机硅氮烷组成的组中的至少一种。
关于上述有机硅化合物的表面处理量,表面处理剂对二氧化硅颗粒表面的反应量优选每单位表面积(nm2)为0.1个~10个,更优选为0.3个~7个。
作为上述二氧化硅颗粒(B),可以使用一种或两种以上物性不同的二氧化硅颗粒。
另外,二氧化硅颗粒(B)可以直接使用粉体,也可以使用分散于树脂中的物质。
本公开的水性涂料组合物混配能够熔融成型的氟树脂颗粒(A)。通过使用这样的氟树脂颗粒(A),成型后的涂膜的均匀性和膜强度提高,加工性提高,在这一点上是优选的。
作为上述能够熔融成型的氟树脂颗粒(A)的组成,没有特别限定,例如可以举出四氟乙烯[TFE]/六氟丙烯[HFP]共聚物[FEP]、TFE/氟代烷基乙烯基醚共聚物[PFA]、TFE/HFP/氟代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30万以下的四氟乙烯[LMW-PTFE]等。可以使用1种,也可以混合2种以上。
作为上述氟代烷基乙烯基醚,例如优选为选自由下述物质组成的组中的至少1种,所述物质为:
通式(110):CF2=CF-ORf111
(式中,Rf111表示全氟有机基团。)所示的含氟单体;
通式(120):CF2=CF-OCH2-Rf121
(式中,Rf121表示碳原子数1~5的全氟烷基)所示的含氟单体;
通式(130):CF2=CFOCF2ORf131
(式中,Rf131为碳原子数1~6的直链或支链全氟烷基、碳原子数5~6的环式全氟烷基、含有1~3个氧原子的碳原子数2~6的直链或支链全氟氧烷基。)所示的含氟单体;
通式(140):CF2=CFO(CF2CF(Y141)O)m(CF2)nF
(式中,Y141表示氟原子或三氟甲基。m为1~4的整数。n为1~4的整数。)所示的含氟单体;以及
通式(150):CF2=CF-O-(CF2CFY151-O)n-(CFY152)m-A151
(式中,Y151表示氟原子、氯原子、-SO2F基或全氟烷基。全氟烷基可以含有醚氧和-SO2F基。n表示0~3的整数。n个Y151可以相同也可以不同。Y152表示氟原子、氯原子或-SO2F基。m表示1~5的整数。m个Y152可以相同也可以不同。A151表示-SO2X151、-COZ151或-POZ152Z153。X151表示F、Cl、Br、I、-OR151或-NR152R153。Z151、Z152和Z153相同或不同,表示-NR154R155或-OR156。R151、R152、R153、R154、R155及R156相同或不同,表示H、铵、碱金属、可以含有氟原子的烷基、芳基、或含磺酰基的基团。)所示的含氟单体。
本说明书中,上述“全氟有机基团”是指与碳原子键合的氢原子全部被氟原子取代而成的有机基团。上述全氟有机基团可以具有醚氧。
作为通式(110)所示的含氟单体,可以举出Rf111为碳原子数1~10的全氟烷基的含氟单体。上述全氟烷基的碳原子数优选为1~5。
作为通式(110)中的全氟有机基团,可以举出例如全氟甲基、全氟乙基、全氟丙基、全氟丁基、全氟戊基、全氟己基等。
作为通式(110)所示的含氟单体,还可以举出下述含氟单体:
上述通式(110)中,
Rf111为碳原子数4~9的全氟(烷氧基烷基)的含氟单体;
Rf111为下式:
[化1]
(式中,m表示0或1~4的整数。)所示的基团的含氟单体;
Rf111为下式:
[化2]
(式中,n表示1~4的整数。)所示的基团的含氟单体;等等。
作为通式(110)所示的含氟单体,其中,优选为
通式(160):CF2=CF-ORf161
(式中,Rf161表示碳原子数1~10的全氟烷基。)所示的含氟单体。Rf161优选为碳原子数为1~5的全氟烷基。
作为氟代烷基乙烯基醚,优选为选自由通式(160)、(130)和(140)所示的含氟单体组成的组中的至少1种。
作为通式(160)所示的含氟单体,优选选自由全氟(甲基乙烯基醚)、全氟(乙基乙烯基醚)以及全氟(丙基乙烯基醚)组成的组中的至少1种,更优选选自由全氟(甲基乙烯基醚)以及全氟(丙基乙烯基醚)组成的组中的至少1种。
作为通式(130)所示的含氟单体,优选为选自由CF2=CFOCF2OCF3、CF2=CFOCF2OCF2CF3以及CF2=CFOCF2OCF2CF2OCF3组成的组中的至少1种。
作为通式(140)所示的含氟单体,优选为选自由CF2=CFOCF2CF(CF3)O(CF2)3F、CF2=CFO(CF2CF(CF3)O)2(CF2)3F以及CF2=CFO(CF2CF(CF3)O)2(CF2)2F组成的组中的至少1种。
作为通式(150)所示的含氟单体,优选为选自由CF2=CFOCF2CF2SO2F、CF2=CFOCF2CF(CF3)OCF2CF2SO2F、CF2=CFOCF2CF(CF2CF2SO2F)OCF2CF2SO2F和CF2=CFOCF2CF(SO2F)2组成的组中的至少1种。
本说明书中,“有机基团”是指含有1个以上的碳原子的基团、或者从有机化合物中除去1个氢原子而形成的基团。
该“有机基团”的例子包括:
可以具有1个以上的取代基的烷基、
可以具有1个以上的取代基的烯基、
可以具有1个以上的取代基的炔基、
可以具有1个以上的取代基的环烷基、
可以具有1个以上的取代基的环烯基、
可以具有1个以上的取代基的环烷二烯基、
可以具有1个以上的取代基的芳基、
可以具有1个以上的取代基的芳烷基、
可以具有1个以上的取代基的非芳香族杂环基、
可以具有1个以上的取代基的杂芳基、
氰基、甲酰基、RaO-、RaCO-、RaSO2-、RaCOO-、RaNRaCO-、RaCONRa-、RaOCO-、RaOSO2-、以及RaNRbSO2-
(这些式中,Ra独立地为
可以具有1个以上的取代基的烷基、
可以具有1个以上的取代基的烯基、
可以具有1个以上的取代基的炔基、
可以具有1个以上的取代基的环烷基、
可以具有1个以上的取代基的环烯基、
可以具有1个以上的取代基的环烷二烯基、
可以具有1个以上的取代基的芳基、
可以具有1个以上的取代基的芳烷基、
可以具有1个以上的取代基的非芳香族杂环基、或者
可以具有1个以上的取代基的杂芳基,
Rb独立地为H或者可以具有1个以上的取代基的烷基)。
作为上述有机基团,优选可以具有1个以上的取代基的烷基。
作为上述氟树脂颗粒(A),从非粘合性、表面平滑性的观点出发,优选FEP、PFA或EPA,PFA的熔点为300℃以上,由于没有钎焊加工时的变形,因此特别优选PFA。
上述氟树脂颗粒(A)的平均粒径为0.05μm~1000μm,优选为0.1μm~100μm,更优选为0.1μm~30μm。若平均粒径在上述范围内,则能够得到薄膜且平滑的树脂被覆层,因此优选。
上述平均粒径例如为通过激光衍射/散射法测定的体积平均粒径。为了使上述氟树脂颗粒(A)成为所期望的粒径,可以进行利用筛、风力的分级。
上述氟树脂颗粒(A)的体积基准累积50%直径优选为0.05μm~40μm,更优选为7μm~40μm。上述体积基准累积50%直径是通过激光衍射/散射法测定粒度分布,将颗粒的集团的总体积设为100%而求出累积曲线,在该累积曲线上累积体积成为50%的点的粒径。若上述体积基准累积50%直径为上述范围内,则能够形成薄膜且平滑的被覆树脂层,因此优选。
上述氟树脂颗粒(A)的制造方法没有特别限定,具体而言,例如可以通过日本特开2009-1767号公报中记载的方法等来制造。
作为构成上述氟树脂颗粒(A)的氟树脂的聚合方法,没有特别限制,可以举出本体聚合、悬浮聚合、溶液聚合、乳液聚合等。在上述聚合中,温度、压力等各条件、聚合引发剂、其它添加剂可以根据所期望的氟树脂的组成、量适当设定。
上述水性涂料组合物中的氟树脂颗粒(A)的混配量为全部组合物质量的15质量%~80质量%,优选为15质量%~75质量%,更优选为20质量%~50质量%。若氟树脂颗粒(A)的混配量少于上述下限,则粘度过低,即使涂装于物品表面也会立即产生流挂,另外也无法进行厚涂。另一方面,若氟树脂颗粒(A)的混配量过多,则涂料组合物不具有流动性,无法涂装。具体的混配量只要考虑涂装方法、膜厚的调整等而在上述范围内适当选择即可,但在喷雾涂装等情况下设为比较低的浓度,另一方面,在按压涂装等情况下设为成为糊状的50质量%以上即可。
本公开中,水性涂料组合物的固体成分浓度通过加热残余质量测定法来测定。
本公开的水性涂料组合物为氟树脂颗粒(A):二氧化硅颗粒(B)=10:90~90:10(质量比)。通过以该比例混配氟树脂颗粒(A)和二氧化硅颗粒(B),可以得到防止翘曲等效果。关于上述混配量,氟树脂颗粒(A)的混配量的下限更优选为10,进一步优选为20。关于上述混配量,氟树脂颗粒(A)的混配量的上限更优选为90,进一步优选为80。关于上述混配量,二氧化硅颗粒(B)的混配量的上限更优选为60,进一步优选为50。
本公开的水性涂料组合物还含有非氟系表面活性剂(C)。若考虑成本方面,则含有非氟系表面活性剂而不是氟系表面活性剂也是优选本公开的水性涂料组合物的理由之一。
另外,若混配氟系表面活性剂,则在进行上述氟树脂颗粒(A)的烧成时,产生氢氟酸。该氢氟酸促进二氧化硅颗粒(B)的劣化,因此优选不含有。
作为上述非氟系表面活性剂(C),只要能够使氟树脂颗粒(A)稳定地分散于组合物中就没有特别限定,可以使用阴离子型表面活性剂、阳离子型表面活性剂、非离子型表面活性剂、两性表面活性剂中的任一种。可以举出例如:烷基硫酸钠、烷基醚硫酸钠、烷基硫酸三乙醇胺盐、烷基醚硫酸三乙醇胺盐、烷基硫酸铵、烷基醚硫酸铵、烷基醚磷酸钠、氟代烷基羧酸钠等阴离子型表面活性剂;烷基铵盐、烷基苄基铵盐等阳离子型表面活性剂;聚氧乙烯烷基醚、聚氧乙烯苯基醚、聚氧乙烯烷基酯、丙二醇-氧化丙烯共聚物、全氟烷基氧化乙烯加成物、2-乙基己醇氧化乙烯加成物等非离子型表面活性剂;烷基氨基乙酸甜菜碱、烷基酰胺乙酸甜菜碱、咪唑鎓甜菜碱等两性表面活性剂。其中,优选阴离子型和非离子型表面活性剂。特别优选的表面活性剂为热分解残余量少的具有氧化乙烯链的非离子型表面活性剂。
作为上述非氟系表面活性剂(C),还可以使用烃系表面活性剂、有机硅系表面活性剂、炔二醇等乙炔系表面活性剂等。另外,可以使用这些非氟系表面活性剂中的一种或组合2种以上使用。需要说明的是,优选不使用壬基苯酚系表面活性剂。
作为上述非氟系表面活性剂(C),特别优选有机硅系表面活性剂。作为上述有机硅系表面活性剂,没有特别限定,可以举出例如聚氧乙烯(POE)改性有机聚硅氧烷、聚氧乙烯·聚氧丙烯(POE·POP)改性有机聚硅氧烷、POE山梨糖醇酐改性有机聚硅氧烷、POE甘油改性有机聚硅氧烷等被亲水基改性的有机聚硅氧烷等。
作为具体例,可以举出DBE-712、DBE-821(AZmax公司制)、KP系列、KF-6015、KF-6016、KF-6017、KF-6028(信越化学工业公司制)、ABIL-EM97(Goldschmidt公司制)、POLYFLOW KL-100、POLYFLOW KL-401、POLYFLOW KL-402、POLYFLOW KL-700(共荣社化学制)、“FZ-77”(Dow Corning Toray株式会社制)、“BYK-333”(BYK日本公司制)。
上述非氟系表面活性剂(C)的混配量相对于上述氟树脂颗粒(A)100质量%优选为0.01质量%~50质量%、更优选为0.1质量%~30质量%、进一步优选为0.2质量%~20质量%。若表面活性剂的添加量过少,则氟树脂颗粒的分散变得不均匀,有时一部分浮起。另一方面,若表面活性剂的添加量过多,则由烧成引起的表面活性剂的分解残渣变多而产生着色,除此之外,被覆膜的耐热性、非粘合性等降低。
本公开的水性涂料组合物含有水(D)作为溶剂。由于介质为水,因此从对环境的不良影响少的方面考虑是优选的。
进而,本公开的水性涂料组合物优选与水并用而含有水溶性溶剂。上述水溶性溶剂具有润湿上述氟树脂颗粒(A)的作用,进而高沸点的溶剂在涂装后的干燥时将树脂彼此连接,作为防止裂纹产生的干燥延迟剂发挥作用。即使是高沸点溶剂,在氟树脂的烧成温度下也会蒸发,因此不会对被覆膜造成不良影响。
对于上述水溶性溶剂的具体例而言,作为沸点至100℃的低沸点有机溶剂,可以举出甲醇、乙醇、异丙醇、仲丁醇、叔丁醇、丙酮、甲乙酮等;作为沸点为100℃~150℃的中沸点有机溶剂,可以举出甲基溶纤剂、乙基溶纤剂等;作为沸点为150℃以上的高沸点有机溶剂,可以举出N-甲基-2-吡咯烷酮、N,N-二甲基乙酰胺、3-丁氧基-N,N-二甲基丙酰胺、3-丁氧基-N,N-二甲基丙酰胺、N,N-二甲基甲酰胺、乙二醇、丙二醇、甘油、二甲基卡必醇、丁基二卡必醇、丁基溶纤剂、1,4-丁二醇、二乙二醇、三乙二醇、四乙二醇等。另外,这些水溶性溶剂可以使用1种或混合使用2种以上。作为上述水溶性溶剂,优选高沸点有机溶剂,其中,从分散稳定性、安全性的方面考虑,更优选二醇系溶剂(E)。
上述水溶性溶剂的混配量优选为总水量的0.5质量%~50质量%,更优选为1质量%~30质量%。在低沸点有机溶剂的情况下,若混配量过少,则容易引起泡的混入等,若过多,则组合物整体成为易燃性,损害水性分散组合物的优点。在中沸点有机溶剂的情况下,若混配量过多,则烧成后有时也残留在被覆膜中而造成不良影响,若过少,则涂布后的干燥时氟树脂恢复成粉末而无法烧成。在高沸点有机溶剂的情况下,若混配量过多,则有时在烧成后也残留在被覆膜中而造成不良影响。上述水溶性溶剂优选选择容易挥发的性质的溶剂、或调整混配量等,即使在上述氟树脂颗粒(A)的烧成后也不会残留在被覆膜中。需要说明的是,二醇系溶剂(E)在氟树脂颗粒(A)的烧成后没有残留的情况可以通过如下方式确认:刮取烧成后的涂膜,通过TG/DTA测定在二醇系溶剂的沸点附近没有重量减少。
本公开的水性涂料组合物可以根据需要进一步含有粘结剂树脂。但是,该情况下,优选不含有在N2下以10℃/分钟的条件测定的400℃的重量减少小于55%的树脂。包含这样的树脂的水性涂料组合物在用于涂膜化的加热后,粘结剂树脂也有可能未完全分解而残留,因此有时成为涂膜物性降低的原因。
在上述水性涂料组合物中,可以混配在氟树脂组合物中通常添加的各种添加剂,例如颜料、稳定剂、增稠剂、分解促进剂、防锈剂、防腐剂、消泡剂等。作为上述颜料,可示例出无机颜料、复合氧化物颜料等,可以举出白炭黑、碳酸钙、硫酸钡、滑石、硅酸钙等。
上述水性涂料组合物可以是不含着色颜料的透明涂料,也可以是根据需要含有着色颜料的着色涂料。
特征在于具有通过涂装上述水性涂料组合物而形成的被覆层的涂装物品也是本公开之一。
上述水性涂料组合物可以通过通常的涂料中使用的涂装方法进行涂装,作为上述涂装方法,可以举出喷雾涂装、辊涂装、利用刮刀的涂装、浸渍(浸没)涂装、浸渗涂装、旋流涂装、帘流涂装、利用棒涂机的涂装、凹版涂布法、微凹版涂布法等。
在上述涂装后,通过进行干燥、烧成,可以制成本公开的涂装物品。作为上述干燥,只要是能够除去水性介质的方法就没有特别限定,例如可以举出根据需要进行加热,在室温~130℃下进行5分钟~30分钟的方法等。上述烧成在氟树脂颗粒的熔融温度以上进行,通常优选在200℃~400℃的范围进行10分钟~60分钟。为了防止所涂布的金属箔的氧化,优选在非活性气体下的干燥、烧成。
作为本公开的涂装物品中的物品基材,可以使用:铁、不锈钢、铜、铝、黄铜等金属类;玻璃板、玻璃纤维的织布及无纺布等玻璃制品;聚丙烯、聚甲醛、聚酰亚胺、改性聚酰亚胺、聚酰胺酰亚胺、聚砜、聚醚砜、聚醚醚酮、液晶聚合物等通用及耐热性树脂的成型品及被覆物;SBR、丁基橡胶、NBR、EPDM等通用橡胶、硅橡胶、氟橡胶等耐热性橡胶的成型品及被覆物;天然纤维及合成纤维的织布及无纺布;或将它们组合而形成的层积基材等。
上述物品基材可以是进行了表面加工的基材。作为上述表面加工,可以举出使用喷砂粗糙化至所期望的粗糙度的表面加工、使颗粒附着而粗糙化的表面加工、实施了金属抗氧化处理的表面加工。
本公开的涂装物品可以在要求耐热性、耐溶剂性、润滑性、非粘合性等领域中使用,可以用于膜、纤维强化膜、预浸料、带树脂的金属箔、覆金属层积板、印刷基板、基板用介电材料、层积电路基板等。
本公开的涂装物品特别优选在铜箔上具有由本公开的水性涂料组合物形成的被覆层。近年来,在各种领域中,高频区域中的通信变得盛行。为了减小在高频区域中使用时的传输损耗,使用将含有含氟聚合物的电介质层与铜箔层积而成的材料。在这样的用途中,本公开的水性涂料组合物可以特别适宜地使用。
实施例
以下,通过实施例说明本公开。实施例中,在混配比例中,只要没有特别提及,则%、“份”是指质量%、质量份。本公开并不限定于以下记载的实施例。
实施例1
步骤1.预粉碎(干式粉碎)
通过悬浮聚合制造四氟乙烯(TFE)/全氟乙烯基醚(PFVE)共聚物(PFA:熔点=300℃、MFR=25g/10分钟),将得到的干燥粉末直接通过气流粉碎机装置(I.M.MATERIAL公司制)粉碎,得到平均粒径10μm的微粉末。
步骤2.预混合(预分散)
相对于通过步骤1.得到的PFA微粉末100质量份,将炔二醇系分散剂(Surfynol440、Air Products Japan公司制)10质量份、有机硅系表面活性剂(KP-106、信越化学工业公司制)10质量份及离子交换水280质量份与PFA微粉末充分搅拌、混合,得到PFA分散液。
步骤3.湿式粉碎
将通过步骤2.得到的PFA分散液用100目金属网过滤后,通过高压乳化机(Nanomizer NMII,吉田机械兴业公司制造,粉碎压力=200MPa),获得平均粒径0.20μm的(利用CAPA700:堀场制作所公司制造测定)PFA微粉末分散液(氟树脂颗粒(A-1)分散液)。
所得到的PFA微粉末的体积基准累积50%直径为0.20μm。
步骤4.涂料化
相对于通过步骤3.得到的PFA微粉末分散液100质量份,加入有机硅系表面活性剂(KP-106、信越化学工业公司制造)2.5质量份、乙二醇(双叶化学公司制造)2.5质量份、二氧化硅颗粒58质量份、以及离子交换水20质量份,进行涂料化。
需要说明的是,所使用的二氧化硅颗粒如下。
B-1:Admatechs制Admafine SC2500-SQ平均粒径0.5μm、比表面积6.1m2/g、最大粒径1.7μm
B-2:Admatechs制Admafine SC6500-SQ平均粒径1.5μm、比表面积4.0m2/g、最大粒径4.2μm
确认到所有二氧化硅均以70质量%显示出良好的水分散性。
实施例2~8
除了如表1所示那样变更各混配成分以外,与实施例1同样地进行涂料化。
实施例9
使用平均粒径25μm的PFA微粉末,省略湿式粉碎,除此以外,与实施例1同样地进行涂料化(氟树脂颗粒(A-2)分散液)。
所得到的PFA微粉末的体积基准累积50%直径为22.9μm。
实施例10~16
除了如表2所示那样变更各混配成分以外,与实施例9同样地进行涂料化。
实施例17~20
添加聚乙烯醇(PVA、皂化度:78~82mol%富士胶片和光纯药株式会社制)10wt%水溶液10质量份作为粘结剂树脂,如表3所示变更各混配成分,除此以外与实施例9同样地进行涂料化。
比较例1~4
除了如表4所示那样变更各混配成分以外,与实施例1和9同样地进行涂料化。
作为氟系表面活性剂,加入Ftergent 250(Neos公司制)2.5质量份。需要说明的是,比较例4不添加乙二醇而进行了涂料化。
对于所得到的涂料组合物,基于以下的基准进行评价。
按照以下的方法,得到树脂被覆层。
使用棒涂机(No.40)在铜箔(福田金属箔粉工业制CF-V9S-SV-18)上涂布涂料。将涂布后的铜箔在130℃下干燥15分钟,评价落粉。进而,在氮气气氛下、350℃下烧成15分钟,制作膜厚30μm的涂膜。烧成后的涂膜中没有残留乙二醇。
(覆铜层积板的翘曲)
对于所得到的覆铜层积体,通过目视确认有无翘曲。
×:卷曲成圆筒状。
△:观察到浮起。
〇:未观察到浮起。
(落粉)
在用手指抚摸的情况和指压的情况下,目视确认氟树脂粉末的脱落。
×:观察到脱落。
〇:未观察到脱落。
(二氧化硅的劣化)
用SEM确认涂布表面,确认二氧化硅颗粒有无变形。
×:有变形。
〇:无变形。
[表1]
[表2]
[表3]
[表4]
由表1~4的结果可知,本公开的水性涂料组合物能够形成抑制铜箔的翘曲、不产生落粉、二氧化硅的劣化的良好的氟树脂被覆层。
工业实用性
根据本公开,能够得到能够形成抑制铜箔等基材的翘曲、并且抑制落粉和抑制二氧化硅颗粒的劣化优异的被覆层的水性涂料组合物。上述水性涂料组合物适合用于印刷基板、基板用介电材料、层积电路基板等的涂装。
Claims (11)
1.一种水性涂料组合物,其为含有能够熔融成型的氟树脂颗粒(A)的水性涂料组合物,其特征在于,
所述水性涂料组合物还含有二氧化硅颗粒(B)、非氟系表面活性剂(C)及水(D),
所述氟树脂颗粒(A)的平均粒径为0.05μm~1000μm,
所述二氧化硅颗粒(B)的平均粒径为0.1μm~20μm,
所述氟树脂颗粒(A)与所述二氧化硅颗粒(B)的混配比以质量比计为氟树脂颗粒(A):二氧化硅颗粒(B)=10:90~90:10,
相对于涂料固体成分100质量%,含有15质量%~80质量%的所述氟树脂颗粒(A)。
2.根据权利要求1所述的水性涂料组合物,其还含有二醇系溶剂(E)。
3.根据权利要求2所述的水性涂料组合物,其中,二醇系溶剂(E)在氟树脂颗粒(A)的烧成后不残留。
4.根据权利要求1~3中任一项所述的水性涂料组合物,其中,二氧化硅颗粒(B)的最大粒径为10μm以下。
5.根据权利要求1~4中任一项所述的水性涂料组合物,其中,二氧化硅颗粒(B)的水分散性为30质量%以上。
6.根据权利要求1~5中任一项所述的水性涂料组合物,其中,氟树脂颗粒(A)的平均粒径为0.1μm~100μm。
7.根据权利要求1~6中任一项所述的水性涂料组合物,其中,氟树脂颗粒(A)的体积基准累积50%直径为0.05μm~40μm。
8.根据权利要求1~7中任一项所述的水性涂料组合物,其中,非氟系表面活性剂(C)为有机硅系表面活性剂。
9.一种涂装物品,其特征在于,具有通过涂装权利要求1~8中任一项所述的水性涂料组合物而形成的被覆层。
10.根据权利要求9所述的涂装物品,其中,在金属基材上具有通过涂装权利要求1~8中任一项所述的水性涂料组合物而形成的被覆层。
11.根据权利要求9或10所述的涂装物品,其为印刷基板、基板用介电材料或层积电路基板。
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WO1994005729A1 (en) | 1992-08-28 | 1994-03-17 | Daikin Industries, Ltd. | Water-base molten fluororesin dispersion composition |
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WO2020071382A1 (ja) | 2018-10-03 | 2020-04-09 | Agc株式会社 | 分散液及び樹脂付金属箔の製造方法 |
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EP0442363A1 (en) * | 1990-02-16 | 1991-08-21 | International Business Machines Corporation | Fluorinated polymeric composition, fabrication and use thereof |
WO1994005720A1 (en) * | 1992-09-09 | 1994-03-17 | Kao Corporation | Organo(poly)siloxane modified with phosphoric ester and process for producing the same |
WO2010050572A1 (ja) * | 2008-10-31 | 2010-05-06 | 株式会社スリーボンド | 水性コーティング剤組成物 |
WO2018016644A1 (ja) * | 2016-07-22 | 2018-01-25 | 旭硝子株式会社 | 液状組成物、並びに該液状組成物を使用した、フィルムおよび積層体の製造方法 |
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