CN114746271A - 聚芳硫醚树脂组合物、成型品、层叠体和它们的制造方法 - Google Patents
聚芳硫醚树脂组合物、成型品、层叠体和它们的制造方法 Download PDFInfo
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- CN114746271A CN114746271A CN202080081633.3A CN202080081633A CN114746271A CN 114746271 A CN114746271 A CN 114746271A CN 202080081633 A CN202080081633 A CN 202080081633A CN 114746271 A CN114746271 A CN 114746271A
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- Prior art keywords
- carbonate
- polyarylene sulfide
- sulfide resin
- resin composition
- pas
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 239000011342 resin composition Substances 0.000 title claims abstract description 64
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229920000412 polyarylene Polymers 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 claims abstract description 107
- 239000011347 resin Substances 0.000 claims abstract description 107
- 229910052751 metal Inorganic materials 0.000 claims abstract description 99
- 239000002184 metal Substances 0.000 claims abstract description 99
- 238000007747 plating Methods 0.000 claims abstract description 51
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 44
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 36
- 229920002725 thermoplastic elastomer Polymers 0.000 claims abstract description 29
- 229920000098 polyolefin Polymers 0.000 claims abstract description 27
- 238000000465 moulding Methods 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims description 30
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 17
- 238000007788 roughening Methods 0.000 claims description 13
- 238000003486 chemical etching Methods 0.000 claims description 12
- 238000007772 electroless plating Methods 0.000 claims description 12
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 238000009713 electroplating Methods 0.000 claims description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 235000010216 calcium carbonate Nutrition 0.000 claims description 10
- 238000005530 etching Methods 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000001095 magnesium carbonate Substances 0.000 claims description 7
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 7
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 239000004277 Ferrous carbonate Substances 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 5
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 5
- 229940116318 copper carbonate Drugs 0.000 claims description 5
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 5
- 239000010459 dolomite Substances 0.000 claims description 5
- 229910000514 dolomite Inorganic materials 0.000 claims description 5
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 5
- 235000019268 ferrous carbonate Nutrition 0.000 claims description 5
- 229960004652 ferrous carbonate Drugs 0.000 claims description 5
- 239000012765 fibrous filler Substances 0.000 claims description 5
- 229910000015 iron(II) carbonate Inorganic materials 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- 239000011656 manganese carbonate Substances 0.000 claims description 5
- 235000006748 manganese carbonate Nutrition 0.000 claims description 5
- 229940093474 manganese carbonate Drugs 0.000 claims description 5
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 5
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 5
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 235000011181 potassium carbonates Nutrition 0.000 claims description 5
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 5
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 239000011667 zinc carbonate Substances 0.000 claims description 5
- 235000004416 zinc carbonate Nutrition 0.000 claims description 5
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052793 cadmium Inorganic materials 0.000 claims description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000011133 lead Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052703 rhodium Inorganic materials 0.000 claims description 4
- 239000010948 rhodium Substances 0.000 claims description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 239000011135 tin Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims 3
- 239000011236 particulate material Substances 0.000 claims 2
- 239000013618 particulate matter Substances 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 14
- 239000000047 product Substances 0.000 description 42
- -1 alkali metal salt Chemical class 0.000 description 26
- 239000000243 solution Substances 0.000 description 25
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 14
- 125000004432 carbon atom Chemical group C* 0.000 description 14
- 238000002844 melting Methods 0.000 description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 10
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 9
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 6
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- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 5
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 5
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 4
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Abstract
提供:能以高粘接力在聚芳硫醚(PAS)成型品表面以简便的工序形成金属膜的层叠体的制造方法。进而,提供:可以供于能以高粘接力在PAS成型品表面通过更简便的工序形成金属膜的层叠体和其制造方法的、聚芳硫醚树脂组合物、成型品和它们的制造方法。更详细地,提供:配混聚芳硫醚树脂、热塑性弹性体和/或具有水解性的热塑性树脂、碳酸盐以及聚烯烃系蜡而成的聚芳硫醚树脂组合物、将其熔融成型而成、并经表面粗糙化的成型品、进一步具有金属镀层的层叠体和它们的制造方法。
Description
技术领域
本发明涉及聚苯硫醚树脂组合物、成型品和层叠体和它们的制造方法。更详细地,涉及:能以高密合力在聚苯硫醚树脂成型品的表面简便地形成金属膜的层叠体和其制造方法、用于提供该层叠体的聚芳硫醚树脂组合物、成型品和它们的制造方法。
背景技术
近年来,汽车领域中,为了通过轻量化而实现低燃油消耗化等,以往进行了将为金属制的各种构件替换为更轻量、且具有耐热性、耐化学药品性的工程塑料的操作。另外,作为在较高温下驱动的功率半导体的构件也具有耐热性的工程塑料备受关注。
前述工程塑料中,从耐热性、耐化学药品性优异的方面出发,含有以所谓聚苯硫醚(也有时省略为“PPS”)为代表的聚芳硫醚(也有时省略为“PAS”)的树脂组合物其成型品是有用的。然而,必须在其表面形成金属膜,例如用于电子电路、布线连接器等的情况下,PAS树脂组合物或其成型品是难粘接(难密合)的,因此,即使对其表面实施粗糙化处理并形成金属膜,也存在该金属膜容易剥离的问题。
作为解决上述问题的方法,提出了如下方法:对PAS成型品的表面以蚀刻液进行蚀刻处理,赋予钯催化剂后进行化学镀铜,形成镀铜层(例如参照专利文献1)。然而,该方法中,PAS成型品的表面被蚀刻液所侵蚀而变脆弱,存在形成于其上的镀铜层也变得容易经时地剥离的问题。因此,通过该方法制成导电性图案的情况下,存在产生镀铜层的断路、导电性的降低(电阻值的上升)的问题。
另外,提出了如下方法:在通过喷砂、喷丸等将PAS成型品表面粗糙化的基础上涂布底漆树脂,改善与金属蒸镀、金属镀层等覆膜的粘接力(参照专利文献2)。然而,为了确保充分的粘接力,使聚苯硫醚的表面粗糙化至1~10μm的深度,因此,不适于镜面那样的需要表面平滑性的灯反射器等材料。
因此,寻求以高粘接力在PAS成型品表面形成有金属膜的层叠体。因此,提出了如下方法:通过浸渍法在PAS成型品表面分别形成底漆树脂层和含有金属颗粒的金属层,之后,通过电解镀法、化学镀法等形成金属镀层的方法,凭借该方法,如果在聚苯硫醚的表面形成金属膜,则可以以高粘接力在聚苯硫醚的表面简便地形成金属膜(参照专利文献3、4)。然而,该方法为在PAS成型品表面依次形成底漆树脂层、含有金属颗粒的金属层、金属镀层的方法,因此工序数多,进一步从生产率的观点出发,期望提出工序更少的方法。
现有技术文献
专利文献
专利文献1:日本特开昭63-14880号公报
专利文献2:日本特开2002-97292号公报
专利文献3:国际公开2017/154879号小册子
专利文献4:日本专利第6355008号公报
发明内容
发明要解决的问题
本发明要解决的课题在于,可以提供:能以高粘接力在PAS成型品表面以简便的工序形成金属膜的层叠体和其制造方法。进而,提供:能供于这种层叠体和其制造方法的、PAS树脂组合物、成型品和它们的制造方法。
用于解决问题的方案
本发明人等为了解决上述课题而进行了深入研究,结果发现:对于将配混PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)而成的PAS树脂组合物进行熔融成型而成的成型品,以化学蚀刻处理进行粗糙化时,在其粗糙化后的表面以金属镀层处理法形成的金属膜呈现高粘接力,完成了本发明。
即,本发明涉及一种层叠体的制造方法,其特征在于,具备如下工序:对将PAS树脂组合物成型而成的成型品的表面以化学蚀刻处理进行粗糙化处理的工序;对经粗糙化处理的前述成型品表面进行金属镀层处理的工序,
前述PAS树脂组合物中配混有:
PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)。
另外,本发明涉及一种层叠体,其特征在于,在将PAS树脂组合物成型而成的成型品的经粗糙化的表面层叠有金属层,
前述PAS树脂组合物中配混有:
PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)。
另外,本发明涉及一种PAS树脂组合物的制造方法,其特征在于,具备如下工序:将PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)配混并熔融混炼。
另外,本发明涉及一种成型品的制造方法,其具备如下工序:将以前述中记载的PAS树脂组合物的制造方法制造的PAS树脂组合物进行熔融成型。
另外,本发明涉及一种PAS树脂组合物,其特征在于,其是配混PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)而成的。
另外,本发明涉及一种成型品,其是将前述中记载的PAS树脂组合物进行熔融成型而成的。
需要说明的是,本发明中,将PAS成型品表面与金属膜彼此接合记作粘接。
发明的效果
根据本发明,可以提供:能以高粘接力在PAS成型品表面通过更简便的工序形成金属膜的层叠体和其制造方法。进而,可以提供:能供于这种层叠体和其制造方法的、PAS树脂组合物、成型品和它们的制造方法。
附图说明
图1为实施例3中制造的PAS成型品的粗糙化表面前的SEM照片。
图2为实施例3中制造的PAS成型品的粗糙化表面后的SEM照片。
图3为比较例4中制造的PAS成型品的粗糙化表面前的SEM照片。
图4为比较例4中制造的PAS成型品的粗糙化表面后的SEM照片。
图5为镀层粘接性试验中使用的成型品(尺寸为mm单位)的概念图。
具体实施方式
本发明的层叠体的制造方法的特征在于,具备如下工序:以将PAS树脂组合物成型而成的成型品为支撑体,对该支撑体表面以化学蚀刻处理进行粗糙化处理的工序;对经粗糙化处理的前述支撑体表面进行金属镀层处理的工序,
前述PAS树脂组合物中配混有:
PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)。
前述PAS树脂(A)具有将芳香环与硫原子键合的结构作为重复单元的树脂结构,具体而言,是将下述通式(1)所示的结构部位作为重复单元的树脂。
(式中,R1和R2分别独立地表示氢原子、碳原子数1~4的烷基、硝基、氨基、苯基、甲氧基、乙氧基。)
从前述PAS树脂(A)的机械强度改善的方面出发,上述通式(1)中的R1和R2优选为氢原子,该情况下,可以举出下述通式(2)所示的以对位键合者、和下述通式(3)所示的以间位键合者。
其中,从前述PAS(A)的耐热性、结晶性改善的方面出发,特别优选重复单元中的硫原子对芳香环的键合为上述通式(2)所示的以对位键合的结构。
另外,前述PAS树脂(A)不仅具有上述通式(1)所示的结构部位,还可以具有选自下述通式(4)~(7)所示的结构部位中的至少1者。具有下述通式(4)~(7)的结构部位的情况下,从耐热性、机械强度变得良好的方面出发,这些结构部位在前述PAS树脂(A)中的摩尔比率优选30摩尔%以下、更优选10摩尔%以下。
前述PAS树脂(A)中,包含上述通式(4)~(7)所示的结构部位的情况下,作为与上述通式(1)所示的结构部位的重复单元的键合,可以为无规型,也可以为嵌段型。
进而,前述PAS树脂(A)在其结构中可以具有下述通式(8)所示的3官能的结构部位、萘基硫醚键等。需要说明的是,该情况下,这结构部位在前述PAS树脂(A)中的摩尔比率优选3摩尔%以下,特别是更优选1摩尔%以下。
前述PAS树脂(A)例如可以通过下述(1)~(5)的方法而制造。
方法(1),在N-甲基吡咯烷酮、二甲基乙酰胺等酰胺系溶剂、环丁砜等砜系溶剂中使硫化钠与对二氯苯反应。
方法(2),使对二氯苯在硫与碳酸钠的存在下聚合。
方法(3),在极性溶剂与对二氯苯的混合溶剂中滴加硫化钠、或滴加硫氢化钠与氢氧化钠的混合物、或滴加硫化氢与氢氧化钠的混合物并进行聚合。
方法(4),基于对氯苯硫酚的自缩合。
方法(5),包括如下步骤:使二碘芳香族化合物与单质硫与根据需要具有官能团的阻聚剂以熔融状态进行反应,使前述二碘芳香族化合物和前述单质硫、或它们的反应产物与根据需要的前述阻聚剂以熔融状态进行反应。
其中,从反应控制容易、工业生产率优异的方面出发,优选方法(1)的在N-甲基吡咯烷酮、二甲基乙酰胺等酰胺系溶剂、环丁砜等砜系溶剂中使硫化钠与对二氯苯反应的方法。另外,该方法(1)中,为了调节聚合度,优选添加羧酸的碱金属盐、磺酸的碱金属盐、氢氧化物等碱。
前述PAS树脂的300℃下测得的熔融粘度优选2Pa·s以上、更优选10Pa·s以上、进一步优选60Pa·s以上至优选1000Pa·s以下、更优选500Pa·s以下,进一步优选200Pa·s以下的范围。熔融粘度如果为2Pa·s以上,则可以保持材料强度,故优选。另一方面,熔融粘度如果为1000Pa·s以下,则从成型性的观点出发而优选。需要说明的是,本说明书中,“熔融粘度”的值采用的是,使用高化式流动试验仪(岛津制作所、CFT-500D),在300℃、载荷:1.96×106Pa、L/D=10(mm)/1(mm)下保持6分钟后测定熔融粘度(V6)而得到的值。
进而,对于前述PAS树脂(A),从可以减少残留金属离子量、改善耐湿特性、且可以减少聚合时副产的低分子量杂质的残留量的方面出发,优选制造前述PAS(A)后进行酸处理,接着,用水进行清洗而成者。
作为前述酸处理中使用的酸,例如优选乙酸、盐酸、硫酸、磷酸、硅酸、碳酸、丙酸。另外,这些酸中,可以有效地减少残留金属离子量而不分解前述PAS(A)的方面出发,优选乙酸、盐酸。
前述酸处理的方法可以举出使前述PAS树脂(A)浸渍于酸或酸水溶液的方法。此时,可以根据需要进一步进行搅拌或加热。
此处,作为酸处理的具体方法,如果列举使用乙酸的方法作为例子,则可以举出如下方法:首先,将pH4的乙酸水溶液加热至80~90℃,使前述PAS树脂(A)浸渍于其中,搅拌20~40分钟。
对于如此经酸处理的前述PAS树脂(A),为了以物理方式去除残留的酸、盐,用水或热水进行多次清洗。作为此时使用的水,优选蒸馏水或去离子水。
另外,供于前述酸处理的PAS树脂(A)优选为粉粒体,具体而言,可以为粒料那样的粒状体,也可以处于聚合后的浆料状体。
本发明中,对于PAS成型品,从基于前述金属镀层处理的与金属层的粘接力改善的方面出发,本发明的PAS树脂组合物中进一步配混有选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)作为必须成分。
作为本发明中使用的热塑性弹性体(b1),只要为公知的物质就没有特别限制,优选通过后述的化学蚀刻处理而去除者。具体而言,可以举出聚烯烃系热塑性弹性体(也有时称为“烯烃共聚物系热塑性弹性体”)、氟系热塑性弹性体、有机硅系热塑性弹性体、苯乙烯系热塑性弹性体、氟树脂系热塑性弹性体、聚氨酯树脂系热塑性弹性体等,可以举出聚烯烃系热塑性弹性体作为特别优选例。
作为前述聚烯烃系热塑性弹性体,可以举出α-烯烃的均聚物、2种以上的α-烯烃的共聚物、1种或2种以上的α-烯烃与具有官能团的乙烯基聚合性化合物的共聚物。此时,作为前述α-烯烃,可以举出乙烯、丙烯、1-丁烯等碳原子数为2以上至8以下的范围的α-烯烃。另外,作为前述官能团,可以举出羧基、酸酐基(-C(=O)OC(=O)-)、环氧基、氨基、羟基、巯基、异氰酸酯基、噁唑啉基等。而且,作为具有前述官能团的乙烯基聚合性化合物,可以举出乙酸乙烯酯;(甲基)丙烯酸等α,β-不饱和羧酸;丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯等α,β-不饱和羧酸的烷基酯;离聚物等α,β-不饱和羧酸的金属盐(作为金属,为钠等碱金属、钙等碱土金属、锌等);甲基丙烯酸缩水甘油酯等α,β-不饱和羧酸的缩水甘油酯等;马来酸、富马酸、衣康酸等α,β-不饱和二羧酸;前述α,β-不饱和二羧酸的衍生物(单酯、二酯、酸酐)等中的1种或2种以上。另外,例如还可以举出乙烯-丙烯系橡胶(EPM)、乙烯-丙烯-二烯系橡胶(EPDM)、丁二烯系橡胶、氯丁烯橡胶、腈系橡胶、丁基系橡胶、丙烯酸类橡胶等。另外,作为苯乙烯系热塑性弹性体,可以举出苯乙烯-丁二烯系橡胶(SBR)、氢化SBR等。另外,可以举出有机硅系橡胶等有机硅系热塑性弹性体、氟系橡胶等氟树脂系热塑性弹性体、氨基甲酸酯系橡胶等聚氨酯树脂系热塑性弹性体等。上述热塑性弹性体可以单独使用,也可以组合2种以上而使用。
此处,作为具有水解性的热塑性树脂(b2),只要为具有水解性的公知的热塑性树脂就没有特别限制,优选可以举出通过后述的化学蚀刻处理而示出水解性的树脂。具体而言,可以举出聚酰胺树脂、聚酯树脂、聚碳酸酯树脂、聚醚树脂、聚氨酯树脂、聚酮树脂、聚内酯树脂、聚缩醛树脂、聚酰亚胺树脂、聚酰胺酰亚胺树脂、聚丙烯酸酯树脂、聚醚酰亚胺树脂、聚醚醚酮树脂、热塑性环氧树脂、热塑性酚醛树脂、和包含前述树脂结构的共聚物等。
前述热塑性树脂(b2)中,从得到的PAS成型品与金属层的粘接力优异的方面出发,可以示例聚酰胺树脂、聚碳酸酯树脂作为优选例,进而,可以示例聚酰胺树脂作为更优选例。
作为前述芳香族聚酰胺树脂,可以示例包含下述结构式(10)所示的重复单元的芳香族聚酰胺树脂。
前述结构式(10)中,R2表示碳原子数为2以上至12以下的范围的亚烷基。上述对苯二甲酸酰胺结构具体而言,通过使对苯二甲酸、或对苯二甲二酰卤与碳原子数为2以上至12以下的范围的脂肪族二胺的反应而形成。此处使用的碳原子数为2以上至12以下的范围的脂肪族二胺具体而言可以举出:乙二胺、丙二胺、1,4-丁二胺、1,6-己二胺、1,7-庚二胺、1,8-辛二胺、1,9-壬二胺、1,10-癸二胺、1,11-十一烷二胺、1,12-十二烷二胺等直链状脂肪族亚烷基二胺;1-丁基-1,2-乙二胺、1,1-二甲基-1,4-丁二胺、1-乙基-1,4-丁二胺、1,2-二甲基-1,4-丁二胺、1,3-二甲基-1,4-丁二胺、1,4-二甲基-1,4-丁二胺、2,3-二甲基-1,4-丁二胺、2-甲基-1,5-戊二胺、3-甲基-1,5-戊二胺、2,5-二甲基-1,6-己二胺、2,4-二甲基-1,6-己二胺、3,3-二甲基-1,6-己二胺、2,2-二甲基-1,6-己二胺、2,2,4-三甲基-1,6-己二胺、2,4,4-三甲基-1,6-己二胺、2,4-二乙基-1,6-己二胺、2,2-二甲基-1,7-庚二胺、2,3-二甲基-1,7-庚二胺、2,4-二甲基-1,7-庚二胺、2,5-二甲基-1,7-庚二胺、2-甲基-1,8-辛二胺、3-甲基-1,8-辛二胺、4-甲基-1,8-辛二胺、1,3-二甲基-1,8-辛二胺、1,4-二甲基-1,8-辛二胺、2,4-二甲基-1,8-辛二胺、3,4-二甲基-1,8-辛二胺、4,5-二甲基-1,8-辛二胺、2,2-二甲基-1,8-辛二胺、3,3-二甲基-1,8-辛二胺、4,4-二甲基-1,8-辛二胺、5-甲基-1,9-壬二胺等支链状脂肪族亚烷基二胺;环己二胺、甲基环己二胺、异佛尔酮二胺、降冰片烷二甲胺、三环癸烷二甲胺等脂环族二胺类。
其中,从得到的PAS成型品中,与金属层的粘接力更优异的方面出发,特别优选碳原子数为4以上至8以下的范围的直链状脂肪族亚烷基二胺、碳原子数为5以上至10以下的范围的支链状脂肪族亚烷基二胺。
另外,前述芳香族聚酰胺树脂还可以示例包含下述结构式(11)所示的重复单元的芳香族聚酰胺树脂。
(式中,R2与结构式(10)中的R2为相同含义。)
进而,前述芳香族聚酰胺树脂可以具有下述结构式(12)所示的酸酰胺结构。
(式中,R2与结构式(10)中的R2为相同含义,R3表示碳原子数为4以上至10以下的范围的脂肪族烃基。)
此处,上述结构式(12)所示的酸酰胺结构是通过碳原子数为4以上至10以下的范围的脂肪族二羧酸、其酸酯化物、其酸酐、或其酰卤与碳原子数为2以上至12以下的范围的脂肪族二胺的反应而形成的。此处使用的碳原子数为4以上至10以下的范围的脂肪族二羧酸具体而言可以举出丙二酸、二甲基丙二酸、琥珀酸、戊二酸、己二酸、2-甲基己二酸、三甲基己二酸、庚二酸、2,2-二甲基戊二酸、3,3-二乙基琥珀酸、壬二酸、癸二酸、辛二酸等脂肪族二羧酸;1,3-环戊烷二羧酸、1,4-环己烷二羧酸等脂环式二羧酸等脂肪族二羧酸类。
上述碳原子数为4以上至10以下的范围的脂肪族二羧酸的酸酯化物具体而言可以举出甲酯体、乙酯体、叔丁酯体等,另外,构成前述脂肪族二羧酸的酰卤的卤素原子可以举出溴原子、氯原子。
前述芳香族聚酰胺树脂如上述,优选具有前述结构式(10)、结构式(11)、结构式(12)所示的酰胺结构作为结构部位,将由二羧酸1分子和二胺1分子构成的酸酰胺结构作为1个单元的情况下,从在得到的PAS成型品中与金属层的粘接力更优异的方面出发,优选:相对于构成该芳香族聚酰胺树脂(B)的全部酸酰胺结构,包含前述对苯二甲酸酰胺结构50摩尔%以上、包含间苯二甲酸酰胺结构10摩尔%以上、包含脂肪族烃酸酰胺结构5摩尔%以上。
进而,对于前述芳香族聚酰胺树脂,从在得到的PAS成型品中,与金属层的粘接力更优异的方面出发,优选:
以50摩尔%以上至80摩尔%以下的范围构成前述结构式(10)所示的对苯二甲酸酰胺结构、
以10摩尔%以上至30摩尔%以下的范围构成前述结构式(11)所示的间苯二甲酸酰胺结构、
以5摩尔%以上至20摩尔%以下的范围构成前述结构式(12)所示的酸酰胺结构
的聚酰胺树脂。
另外,从前述芳香族聚酰胺树脂的重结晶峰温度变得更低、与前述PAS树脂的分散性变良好的方面出发,优选熔点290℃以上至330℃以下的范围、另外,Tg90℃以上至140℃以下的范围。
前述芳香族聚酰胺树脂例如通过以下的(1)或(3)的方法而制造。
界面聚合法(1),使包含对苯二甲酸的二羧酸成分的酰卤与包含碳原子数为2以上至12以下的范围的脂肪族二胺的二胺成分溶解于彼此不相溶的两种溶剂后,在碱和催化剂量的季铵盐的存在下将两种液体混合并搅拌,进行缩聚反应。
溶液聚合法(2),使包含对苯二甲酸的二羧酸成分的酰卤与包含碳原子数为2以上至12以下的范围的脂肪族二胺的二胺成分在叔胺等接受酸的碱性化合物的存在下、在有机溶剂中进行反应。
熔融聚合法(3),将包含对苯二甲酸的二羧酸成分的二酯化物和芳香族二胺作为原料,以熔融状态进行酰胺交换反应。
前述热塑性树脂(B)的配混比例没有特别限定,从基于前述金属镀层处理的与金属层的粘接力进一步改善的方面出发,选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)的总量相对于前述PAS树脂(A)的100质量份,优选5质量份以上、更优选15质量份以上、进一步优选30质量份以上至优选70质量份以下、更优选60质量份以下,进一步优选50质量份以下的范围。
本发明中,对于PAS成型品,从基于前述金属镀层处理的与金属层的粘接力改善的方面出发,本发明的PAS树脂组合物中进一步配混碳酸盐(C)作为必须成分。作为该碳酸盐(C),只要为公知的物质就没有特别限制,优选可以举出通过后述的化学蚀刻处理而去除者。具体而言,可以举出碳酸钙、碳酸镁、碳酸钾、碳酸钠、碳酸氢钠、碳酸铵、碳酸钡、碳酸锂、碳酸铜、碳酸亚铁、碳酸银、碳酸锰、碳酸锌、白云石和水菱镁矿等,可以举出碳酸钙作为特别优选例。
前述碳酸盐(C)的大小没有特别限定,从得到的PAS成型品中与金属层的粘接力更优异的的方面出发,其平均粒径优选6μm以下的范围、更优选3μm以下,进一步优选1.2μm以下,另一方面,下限值没有限定,优选0.3μm以上的范围、更优选0.5μm以上、更优选0.8μm以上的范围。需要说明的是,该平均粒径可以以对得到的成型品的截面进行基于电子显微镜的观察照片而进行,例如可以举出如下方法:在一边尺寸的3000倍的观察范围内测量任意的至少100个,求出其平均值。
前述碳酸盐(C)的配混的比例没有特别限定,从基于前述金属镀层处理的与金属层的粘接力进一步改善的方面出发,相对于前述PAS树脂(A)的100质量份,优选10质量份以上、更优选25质量份以上、进一步优选40质量份以上至优选90质量份以下、更优选80质量份以下,进一步优选70质量份以下的范围。
本发明中,对于PAS成型品,从基于前述金属镀层处理的与金属层的粘接力改善的方面出发,本发明的PAS树脂组合物中进一步配混聚烯烃系蜡(D)作为必须成分。
本发明中使用的聚烯烃系蜡(有时也称为“聚烯烃蜡”)只要为使具有烯烃结构的单体聚合而得到的具有聚烯烃结构的蜡即可,可以举出公知的物质。需要说明的是,本发明中,蜡是指:通过聚合而制造的、通常在25℃下为固体状的低分子量树脂、作为对PAS树脂组合物的添加剂在熔融成型时例如在模具内呈现脱模效果的物质。通常是指:分子量(Mn)优选250以上、更优选300以上至优选20000以下、更优选10000以下的范围者。分子量如果为250以上,则有熔融混炼时或熔融成型时等可以抑制来自真空排气口的挥发、且变得容易发挥脱模效果的倾向。另外,成型中,也有时抑制蜡渗出至所需以上而成为模具污染的原因的情况。另一方面,分子量如果为20000以下,则成为不易渗出的倾向,且有改善脱模效果的倾向。
作为该烯烃系蜡(D),特别优选使用将乙烯和/或1-烯烃作为原料聚合而成的聚乙烯蜡和/或1-烯烃聚合物,不仅可以得到极其良好的脱模效果,而且得到的PAS成型品中,与金属层的粘接力更优异。作为聚乙烯蜡的制造方法,可以使用目前通常广泛已知的方法,可以举出如下方法:使乙烯在高温高压下进行聚合的方法、使聚乙烯热分解的方法、从聚乙烯聚合物中分离纯化低分子量成分的方法等。作为1-烯烃,可以举出丙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯、1-十七碳烯、1-十八碳烯、1-十九碳烯、1-二十碳烯、1-二十一碳烯、1-二十二碳烯、1-二十三碳烯、1-二十四碳烯、1-二十五碳烯、1-二十六碳烯、1-二十七碳烯、1-二十八碳烯、1-二十九碳烯等。构成本发明中使用的烯烃蜡(B)的脂肪族烃基可以使用直链型、支链型这两者。
本发明中使用的烯烃系蜡(D)可以具有极性基团。作为极性基团,可以示例选自由羧基、酸酐、氨基、羟基、巯基、环氧基、醚键、酯键、酰胺键、酰亚胺键、尿素键、脲键和硫醚键组成的组中的至少1者。本发明中使用的烯烃系蜡(D)具有极性基团的情况下,还可以举出:使具有前述乙烯和/或1-烯烃聚合或共聚时能跟上述单体共聚的选自由羧基、酸酐、氨基、羟基、巯基、环氧基、醚键、酯键、酰胺键、酰亚胺键、尿素键、脲键和硫醚键组成的组中的至少1者、且具有烯属双键的化合物,优选马来酸酐或马来酸酐和马来酸进行共聚而成者。
前述烯烃系蜡(D)的配混的比例没有特别限定,从基于前述金属镀层处理的与金属层的粘接力进一步改善的方面出发,相对于前述PAS树脂(A)的100质量份,优选0.01质量份上、更优选0.05质量份上、进一步优选0.1质量份以上至优选10质量份以下、更优选5质量份以下,进一步优选2质量份以下的范围。
本发明的PAS树脂组合物可以进一步配混除碳酸盐(C)以外的填充剂作为任意成分。作为上述填充材料,只要不有损本发明的效果就可以使用公知常用的材料,例如可以举出粒状、纤维状等各种形状的填充材料等。具体而言,可以使用玻璃纤维、碳纤维、硅烷玻璃纤维、陶瓷纤维、芳族聚酰胺纤维、金属纤维、钛酸钾、碳化硅、硫酸钙、硅酸钙等纤维、硅灰石等天然纤维等纤维状的填充材料。而且,可以使用硫酸钡、硫酸钙、粘土、叶蜡石、膨润土、绢云母、沸石、云母、滑石、凹凸棒石、铁氧体、硅酸钙、玻璃珠等。本发明中使用的填充剂不是必须成分,使用的情况下,其配混的比例只要不有损本发明的效果就没有特别限定,另外,根据各自的目的而不同,不能一概地限定,例如,相对于前述PAS树脂100质量份,以优选10质量份以上、更优选40质量份以上、优选90质量份以下、更优选70质量份以下进行配混。在该范围内,可以根据加入填充剂的目的,改善强度、刚性、耐热性、放热性和尺寸稳定性等各种性能。
前述填充材料也可以使用以表面处理剂、集束剂加工而成者。由此,可以改善与PAS树脂(A)的粘接力,故优选。作为前述表面处理剂或集束剂,例如可以举出选自由具有氨基、环氧基、异氰酸酯基、乙烯基等官能团的硅烷化合物、钛酸酯化合物、丙烯酸类树脂、聚氨酯树脂和环氧树脂等组成的组中的至少1种聚合物等。
进而,本发明的PAS树脂组合物中,对于除前述热塑性树脂(B)和前述烯烃系蜡(D)以外的成分,可以根据用途适宜配混合成树脂、例如环氧树脂、聚酰亚胺树脂、聚醚酰亚胺树脂、聚苯醚树脂、聚砜树脂、聚醚砜树脂、聚醚醚酮树脂、聚醚酮树脂、聚芳酯树脂、聚乙烯树脂、聚丙烯树脂、聚四氟乙烯树脂、聚二氟乙烯树脂、聚苯乙烯树脂、ABS树脂、酚醛树脂、聚氨酯树脂、液晶聚合物等合成树脂(以下,简称为合成树脂)作为任意成分。本发明中,前述合成树脂不是必须成分,配混的情况下,其配混的比例只要不有损本发明的效果就没有特别限定,另外,根据各自的目的而不同,不能一概地限定,作为本发明的树脂组合物中配混的合成树脂的比例,例如可以举出:相对于PAS树脂(A)100质量份、5质量份以上且15质量份以下的范围。换言之,相对于PAS树脂(A)与合成树脂的总计,PAS树脂(A)的比例以质量基准计、优选可以为(100/115)以上的范围,而且优选可以为(100/105)以下的范围。
而且,本发明的PAS树脂组合物此外还可以根据需要配混着色剂、抗静电剂、抗氧化剂、耐热稳定剂、紫外线稳定剂、紫外线吸收剂、发泡剂、阻燃剂、阻燃助剂、防锈剂、和偶联剂等公知常用的添加剂作为任意成分。这些添加剂不是必须成分,配混的情况下,其配混的比例只要不有损本发明的效果就没有特别限定,另外,根据各自的目的而不同,不能一概地限定,例如,相对于PAS树脂(A)100质量份,可以优选以0.01质量份以上且1000质量份以下的范围,以不有损本发明的效果的方式根据目的、用途适宜调整而使用。
本发明的PAS树脂组合物是将PAS树脂(A)、前述热塑性树脂(B)、前述碳酸盐(C)和前述聚烯烃系蜡(D)作为必须成分、根据需要配混上述任意成分而成的。该PAS树脂组合物的制造方法具备如下工序:将PAS树脂(A)、前述热塑性树脂(B)、前述碳酸盐(C)和前述聚烯烃系蜡(D)作为必须成分,根据需要配混上述任意成分,在PAS树脂的熔点以上进行熔融混炼。
本发明的PAS树脂组合物的优选制造方法可以经如下工序而制造:将前述必须成分与前述任意成分以粉末、粒料、小片等各种形态投入至螺带式搅拌机、亨舍尔混合机、V型搅拌机等进行干混后,投入至班伯里密炼机、搅拌辊、单螺杆或双螺杆挤出机和捏合机等公知的熔融混炼机,在树脂温度成为PAS树脂的熔点以上的温度范围、优选成为该熔点+10℃以上的温度范围、更优选成为该熔点+20℃以上的温度范围、而且在成为该熔点+100℃以下的温度范围、更优选成为熔点+50℃以下的温度范围内进行熔融混炼。各成分向熔融混炼机的添加、混合可以同时进行,也可以分批进行。
作为前述熔融混炼机,从分散性、生产率的观点出发,优选双螺杆混炼挤出机,例如优选边将树脂成分的排出量在5~500(kg/小时)的范围适宜调整和螺杆转速在50~500(rpm)的范围适宜调整,边进行熔融混炼,进一步优选在它们的比率(排出量/螺杆转速)成为0.02~5(kg/小时/rpm)的范围的条件下进行熔融混炼。另外,前述成分中添加填充剂、添加剂的情况下,从分散性的观点出发,优选从前述双螺杆混炼挤出机的侧喂料机向该挤出机内投入。对于上述侧喂料机的位置,相对于前述双螺杆混炼挤出机的螺杆总长度,该挤出机树脂投入部(顶部喂料机)至该侧喂料机的距离的比率优选0.1以上、更优选0.3以上。另外,上述比率优选0.9以下、更优选0.7以下。
如此熔融混炼得到的本发明的PAS树脂组合物是包含前述必须成分、及根据需要加入的任意成分和源自这些的成分的熔融混合物。优选:该熔融混炼后,以公知的方法、例如将熔融状态的PAS树脂组合物挤出成型为股线状后,加工成粒料、小片、颗粒、粉末等形态后,根据需要在100~150℃的温度范围内实施预干燥,供于各种成型。挤出成型为股线状时,可以具备如下工序:将本发明的树脂组合物在优选剪切速度500sec-1以下的剪切区域、更优选剪切速度100sec-1以下至0sec-1以上的剪切区域内进行熔融。
通过前述制造方法制造的本发明的PAS树脂组合物除PAS树脂(A)之外可以还含有前述热塑性树脂(B)、前述碳酸盐(C)和前述聚烯烃系蜡(D)。认为:该PAS树脂组合物具有在PAS树脂的连续相中形成有至少前述热塑性树脂(B)或前述碳酸盐(C)的各分散相的形态学。进而,通过使用聚烯烃系蜡(D),从而将前述热塑性树脂(B)和前述碳酸盐(C)挤出至成型品表面的效果变高,结果认为:粗糙化处理工序中,形成于PAS成型品的粗糙化表面的、前述热塑性树脂(B)和前述碳酸盐被去除,通过金属镀层处理构成金属层的金属变得容易填充至所形成的孔隙,与金属层的粘接力进一步改善。
本发明的PAS成型品例如通过将前述PAS树脂组合物进行熔融成型而得到。本发明的PAS成型品的制造方法具备:将前述PAS树脂组合物进行熔融成型的工序。另外,本发明的PAS成型品的制造方法可以具备如下工序:将前述PAS树脂组合物在优选剪切速度500sec-1以下的剪切区域、更优选剪切速度100sec-1以下至0sec-1以上的剪切区域内进行熔融。熔融成型可以应用公知的方法、例如注射成型、压缩成型、合成材料、片、管等挤出成型、拉拔成型、吹塑成型、传递成型等各种成型方法。以注射成型进行成型的情况下,各种成型条件没有特别限定,可以以通常一般的方法进行成型。例如,可以经如下工序:在注射成型机内,在树脂温度成为PAS树脂的熔点以上的温度范围、优选成为该熔点+10℃以上的温度范围、更优选成为该熔点+20℃以上的温度范围、且成为该熔点+100℃以下的温度范围、更优选成为熔点+50℃以下的温度范围内将前述PAS树脂组合物进行熔融,然后,从树脂排出口向模具内注入并进行成型。此时,模具温度的范围也设为公知的温度范围、例如优选设为室温(23℃)以上、更优选设为40℃以上,进一步优选设为120℃以上。进一步模具温度优选设为300℃以下、更优选设为200℃以下,进一步优选设为180℃以下。
作为本发明的PAS成型品的形状,没有特别限定。如后述,形成导电性图案以电子电路用途使用的情况下,例如可以制成板状、薄膜或片状。制成板状的情况下,优选制成厚度优选0.5mm以上、更优选1.0mm以上至优选100mm以下、更优选10mm以下的范围的支撑体状。制成薄膜或片的情况下,厚度可以举出优选1μm以上、优选5000μm以下、更优选300μm以下、进一步优选200μm以下的范围。另外,也可以为连接器、柔性管等以模具成型的立体形状者。
如此得到的PAS成型品如后述可以用于本发明的层叠体和其制造方法。
本发明的层叠体的特征在于,在将PAS树脂组合物成型而成的成型品的经粗糙化的表面层叠有金属层,
前述PAS树脂组合物中配混有:
PAS树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除PAS树脂以外的热塑性树脂(B)、碳酸盐(C)和烯烃系蜡(D)。
本发明的层叠体可以通过具备如下工序的制造方法而制造:对将PAS树脂组合物成型而成的成型品的表面以化学蚀刻处理进行粗糙化处理的工序(以下,有时简称为“粗糙化处理工序”);对经粗糙化处理的前述成型品表面进行金属镀层处理的工序(以下,有时简称为“金属镀层处理工序”)。
前述粗糙化处理工序具备如下工序:通过浸渍法涂布蚀刻液等与前述PAS成型品的表面接触的工序。
作为该蚀刻液,只要可以去除存在于PAS成型品的表面的前述热塑性树脂(B)和前述碳酸盐就没有特别限定,例如优选包含强酸或其盐者。作为这种强酸或其盐,可以示例铬酸、硫酸、氟化铵、硝酸、铬酸酐,可以使用这些中的1种或组合2种以上而使用。使蚀刻液与前述PAS成型品的表面接触时的条件优选边适宜调整蚀刻液中的强酸或其盐的浓度、接触时的温度。
蚀刻液可以使用公知的物质。例如可以使用日本特开平5-155127号公报中记载者,即,由硫酸400g/升、铬酸酐400g/升、和稀释水(设为总蚀刻液量1升的量)形成的蚀刻液。
通过前述粗糙化处理工序,均匀地分散于PAS成型品的表面的前述热塑性树脂(B)和前述碳酸盐(C)的至少一部分被去除而形成孔隙。该孔隙的存在或比表面积的增加进一步改善与构成金属层的金属颗粒的相互作用,该PAS成型品与金属层的粘接力改善。另外,以往如果要想沿成型品表面的垂直方向用粘接剂等形成涂膜与金属层粘接,则制造时未固化的粘接剂等受到自重的影响而下垂,膜厚产生偏差,因此,有粘接力容易产生不均的倾向,但本发明中,有不易产生成型品表面上的部位所导致的孔隙不均的倾向,因此,粘接力的均匀性也优异。PAS成型品的粗糙化表面的表面粗糙度没有特别限定,从粘接力优异的观点出发,以十点平均粗糙度Rz计、优选0.1μm以上、更优选1μm以上至优选10μm以下、更优选5μm以下的范围。
金属镀层处理工序具备:通过电解镀法、化学镀法或它们的组合形成在前述PAS成型品的粗糙化表面的工序。
电解镀法、化学镀法的湿式镀覆法中,通过金属镀层处理构成金属层的金属容易填充至形成于PAS成型品的粗糙化表面的、前述热塑性树脂(B)和前述碳酸盐被去除而形成的孔隙中,不仅与金属层的粘接力进一步改善,而且也可以得到导电性优异的导电性图案,故优选。
上述化学镀法例如如下:使化学镀液与前述PAS成型品的粗糙化表面接触,从而使化学镀液中所含的铜等金属析出,可以形成由金属覆膜形成的化学镀层(覆膜)。
作为前述化学镀液,例如可以举出:含有选自由镍、铜、铬、锌、金、银、铝、铁、锡、钴、钨、钯、铅、铂、镉、和铑等组成的组中的至少1种金属(需要说明的是,将这些金属也称为“构成金属镀层的金属”、“构成金属层的金属”)、还原剂、以及水性介质、有机溶剂等溶剂者。
作为前述还原剂,例如可以举出二甲基氨基硼烷、次磷酸、次磷酸钠、二甲胺硼烷、肼、甲醛、硼氢钠、苯酚等。
另外,作为前述化学镀液,根据需要可以使用含有乙酸、甲酸等单羧酸;丙二酸、琥珀酸、己二酸、马来酸、富马酸等二羧酸化合物;苹果酸、乳酸、乙醇酸、葡萄糖酸、柠檬酸等羟基羧酸化合物;甘氨酸、丙氨酸、亚氨基二乙酸、精氨酸、天冬氨酸、谷氨酸等氨基酸化合物;亚氨基二乙酸、次氮基三乙酸、乙二胺二乙酸、乙二胺四乙酸、二亚乙基三胺五乙酸等氨基聚羧酸化合物等有机酸、或这些有机酸的可溶性盐(钠盐、钾盐、铵盐等)、乙二胺、二亚乙基三胺、三亚乙基四胺等胺化合物等螯合剂者。
前述化学镀液优选在20~98℃的范围内使用。
前述电解镀法例如为如下方法:对通过前述化学镀处理而形成的化学镀层(覆膜)的表面以接触电解镀液的状态通电,从而使前述电解镀液中所含的铜等金属在设置于阴极的前述化学镀处理所形成的化学镀层(覆膜)的表面析出,形成电解镀层(金属覆膜)。
作为前述电解镀液,例如可以举出:含有镍、铜、铬、锌、金、银、铝、铁、锡、钴、钯、铅、铂、镉、钨和铑等金属(需要说明的是,将这些金属也称为“构成金属镀层的金属”、“构成金属层的金属”)的硫化物、硫酸、以及水性介质者等。具体而言,可以举出含有硫酸铜、硫酸以及水性介质者。
前述电解镀液优选在20~98℃的范围内使用。
通过前述金属镀层处理形成的金属层的膜厚没有特别限定,例如优选0.1μm以上至优选500μm以下的范围。通过前述金属镀层处理形成的金属层的膜厚可以根据金属镀层处理工序中的处理时间、电流密度、镀覆用添加剂的用量等而调整。
通过以上的制造方法制造的本发明的层叠体在PAS成型品的粗糙化表面、即前述热塑性树脂(B)和前述碳酸盐(C)被去除而形成的孔隙中,通过金属镀层处理形成有金属膜,金属膜以高粘接力与PAS成型品粘接。因此,本发明的层叠体可以用于电气/电子领域中、电子电路、布线连接器、光缆用光连接器、蓝光光碟、DVD等光拾取器、电磁波屏蔽、柔性印刷电路板、非接触IC卡等RFID、薄膜电容器等各种构件。另外,包含汽车的机械领域中,可以用于轴承构件、滑动构件、灯反射器、电装构件、电磁波屏蔽构件、电气发动机周边构件、电池构件、换热机构件、激光打印机等的加压辊、用水(水管配管)等。另外,PAS成型品的粗糙化表面不易产生位置所导致的孔隙不均,粘接力的均匀性优异,因此,也优选用于在具有三维形状的PAS成型品上层叠有金属层的层叠体等具有复杂形状的PAS成型品。
实施例
以下,根据实施例对本发明详细地进行说明,但本发明不限定于下述的实施例。需要说明的是,份、%没有特别限定的情况下,记作质量基准。
(PPS树脂的熔融粘度的测定)
使用高化式流动试验仪(岛津制作所、CFT-500D),在300℃、载荷:1.96×106Pa、L/D=10(mm)/1(mm)下,将下述制造例中制造的PPS树脂保持6分钟后测定熔融粘度。
〔实施例1~12、比较例1~8〕
(PAS成型品的制造工序)
依据表1~5中记载的组成成分和配混量(全部为质量份),将除玻璃纤维之外的各材料在滚筒中均匀地混合。之后,向带排气口的双螺杆挤出机(日本制钢所、TEX30α)的投入口(顶部喂料机)中投入前述配混材料,从侧喂料机投入玻璃纤维,将树脂成分排出量设定为30kg/小时、螺杆转速设定为220rpm、设定树脂温度设定为320℃进行熔融混炼,切割从排出口排出的股线状物,得到粒料。
接着,将上述粒料供给至机筒温度设定为310℃的住友重机制注射成型机(SE75D-HP),使用模具温度调节温度至140℃的图5所示的L字型成型用模具进行注射成型,得到L字型的成型品。
(对PAS成型品的粗糙化处理工序)
使上述中得到的成型品浸渍于化学蚀刻处理液中3~20分钟后提起,在成型品形成粗糙化表面。
(对PAS成型品的金属镀层处理工序)
接着,对上述中得到的形成有粗糙化表面的PAS成型品的粗糙化表面以以下方法实施化学镀铜。以55℃浸渍于化学镀铜液(奥野制药株式会社制“OIC Cover、pH12.5)中20分钟,形成化学镀铜膜(厚度0.5μm)。
接着,将上述中得到的化学镀铜的表面设置于阴极、含磷铜设置于阳极,使用包含硫酸铜的电镀液,以电流密度2.5A/dm2进行30分钟电镀,从而在化学镀铜膜的表面层叠厚度15μm的镀铜层。作为前述电镀液,使用的是:硫酸铜70g/升、硫酸200g/升、氯离子50mg/升、TOP Lucina SF(奥野制药工业株式会社制的光泽剂)5g/升。
通过上述方法,得到在PAS成型品的粗糙化表面通过金属镀层处理形成有金属层的层叠体。
〔测定例〕
<镀层粘接性(密合性)的测定>
使用JIS Z 1522中规定的粘合带(粘合力:单位宽25mm为约8N、公称宽度:12~19mm、Nichiban Co.,Ltd.制Cellotape(注册商标)No.405)进行划格试验。即,按照如下步骤进行。首先,在用锐利的刀具制成以可以形成1边为2mm的正方形3×6=18网格的方式到达坯料的条痕的内侧底面与内侧侧面的各镀覆面,在带端残留不与坯料粘附的部分30~50mm,且将带中央放置于网格上,以用手指使带铺平的方式进行贴合。此时边注意不产生气泡边以20N/cm2强力地持续按压约10秒。
在1分钟以内,举起带端的不粘附而残留的部分,以相对于镀覆面为90°的角度以200cm/秒的速度进行剥离。
分别评价内侧底面的18网格、内侧侧面的18网格。表中,“0/18”是指剥离了的网格为0个,“18/18”是指剥离了的网格为18个。需要说明的是,18网格内、剥离面越少,评价为粘接力越大。
将实施例1~12、比较例1~5中实施的PPS树脂组合物的组成、形成层叠体的金属层的粘接性试验的评价结果示于表1~4。
[表1]
※1剥离了的网格数/18网格[表2]
[表3]
[表4]
(使用原料)
以下中,示出成为PAS树脂组合物的原料的各成分和化学蚀刻处理液。
·PAS树脂
(A)线型PPS(基于ASTM D1238-86的MFR:600g/10分钟)
·除PAS树脂以外的热塑性树脂
(B1-1)烯烃系聚合物“Bondfast 7L”(乙烯-马来酸酐-甲基丙烯酸缩水甘油酯共聚物)、住友化学株式会社制
(B1-2)烯烃系聚合物“Engage8842”(乙烯-α-烯烃聚合物)、Dow Inc.制
(B2-1)聚酰胺树脂“AMODEL A-1004”、Amodel Specialty polymers株式会社制
(B2-2)聚碳酸酯树脂“Iupilon MB4304R”、三菱化学株式会社制
·碳酸盐
(C-1)碳酸钙“碳酸钙NS#2300”(平均粒径※3 1.0μm)、日东粉化工业株式会社制
(C-2)碳酸钙“碳酸钙1级”(平均粒径※3 6.4μm)、三共制粉株式会社制
(C-3)碳酸镁(合成菱镁矿)“MAGTHERMO MS-S(平均粒径※3 1.2μm)、神岛化学工业株式会社制”
平均粒径※3是使用基于岛津制作所制、粉体比表面积测定装置SS-100型的每1g粉末的比表面积值,由计算式(平均粒径=6/(比重×比表面积)×10000〔μm〕)计算出的粉末的平均粒径。
·蜡
(D-1)高密度聚乙烯蜡“Luwax AH-6”BASF株式会社制
(D-2)马来酸酐聚乙烯“Recolve CE-2”Clariant Japan Co.,Ltd.制
(d-3)季戊四醇脂肪酸酯“LOXIOL VPG-861”Green Polymer Additives Co.,Ltd.制
(d-4)褐煤酸酯蜡“Licolub WE-40”Clariant Japan Co.,Ltd.制
·其他
(E-1)玻璃纤维“T-717H”(纤维长度3mm、平均直径10μm)日本电气硝子株式会社制
·化学蚀刻处理
F-1:使铬酸酐400g溶解于200ml的96%浓硫酸。进一步用水稀释,使整体为1升。
F-2:使氟化铵100g溶解于600ml的67%硝酸水溶液,进一步加入稀释水,使整体为1升。
Claims (23)
1.一种层叠体的制造方法,其特征在于,具备如下工序:对将聚芳硫醚树脂组合物成型而成的成型品的表面以化学蚀刻处理进行粗糙化处理的工序;对经粗糙化处理的所述成型品表面进行金属镀层处理的工序,
所述聚芳硫醚树脂组合物中配混有:
聚芳硫醚树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除聚芳硫醚树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)。
2.根据权利要求1所述的层叠体的制造方法,其中,对支撑体表面以化学蚀刻处理进行粗糙化处理的工序是使包含强酸或其盐的蚀刻液与所述PAS成型品的表面接触的工序。
3.根据权利要求1或2所述的层叠体的制造方法,其中,碳酸盐(C)是平均粒径0.3μm以上至6μm以下的范围的粒状物。
4.根据权利要求1~3中任一项所述的层叠体的制造方法,其中,碳酸盐(C)为选自由碳酸钙、碳酸镁、碳酸钾、碳酸钠、碳酸氢钠、碳酸铵、碳酸钡、碳酸锂、碳酸铜、碳酸亚铁、碳酸银、碳酸锰、碳酸锌、白云石和水菱镁矿组成的组中的至少1者。
5.根据权利要求1~4中任一项所述的层叠体的制造方法,其中,所述层叠体还包含纤维状填充剂。
6.根据权利要求1~5中任一项所述的层叠体的制造方法,其中,金属镀层处理为电解镀法、化学镀法和它们的组合。
7.根据权利要求1~6中任一项所述的层叠体的制造方法,其中,构成金属镀层的金属为由镍、铜、铬、锌、铁、金、银、铝、锡、钴、钯、铅、铂、镉和铑组成的组中的至少1种。
8.一种层叠体,其特征在于,在将聚芳硫醚树脂组合物成型而成的成型品的经粗糙化的表面层叠有金属层,
所述聚芳硫醚树脂组合物中配混有:
聚芳硫醚树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除聚芳硫醚树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)。
9.根据权利要求8所述的层叠体,其中,碳酸盐(C)是平均粒径0.3μm以上至6μm以下的范围的粒状物。
10.根据权利要求8或9所述的层叠体,其中,碳酸盐(C)为选自由碳酸钙、碳酸镁、碳酸钾、碳酸钠、碳酸氢钠、碳酸铵、碳酸钡、碳酸锂、碳酸铜、碳酸亚铁、碳酸银、碳酸锰、碳酸锌、白云石和水菱镁矿组成的组中的至少1者。
11.根据权利要求8~10中任一项所述的层叠体,其还包含纤维状填充剂。
12.根据权利要求8~11中任一项所述的层叠体,其中,构成金属层的金属为由镍、铜、铬、锌、铁、金、银、铝、锡、钴、钯、铅、铂、镉和铑组成的组中的至少1种。
13.一种聚芳硫醚树脂组合物的制造方法,其特征在于,具备如下工序:将聚芳硫醚树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除聚芳硫醚树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)配混并熔融混炼。
14.根据权利要求13所述的聚芳硫醚树脂组合物的制造方法,其中,碳酸盐(C)是平均粒径0.3μm以上至6μm以下的范围的粒状物。
15.根据权利要求13或14所述的聚芳硫醚树脂组合物的制造方法,其中,碳酸盐(C)为选自由碳酸钙、碳酸镁、碳酸钾、碳酸钠、碳酸氢钠、碳酸铵、碳酸钡、碳酸锂、碳酸铜、碳酸亚铁、碳酸银、碳酸锰、碳酸锌、白云石和水菱镁矿组成的组中的至少1者。
16.根据权利要求13~15中任一项所述的聚芳硫醚树脂组合物的制造方法,其中,所述聚芳硫醚树脂组合物还包含纤维状填充剂。
17.一种成型品的制造方法,其具备如下工序:将以权利要求13~15中任一项所述的制造方法制造的聚芳硫醚树脂组合物进行熔融成型。
18.一种聚芳硫醚树脂组合物,其特征在于,其是配混聚芳硫醚树脂(A)、选自由热塑性弹性体(b1)和具有水解性的热塑性树脂(b2)组成的组中的除聚芳硫醚树脂以外的热塑性树脂(B)、碳酸盐(C)和聚烯烃系蜡(D)而成的。
19.根据权利要求18所述的聚芳硫醚树脂组合物,其中,所述聚芳硫醚树脂组合物中,相对于聚芳硫醚树脂(A)100质量份,所述热塑性树脂(B)为5质量份以上至70质量份以下的范围,碳酸盐(C)为10质量份以上至90质量份以下的范围,聚烯烃系蜡(D)为0.01质量份以上至10质量份以下的范围。
20.根据权利要求18或19所述的聚芳硫醚树脂组合物,其中,碳酸盐(C)是平均粒径0.3μm以上至6μm以下的范围的粒状物。
21.根据权利要求18~20中任一项所述的聚芳硫醚树脂组合物,其中,碳酸盐为选自由碳酸钙、碳酸镁、碳酸钾、碳酸钠、碳酸氢钠、碳酸铵、碳酸钡、碳酸锂、碳酸铜、碳酸亚铁、碳酸银、碳酸锰、碳酸锌、白云石和水菱镁矿组成的组中的至少1者。
22.根据权利要求18~21中任一项所述的聚芳硫醚树脂组合物,其还包含纤维状填充剂。
23.一种成型品,其是将权利要求18~22中任一项所述的聚芳硫醚树脂组合物进行熔融成型而成的。
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KR20220101661A (ko) | 2022-07-19 |
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