CN110225821A - 金属/树脂复合结构体及其制造方法 - Google Patents
金属/树脂复合结构体及其制造方法 Download PDFInfo
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- CN110225821A CN110225821A CN201780084880.7A CN201780084880A CN110225821A CN 110225821 A CN110225821 A CN 110225821A CN 201780084880 A CN201780084880 A CN 201780084880A CN 110225821 A CN110225821 A CN 110225821A
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- resin
- metal
- polyarylene sulfide
- component
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 17
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/263—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by a layer having non-uniform thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/40—Applying molten plastics, e.g. hot melt
- B29C65/405—Applying molten plastics, e.g. hot melt characterised by the composition of the applied molten plastics
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/20—Bonding
- B23K26/32—Bonding taking account of the properties of the material involved
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C45/14311—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles using means for bonding the coating to the articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
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Abstract
提供经表面粗糙化的金属构件与由聚芳硫醚(PAS)树脂组合物构成的树脂构件接合而成的密合力优异的金属/树脂复合结构体;其中使用的流动性优异、呈现优异的密合力的PAS树脂组合物;及呈现优异的密合力的树脂构件及它们的制造方法。更详细而言提供以相对于PAS树脂(A)100质量份、酚醛树脂(B)为0.05~20质量份的范围包含所述树脂(A)和树脂(B)的PAS树脂组合物;将其熔融成形而成的树脂构件;及经表面粗糙化的金属构件与由前述PAS树脂组合物构成的树脂构件接合而成的金属/树脂复合结构体;以及它们的制造方法,前述金属构件为铝、铜、镁、铁、钛或含有它们的合金。
Description
技术领域
本发明涉及金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的金属/树脂复合结构体、其制造方法、以及金属/树脂复合结构体中使用的树脂组合物及树脂构件。
背景技术
从各种部件的轻量化的观点出发,使用了高耐热性的树脂构件作为金属构件替代品。但是,因机械强度等问题而难以用树脂代替全部金属构件的情况下,使用将金属构件和该树脂构件接合一体化而得到的复合结构体(以下,称为金属/树脂复合结构体)。作为这样的金属/树脂复合结构体,例如,可列举出对金属构件表面进行激光照射,形成微小的凹部,从而利用锚固效果与由聚芳硫醚树脂构成的树脂构件接合的方法(专利文献1、2)。通过激光照射形成的金属构件表面非常粗糙,因此与树脂的接合面的摩擦力会增大,对于在与接合面同方向起作用的剪切力而言,会保持耐久性。但是存在如下问题:进行冷热循环试验时,随着树脂的膨胀-收缩,在亚微米级容易发生界面剥离,因此,金属成形体与树脂成形体的密合力、特别是实施冷热循环时的密合力(称为耐冷热循环性)低。
因此,对与由聚芳硫醚树脂构成的树脂构件接合的前述金属构件表面通过激光照射形成凹部时,在该金属构件表面与该凹部侧面所成的角为10~55℃的范围进行,由此能够提供具有高的密合力、特别优异的耐冷热循环性的金属树脂接合成形品(参照专利文献3)。但是,该金属树脂接合成形品是通过将树脂流入到金属构件的凹部从而在固化后形成卡住的部位来得到优异的密合力,因此,为了向金属构件的凹部的流入变得更容易,要求流动性更高的树脂材料。
关于树脂构件的改良,例如,已知有如下而成的复合体:在通过侵蚀性水溶液或侵蚀性悬浮液等化学溶液处理而在表面具有数均内径10~80nm的凹部的铝合金或镁合金上、或在通过阳极氧化法进行处理而在表面具有数均内径10~80nm的凹部的铝合金上,对包含聚苯硫醚与特定比例的选自由马来酸酐改性乙烯系共聚物、甲基丙烯酸缩水甘油酯改性乙烯系共聚物、缩水甘油醚改性乙烯系共聚物及乙烯烷基丙烯酸酯系共聚物组成的组中的1种以上的聚烯烃系树脂的树脂组合物进行注射成形,该树脂组合物在浸入于凹部的状态下固着(参照专利文献5)。对于通过任意处理法形成的金属表面的微细的凹部而言,其内径都非常微细,因此树脂组合物难以浸入,因此不能说金属部件与由树脂组合物构成的树脂构件的密合力充分。
因此,对于基于激光加工、侵蚀性水溶液或侵蚀性悬浮液的处理法、阳极氧化法等,无论其手段如何,为了使树脂材料容易向通过表面粗糙化形成的微细凹凸部浸入,均要求开发流动性更优异的树脂材料。
现有技术文献
专利文献
专利文献1:国际公开2007/072603小册子
专利文献2:日本特开2010-167475号公报
专利文献3:日本特开2013-107273号公报
专利文献4:日本特开2015-100959号公报
专利文献5:日本特开2007-050630号公报
发明内容
发明要解决的问题
因此,本发明要解决的课题在于,提供经表面粗糙化的金属构件与高耐热性的由聚芳硫醚树脂组合物构成的树脂构件接合而成的密合力优异的金属/树脂复合结构体及其制造方法。进而,本发明还在于,提供流动性优异、作为其成形体的树脂构件能够对在表面形成有微细凹凸部的金属部件呈现优异的密合力的聚芳硫醚树脂组合物、及将其熔融成形而成的、能够对在表面形成有微细凹凸部的金属部件呈现优异的密合力的树脂构件。
用于解决问题的方案
本申请发明人等进行了各种研究,结果发现,在聚芳硫醚树脂中配混酚醛树脂而成的聚芳硫醚树脂组合物的流动性优异、并且能够提供对在表面形成有微细凹凸部的金属部件呈现优异的密合力的树脂构件,从而解决了本发明。
即,本发明涉及一种金属/树脂复合结构体,其特征在于,其是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的金属/树脂复合结构体,
前述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
前述聚芳硫醚树脂组合物是将下述树脂组合物成形而成的,所述树脂组合物以相对于聚芳硫醚树脂(A)100质量份、酚醛树脂(B)为0.05~20质量份的范围包含前述聚芳硫醚树脂(A)和前述酚醛树脂(B)。
另外,本发明涉及一种金属/树脂复合结构体的制造方法,其特征在于,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
前述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
所述制造方法中,对于金属构件,将包含聚芳硫醚树脂(A)和酚醛树脂(B)的聚芳硫醚树脂组合物在前述聚芳硫醚树脂(A)的熔点以上熔融成形。
另外,本发明涉及一种聚芳硫醚树脂组合物,其特征在于,其用于金属/树脂复合结构体,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
前述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
前述聚芳硫醚树脂组合物是将聚芳硫醚树脂(A)和酚醛树脂(B)作为必需成分配混而成的,相对于前述聚芳硫醚树脂(A)100质量份,前述酚醛树脂(B)为0.05~20质量份的范围。
另外,本发明涉及一种树脂构件,其特征在于,其用于金属/树脂复合结构体,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
前述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
前述聚芳硫醚树脂组合物是将聚芳硫醚树脂(A)和酚醛树脂(B)作为必需成分配混而成的,相对于前述聚芳硫醚树脂(A)100质量份,前述酚醛树脂(B)为0.05~20质量份的范围,
前述树脂构件是将聚芳硫醚树脂组合物熔融成形而得到的。
发明的效果
根据本发明,提供经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的密合力优异的金属/树脂复合结构体及其制造方法。进而本发明能够提供流动性优异、作为其成形体的树脂构件能够对在表面形成有微细凹凸部的金属部件呈现优异的密合力的聚芳硫醚树脂组合物、及将其熔融成形而成的能够对在表面形成有微细凹凸部的金属部件呈现优异的密合力的树脂构件。
附图说明
图1为相对于金属构件表面为垂直方向的截面图,为用于示出微细凹凸面的测定基准的说明图。
具体实施方式
本发明的金属/树脂复合结构体的特征在于,其是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
前述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
前述聚芳硫醚树脂组合物是将下述树脂组合物成形而成的,所述树脂组合物以相对于聚芳硫醚树脂(A)100质量份、酚醛树脂(B)为0.05~20质量份的范围包含前述聚芳硫醚树脂(A)和前述酚醛树脂(B)。
(金属构件)
构成本发明的金属/树脂复合结构体的金属构件在与由聚芳硫醚树脂组合物构成的树脂构件接合的金属构件表面(以下,简称为金属构件表面)具有微细的凹凸面(以下,简称为微细凹凸面)。
对于本发明的金属/树脂复合结构体,本发明中使用的聚芳硫醚树脂组合物以熔融的状态进入到前述微细凹凸面的凹部并固化,从而金属构件与由该树脂组合物构成的树脂构件接合,形成金属构件与树脂构件的界面(以下,简称为金属-树脂界面)。
本发明中使用的金属构件通过表面粗糙化而在金属构件料面形成有微细凹凸面,对于其凹凸部的间隔,从凸部到邻接的凸部(以下,称为凸部间距)的长度优选为5nm以上的范围、更优选为10nm以上的范围。对于上限值而言,由于即使流动性低也能够流入,因此没有特别限定,若凹凸密度高,则有密合力也提高的倾向,因此优选700μm以下的范围、更优选500μm以下的范围。若凸部间距的长度处于上述范围内,则本发明中使用的聚芳硫醚树脂组合物能够密合性良好地进入到微细凹凸面的凹部,能够在金属-树脂界面发挥优异的密合力。进而若凹凸部的间隔有周期性,则能够在金属-树脂界面发挥更优异的密合力,因此优选。
另外,关于凹凸部的高低差,优选为50nm以上、更优选为100nm以上的范围。越存在高低差,越有密合强度提高的倾向,但考虑向凹凸部填充树脂以使不产生空隙等时,优选500μm以下。
需要说明的是,该凸部间距的长度可以如下来求出:基于利用电子显微镜或激光显微镜对沿金属构件表面的相对于微细凹凸面垂直的方向切断的截面进行拍摄而得到的照片,在凸部的顶上部到邻接的凸部的顶上部的2点间选出至少50点,然后测定金属构件表面的与微细凹凸面平行的方向的部分的长度(图1的符号x),以其数均值的形式而求出。另外,凹凸部的高低差可以如下来求出:基于利用电子显微镜或激光显微镜对前述截面进行拍摄而得到的照片,在凸部的顶上部到邻接的凹部的底面部的2点间选出至少50点,测定金属构件表面的与微细凹凸面垂直的方向的部分的长度(图1的符号y),以其数均值的形式求出。
另外,前述微细凹凸面的凹凸形状没有特别限定,可以以通过后述表面粗糙化而具有比前述凸部间距的距离小的孔径的凹部的形式来形成,也可以为进而进行表面粗糙化从而以林立状态观测到的具有立体表面的突起物的形状,所述立体表面为带有圆形的凸部、即、球状、具有光滑的端部的圆柱或疣状、花林糖状等。
作为构成前述金属构件的金属的种类,可列举出铝、铜、镁、铁、钛或含有它们的合金。更具体而言,可列举出铁、例如,不锈钢、钢材等以铁为主成分、即以20质量%以上、更优选50质量%以上、进一步优选80质量%的比例包含铁、此外还包含碳、硅、锰、铬、钨、钼、磷、钛、钒、镍、锆、硼等的合金(以下,记为铁合金)、铝、以铝为主成分、此外还包含铜、锰、硅、镁、锌、镍的合金(以下,记为铝合金)、镁、以镁为主成分、此外还包含锌、铝、锆等的合金(以下,记为镁合金)、铜、以铜为主成分、此外还包含锌、锡、磷、镍、镁、硅、铬的合金(以下,记为铜合金)、钛、以钛为主成分、此外还包含铜、锰、硅、镁、锌、镍的合金(以下,记为钛合金)。其中,更优选可列举出铁、铁合金、铝合金、镁合金、铜合金、钛合金,进一步可列举出优选铁合金、铝合金、镁合金。
本发明中使用的金属构件优选进行了表面粗糙化从而在表面具有微细凹凸面。表面粗糙化的方法可以没有特别限定地使用公知的方法,例如,可列举出3种方法。
(1)利用侵蚀性水溶液或侵蚀性悬浮液的浸渍法。优选设为在金属表面形成有微细凹凸面的形状,进而更优选采用在金属表面形成有多个凹部的形状、并且将其凹部设为数均内径3μm以下的范围,同样地进一步优选将其凹部设为数均内径10nm~3μm的范围。
(2)阳极氧化法。优选在表面主要形成金属氧化物层,由此在其表面层形成多个具有数均内径1μm以下的范围的开口部,更优选同样形成具有数均内径1nm~1μm的范围的开口部,进而更优选同样形成具有数均内径10~200nm的范围的开口部。
(3)通过对利用机械切削、例如金刚石磨粒研削或喷丸加工制作的具有凹凸的模具冲头进行压制从而在金属表面形成凹凸的方法;通过喷砂、激光加工在金属表面制作凹凸形状的方法。主要优选将表面加工成多个凹部,对于凹部的数均内径或激光加工等形成连续形状的凹部的情况下,其宽度优选设为1~1000μm的范围、进而更优选设为10~800μm的范围。
前述金属构件优选在形成上述微细凹凸面前通过切断加工、基于压制等的塑性加工、冲切加工、切削、研削、放电加工等除肉加工来将上述金属构件加工成规定的形状。
需要说明的是,可以在进行了金属表面处理的金属构件的表面形成底漆层。构成底漆层的材料没有特别限定,通常由包含树脂成分的底漆树脂材料形成。底漆树脂材料没有特别限定,可以使用公知的底漆树脂材料。具体而言,可列举出公知的聚烯烃系底漆、环氧系底漆、氨基甲酸酯系底漆等。底漆层的形成方法没有特别限定,例如,可以将上述底漆树脂材料的溶液、上述底漆树脂材料的乳液涂布于进行了上述表面处理的金属构件来形成。作为制成溶液时使用的溶剂,可列举出甲苯、甲乙酮(MEK)、二甲基甲酰胺(DMF)等。作为乳液用的介质,可列举出脂肪族烃介质、水等。
本发明中使用的聚芳硫醚树脂组合物是将聚芳硫醚树脂(A)作为必需成分配混而成的。
本发明中使用的聚芳硫醚树脂(A)具有将芳香族环与硫原子键合而成的结构作为重复单元的树脂结构,具体而言,为将下述通式(1)所示的结构部位和进一步根据需要的下述通式(2)所示的3官能性的结构部位作为重复单元的树脂。
(式中,R1及R2各自独立地表示氢原子、碳原子数1~4的范围的烷基、硝基、氨基、苯基、甲氧基、乙氧基。)
式(2)所示的3官能性的结构部位相对于其与其它结构部位的合计摩尔数优选为0.001~3摩尔%的范围、特别优选为0.01~1摩尔%的范围。
此处,对于前述通式(1)所示的结构部位,从前述聚芳硫醚树脂的机械强度的方面出发,特别优选该式中的R1及R2为氢原子,该情况下,可以举出下述式(3)中所示的在对位进行键合的结构、及下述式(4)中所示的在间位进行键合的结构。
这些当中,特别是重复单元中的硫原子对芳香族环的键合为前述通式(3)中所示的在对位进行键合的结构时,在前述聚芳硫醚树脂的耐热性、结晶性的方面是优选的。
此外,前述聚芳硫醚树脂也可以不仅包含前述通式(1)、(2)所示的结构部位,还以与前述通式(1)与通式(2)所示的结构部位的合计的30摩尔%以下的量包含下述的结构式(5)~(8)所示的结构部位。
特别是本发明中上述通式(5)~(8)所示的结构部位为10摩尔%以下时,从聚芳硫醚树脂的耐热性、机械强度的方面出发是优选的。前述聚芳硫醚树脂中包含上述通式(5)~(8)所示的结构部位的情况下,作为它们的键合方式,可以为无规共聚物、嵌段共聚物中的任意种。
另外,前述聚芳硫醚树脂可以在其分子结构中具有萘基硫醚键等,相对于与其它结构部位的合计摩尔数,优选为3摩尔%以下、特别优选为1摩尔%以下。
另外,聚芳硫醚树脂的物性只要不损害本发明的效果,就没有特别限定,如下。
(熔融粘度)
对于本发明中使用的聚芳硫醚树脂(A),在300℃下测定的熔融粘度(V6)优选为2~1000〔Pa·s〕的范围,进而从流动性及机械强度的平衡良好的方面出发,更优选10~500〔Pa·s〕的范围,特别优选为60~200〔Pa·s〕的范围。其中,本发明中,熔融粘度(V6)为使用岛津制作所制造的流动试验仪CFT-500D,在300℃、载荷:1.96×106Pa、L/D=10(mm)/1(mm)下将聚芳硫醚树脂保持6分钟后测定熔融粘度所得的值。
(非牛顿指数)
对于本发明中使用的聚芳硫醚树脂(A)的非牛顿指数,只要不损害本发明的效果就没有特别限定,优选为0.90~2.00的范围。在使用线型聚芳硫醚树脂的情况下,非牛顿指数优选为0.90~1.50的范围、进而更优选为0.95~1.20的范围。这样的聚芳硫醚树脂的机械物性、流动性、耐磨耗性优异。其中,非牛顿指数(N值)是使用毛细管流变仪,在300℃、孔长度(L)与孔直径(D)之比为L/D=40的条件下测定剪切速度及剪切应力,使用下述式而算出的值。
SR=K·SSN
[其中,SR表示剪切速度(秒-1),SS表示剪切应力(达因/cm2),并且K表示常数。],示出了N值越接近1,PPS为越接近线状的结构,N值越高,为支链越多的结构。
(制造方法)
作为前述聚芳硫醚树脂(A)的制造方法,没有特别限定,例如可以举出:1)在硫和碳酸钠的存在下,使二卤代芳香族化合物、以及根据需要加入的多卤代芳香族化合物和/或其他共聚成分进行聚合的方法;2)在极性溶剂中,在硫化剂等的存在下,使二卤代芳香族化合物、以及根据需要加入的多卤代芳香族化合物和/或其他共聚成分进行聚合的方法;3)使对氯苯硫酚、以及根据需要加入的其他共聚成分进行自缩合的方法等。这些方法中,2)的方法通用而优选。在反应时,为了调节聚合度,可以添加羧酸、磺酸的碱金属盐、碱金属或碱土金属的氢氧化物。上述2)方法中,特别优选采用如下方法得到:在经过加热的包含有机极性溶剂和二卤代芳香族化合物的混合物中以能够从反应混合物去除水的速度导入含水硫化剂,在有机极性溶剂中,使二卤代芳香族化合物、硫化剂、和根据需要加入的多卤代芳香族化合物进行反应,以及将反应体系内的水分量控制在相对于该有机极性溶剂1摩尔为0.02~0.5摩尔的范围,从而制造聚芳硫醚树脂的方法(参照日本特开平07-228699号公报);在固体的碱金属硫化物及非质子性极性有机溶剂的存在下,加入二卤代芳香族化合物、以及根据需要的多卤代芳香族化合物和/或其他共聚成分,一边将碱金属硫氢化物及有机酸碱金属盐控制为相对于1摩尔硫源为0.01~0.9摩尔范围的有机酸碱金属盐及将反应体系内的水分量控制在相对于1摩尔非质子性极性有机溶剂为0.02摩尔以下的范围,一边进行反应的方法(参照WO2010/058713号小册子)。作为二卤代芳香族化合物的具体例,可以举出对二卤代苯、间二卤代苯、邻二卤代苯、2,5-二卤代甲苯、1,4-二卤代萘、1-甲氧基-2,5-二卤代苯、4,4’-二卤代联苯、3,5-二卤代苯甲酸、2,4-二卤代苯甲酸、2,5-二卤代硝基苯、2,4-二卤代硝基苯、2,4-二卤代苯甲醚、p,p’-二卤代二苯基醚、4,4’-二卤代二苯甲酮、4,4’-二卤代二苯基砜、4,4’-二卤代二苯基亚砜、4,4’-二卤代二苯基硫醚、及上述各化合物的芳香环上具有碳原子数1~18范围的烷基的化合物,作为多卤代芳香族化合物,可以举出1,2,3-三卤代苯、1,2,4-三卤代苯、1,3,5-三卤代苯、1,2,3,5-四卤代苯、1,2,4,5-四卤代苯、1,4,6-三卤代萘等。另外,对于上述各化合物中所含的卤素原子,理想的为氯原子、溴原子。
作为利用聚合工序得到的包含聚芳硫醚树脂的反应混合物的后处理方法,没有特别限制,例如可以举出如下方法:(1)聚合反应结束后,首先,将反应混合物直接或者在加入酸或碱之后,在减压下或常压下蒸馏去除溶剂,接着将蒸馏去除溶剂后的固体物用水、反应溶剂(或相对于低分子聚合物具有同等溶解度的有机溶剂)、丙酮、甲乙酮、醇类等溶剂洗涤1次或2次以上,进而进行中和、水洗、过滤及干燥的方法;或者(2)聚合反应结束后,向反应混合物中添加水、丙酮、甲乙酮、醇类、醚类、卤化烃、芳香族烃、脂肪族烃等溶剂(可溶于使用的聚合溶剂、并且至少相对于聚芳硫醚为不良溶剂的溶剂)作为沉降剂,使聚芳硫醚、无机盐等固体状产物沉降,将它们滤出、洗涤、干燥的方法;或者(3)聚合反应结束后,向反应混合物中加入反应溶剂(或相对于低分子聚合物具有同等溶解度的有机溶剂)进行搅拌后,过滤并去除低分子量聚合物,然后用水、丙酮、甲乙酮、醇类等溶剂洗涤1次或2次以上,之后进行中和、水洗、过滤及干燥的方法;(4)聚合反应结束后,在反应混合物中加入水进行水洗涤、过滤,根据需要在水洗涤时加入酸进行酸处理并干燥的方法;(5)聚合反应结束后,过滤反应混合物,根据需要,用反应溶剂洗涤1次或2次以上,进而进行水洗涤、过滤及干燥的方法;等。
需要说明的是,如上述(1)~(5)中所例示的那样的后处理方法中,聚芳硫醚树脂的干燥可以在真空中进行,也可以在空气中或氮气那样的非活性气体气氛中进行。
本发明中使用的聚芳硫醚树脂组合物是将酚醛树脂(B)作为必需成分配混而成的。
接着,本发明中使用的酚醛树脂是指具有酚骨架的热塑性聚合物,酚醛清漆型酚醛树脂或双酚型酚醛树脂中的任意者可以作为优选的例子来使用,进而更优选酚醛清漆型酚醛树脂。
酚醛树脂通常通过使酚化合物和醛化合物在酸催化剂的存在下、在40~150℃反应1~5小时,接着经过常压脱水、或减压脱水工序而将残留的水分从反应体系内去除,进而将反应体系内存在的缩合物溶解于甲醇等溶剂来获得。〔醛化合物〕/〔酚化合物〕的比率在公知的范围内没有特别限制,优选以摩尔比计为0.3~1.0的范围。该酚骨架源自原料的酚化合物。作为该酚化合物,在公知的范围内没有特别限定,例如可列举出苯酚、萘酚或甲酚、二甲酚、乙基苯酚、丁基苯酚、辛基苯酚等烷基酚类;间苯二酚、儿茶酚等多元酚类;双酚A、双酚F、双酚S、双酚E、硫代双酚、双(羟基苯基)醚、二羟基二苯甲酮、双酚芴等双酚类;卤代酚、苯基酚、氨基酚等。另外,这些酚化合物在其使用时不仅限定于1种,也可以是2种以上的组合使用。
前述醛化合物只要为酚醛树脂制造时通常使用的醛化合物,就可以没有特别限制地使用,可列举出甲醛、多聚甲醛、三聚甲醛(trioxane)等甲醛、乙醛等,另外,也可以使用六亚甲基四胺。
作为前述酸催化剂,可以使用酚醛清漆型酚醛树脂的制造中使用的酸类,例如,可列举出甲酸、盐酸、磷酸、硫酸、对甲苯磺酸、苯酚磺酸等。
酚醛树脂的配混能够使聚芳硫醚树脂组合物的粘度更低、能够提高成形时的流动性,因此该组合物能够流入到金属构件的粘接表面的凹凸的细部从而增大锚固效果。进而,因羟基的存在而能够在金属构件的粘接表面形成多个氢键从而提高密合力。进而,即使在高温高湿环境下,也能够抑制水分向该粘接表面的浸入,表现出高的粘接保持率。
酚醛树脂的羟基当量优选较高,其范围可以为公知的范围,从能进一步提高粘接力或密合力的方面出发,优选为80~200g/当量的范围、更优选为100~180g/当量的范围、进一步优选为110~150g/当量的范围。
酚醛树脂可以为固体型、溶剂型中任意者,更优选使用固体型。使用固体型时,优选使用软化点为50~180℃的范围的物质、更优选使用为70~150℃的范围的物质。使用溶剂型时,优选使用粘度(制成固体成分60%MEK溶液)为50~2000(25℃、mPa·s)的范围的物质、更优选使用为70~1500(25℃、mPa·s)的范围的物质。
相对于聚芳硫醚树脂(A)100质量份,聚芳硫醚树脂组合物中的前述酚醛树脂(B)的配混的比例优选为0.05~20质量份的范围、优选为0.1~15质量份的范围、进而优选为0.5~10质量份的范围。为上述范围内时,能够兼顾优异的金属构件粘接性和熔融混炼时、熔融成形时的低气体性。
本发明的聚芳硫醚树脂组合物根据需要可以含有填充剂作为任选成分。作为这些填充剂,只要不损害本发明的效果,也可以使用公知惯用的材料,例如可以举出纤维状的材料、粒状、板状等非纤维状的材料等各种形状的填充剂等。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、芳纶纤维、金属纤维、钛酸钾、碳化硅、硅酸钙、硅灰石等纤维、天然纤维等纤维状填充剂,另外,也可以使用玻璃微珠、玻璃片、硫酸钡、粘土、叶蜡石、膨润土、绢云母、云母(マイカ)、云母(雲母)、滑石、绿坡缕石、铁氧体、硅酸钙、碳酸钙、碳酸镁、玻璃微珠、沸石、研磨纤维、硫酸钙等非纤维状填充剂。
本发明中,填充剂不是必需成分,在添加的情况下,其含量只要不损害本发明的效果就没有特别限定。作为填充剂的含量,例如相对于聚芳硫醚树脂(A)100质量份优选为1~600质量份的范围、进一步更优选为10~200质量份的范围。在所述范围中,树脂组合物表现出良好的机械强度和成形性,因此优选。
本发明的聚芳硫醚树脂组合物根据需要可以配混硅烷偶联剂作为任选成分。作为硅烷偶联剂,只要不损害本发明的效果就没有特别限定,可以举出具有与羧基反应的官能团、例如具有环氧基、异氰酸酯基、氨基或羟基的硅烷偶联剂作为优选例。作为这样的硅烷偶联剂,例如可以举出γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三乙氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷等含环氧基的烷氧基硅烷化合物;γ-异氰酸酯基丙基三甲氧基硅烷、γ-异氰酸酯基丙基三乙氧基硅烷、γ-异氰酸酯基丙基甲基二甲氧基硅烷、γ-异氰酸酯基丙基甲基二乙氧基硅烷、γ-异氰酸酯基丙基乙基二甲氧基硅烷、γ-异氰酸酯基丙基乙基二乙氧基硅烷、γ-异氰酸酯基丙基三氯硅烷等含异氰酸酯基的烷氧基硅烷化合物;γ-(2-氨基乙基)氨基丙基甲基二甲氧基硅烷、γ-(2-氨基乙基)氨基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷等含氨基的烷氧基硅烷化合物;γ-羟基丙基三甲氧基硅烷、γ-羟基丙基三乙氧基硅烷等含羟基的烷氧基硅烷化合物。本发明中,硅烷偶联剂不是必需成分,在添加的情况下,对于其配混的比例,只要不损害本发明的效果,就没有特别限定,相对于聚芳硫醚树脂(A)100质量份,优选为0.01~10质量份的范围、进一步更优选为0.1~5质量份的范围。在所述范围中,树脂组合物具有良好的耐电晕性和成形性、特别是具有脱模性,并且成形品呈现优异的与环氧树脂的粘接性,并且进而机械强度提高,因此优选。
本发明的聚芳硫醚树脂组合物根据需要可以配混热塑性弹性体作为任选成分。作为热塑性弹性体,可以举出聚烯烃系弹性体、氟系弹性体或有机硅系弹性体,其中可以举出聚烯烃系弹性体作为优选的例子。添加这些弹性体的情况下,其配混的比例只要不损害本发明的效果就没有特别限定,相对于聚芳硫醚树脂(A)100质量份,优选为0.01~30质量份的范围、进一步更优选为0.1~25质量份的范围。在所述范围中,得到的聚芳硫醚树脂组合物的耐冲击性提高,因此优选。
对于前述聚烯烃系弹性体,例如可以通过α-烯烃的均聚或不同的α-烯烃彼此的共聚来得到,进而,在赋予官能团的情况下,可以通过α-烯烃与具有官能团的乙烯基聚合性化合物的共聚来得到。α-烯烃例如可以举出乙烯、丙烯及1-丁烯等碳原子数2~8的范围的烯烃。另外,作为官能团,可以举出羧基、式-(CO)O(CO)-所示的酸酐基、它们的酯、环氧基、氨基、羟基、巯基、异氰酸酯基、或噁唑啉基等。
作为具有这样的官能团的乙烯基聚合性化合物的具体例,例如可以举出(甲基)丙烯酸及(甲基)丙烯酸酯等α,β-不饱和羧酸及其烷基酯、马来酸、富马酸、衣康酸及其它碳原子数4~10的α,β-不饱和羧酸及其衍生物(单酯或二酯、及其酸酐等)、以及(甲基)丙烯酸缩水甘油酯等。这些当中,从机械强度、特别是韧性及耐冲击性的提高的方面出发,具有选自由上述环氧基、羧基、及该酸酐基组成的组中的至少1种官能团的乙烯-丙烯共聚物及乙烯-丁烯共聚物是优选的。
需要说明的是,前述弹性体具有环氧基作为官能团的情况下,在熔融混炼时会与酚醛树脂反应,因此其配混的比例的上限值相对于聚芳硫醚树脂(A)100质量份优选为10质量份以下的范围、进而更优选为5质量份的范围,特别优选为0质量份,即实质上不使用这种具有环氧基的弹性体。
进而,本发明的聚芳硫醚树脂组合物除了上述成分以外,根据用途还可以含有除聚芳硫醚树脂(A)以外的合成树脂作为任意成分。作为该合成树脂,可列举出聚酯树脂、聚酰胺树脂、聚酰亚胺树脂、聚醚酰亚胺树脂、聚碳酸酯树脂、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、聚亚芳基树脂、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、氨基甲酸酯树脂、液晶聚合物等合成树脂等。这些树脂的配混的比例根据各自的目的而不同,不能一概而定,只要在相对于聚芳硫醚树脂(A)100质量份为0.01~1000质量份的范围内、不损害本发明的效果地根据目的、用途来适宜调整使用即可。
另外,本发明的聚芳硫醚树脂组合物此外还可以根据需要含有着色剂、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、脱模剂、防锈剂、及偶联剂等公知惯用的添加剂作为任选成分。这些添加剂不是必需成分,其配混的比例例如可以在相对于聚芳硫醚树脂(A)100质量份优选为0.01~1000质量份的范围内、不损害本发明效果地根据目的、用途来适宜调整而使用。
本发明的聚芳硫醚树脂组合物的制造方法中,配混聚芳硫醚树脂(A)和前述酚醛树脂(B)作为必需成分,并在聚芳硫醚树脂(A)的熔点以上进行熔融混炼。
对于本发明的聚芳硫醚树脂组合物的优选的制造方法,可以经过如下工序来制造:以使成为上述配混的比例,将聚芳硫醚树脂(A)、前述酚醛树脂(B)的各必需成分、和根据需要的填充剂等任意成分以粉末、粒料、细片等各种形态投入到螺带式混合机(ribbonblender)、亨舍尔混合机、V型混合机等中进行干混后,投入到班伯里密炼机、混合辊、单螺杆或双螺杆的挤出机及捏合机等公知的熔融混炼机中,在树脂温度为聚芳硫醚树脂(A)的熔点以上的温度范围、优选为熔点+10℃以上的温度范围、更优选为熔点+10℃~熔点+100℃的温度范围、进一步优选为熔点+20℃~熔点+50℃的温度范围内进行熔融混炼,从而制作。各成分向熔融混炼机中的添加、混合可以同时进行,也可以分开进行。
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,例如优选边适宜调整树脂成分的挤出量为5~500(kg/hr)的范围和螺杆转速为50~500(rpm)的范围边熔融混炼,进一步优选在它们的比率(挤出量/螺杆转速)为0.02~5(kg/hr/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投入至该挤出机内。对于所述侧喂料机的位置,从该挤出机树脂投入部至该侧喂料机的距离相对于前述双螺杆混炼挤出机的螺杆总长度的比率优选为0.1~0.9的范围。其中,特别优选为0.3~0.7的范围。
如此进行熔融混炼而得到的本发明的聚芳硫醚树脂组合物为包含作为必需成分的聚芳硫醚树脂(A)、前述酚醛树脂(B)、和根据需要加入的任意成分及源自它们的成分的熔融混合物,优选在该熔融混炼后,通过公知的方法加工成粒料、小片(chip)、颗粒、粉末等形态,然后根据需要在100~150℃的温度下实施预干燥,供于各种成形。
通过上述制造方法制造的本发明的聚芳硫醚树脂组合物形成具有如下结构的形态:以聚芳硫醚树脂(A)为基质,在该基质中分散有作为必需成分的前述酚醛树脂(B)、源自它们的成分、根据需要添加的任意成分。可以认为本发明中使用的聚芳硫醚树脂组合物通过添加酚醛树脂来破坏作为基质的聚芳硫醚树脂的结晶性从而降低结晶化温度,由此能够提高熔融时的流动性,其结果可以认为能够润湿性良好地进入通过表面粗糙化处理而形成于金属构件的微细凹凸部的凹部,能够在金属-树脂界面发挥更优异的粘接性。由于该粘接性的效果是利用锚固效果这样的物理保持力保持金属-树脂界面的原理,因此只要金属构件被表面粗糙化,则金属自身无论材质如何都能够没有问题地发挥其效果。
对于本发明的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的金属/树脂复合结构体,可以通过对于金属构件,将包含聚芳硫醚树脂(A)和酚醛树脂(B)的聚芳硫醚树脂组合物在前述聚芳硫醚树脂(A)的熔点以上熔融成形来获得。对于本发明中使用的树脂构件在金属材料表面上的熔融成形法,可以通过注射成形、压缩成形、复合材料、片材、管材等的挤出成形、拉拔成形、吹塑成形、传递成形等各种成形法、以熔融成形对本发明中使用的聚芳硫醚树脂组合物来进行,特别是为了脱模性也优异,优选使用预先在模具内设置金属构件而进行注射成形的所谓金属嵌入成形法。使用任意成形法时,对于各种成形条件,均可以采用通常的一般方法来成形。例如,在成形机内,在树脂温度为聚芳硫醚树脂(A)的熔点以上的温度范围、优选该熔点+10℃以上的温度范围、更优选熔点+10℃~熔点+100℃的温度范围、进一步优选熔点+20℃~熔点+50℃的温度范围内将聚芳硫醚树脂组合物熔融,经过该工序后,从树脂挤出口将树脂挤出,金属嵌入成形的情况下,注入到设置有金属构件的模具内等来成形即可。此时,模具温度也设定为公知的温度范围、例如室温(23℃)~300℃、优选40~200℃、进一步优选120~180℃即可。
作为前述复合成形体的主要用途例,也可以应用于如下用途:各种家电制品、手机、及PC(个人计算机,Personal Computer)等电子设备的壳体、箱型的电气/电子部件集成模块用保护·支撑构件·多个分立半导体或组件、传感器、LED灯、连接器、插座、电阻器、继电器箱、开关、线圈骨架、电容器、可变电容器箱、光学拾波器、共振器、各种端子板、变量器、插头、印刷基板、调谐器、扬声器、麦克风、耳机、小型电动机、磁头基座、电源组件、端子台、半导体、液晶、FDD滑架、FDD机架、电动机刷握、抛物面天线、计算机相关部件等为代表的电气/电子部件;VTR部件、电视机部件、熨斗、电吹风、电饭煲部件、微波炉部件、音响部件、音频·激光光盘·微型光盘·DVD光盘·蓝光光盘等声音/影像设备部件、照明部件、冰箱部件、空调部件、打字机部件、文字处理器部件、或者热水器、洗澡器的热水量、温度传感器等水循环设备部件等为代表的家庭、办公电子制品部件;办公计算机相关部件、电话相关部件、传真相关部件、复印机相关部件、洗涤用夹具、电动机部件、打火机、打字机等为代表的机械相关部件:显微镜、双筒望远镜、相机、钟表等为代表的光学设备、精密机械相关部件;交流发电机端线、交流发电机连接器、刷握、集电环、IC调节器、照明调光器用电位计基座、继电器块、抑制开关、排气阀等各种阀、燃料相关·排气系·吸气系各种管、进气喷嘴通气管、进气歧管、燃料泵、发动机冷却水接头、化油器主体、化油器垫片、排气传感器、冷却水传感器、油温传感器、制动磨擦片磨损传感器、节气门位置传感器、曲轴位置传感器、空气流量计、制动磨擦片磨损传感器、空调用恒温器基座、暖房热风流量控制阀、散热器电动机用刷握、水泵叶轮、涡轮叶片、雨刷电动机相关部件、配电器(distributor)、起动器开关、点火线圈及其线圈架、电动机绝缘体、电动机转子、电动机芯、起动继电器、传输用线束、挡风玻璃清洗喷嘴、空调面板开关基板、燃料相关电磁阀用线圈、保险丝用连接器、喇叭终端、电气部件绝缘板、步进电动机转子、灯插座、灯反射器、灯罩、制动器汽缸活塞、电磁线圈骨架、发动机滤油器、点火装置箱等汽车·车辆相关部件、其他各种用途。
实施例
以下举出具体的例子,更详细地对本发明进行说明。另外,份、%在没有特别说明的情况下为质量基准。
(测定例1)聚苯硫醚树脂的熔融粘度的测定
使用岛津制作所制流动试验仪CFT-500D,将参考例中制造的聚苯硫醚树脂在300℃、载荷:1.96×106Pa、L/D=10(mm)/1(mm)下保持6分钟后进行测定。
(制造例1)聚苯硫醚树脂(A-1)的制造
[工序1]
在连接有压力计、温度计、冷凝器、倾析器、精馏塔的带搅拌叶片的150升高压釜中投入对二氯苯(以下,简记为“p-DCB”。)33.222kg(226摩尔)、NMP 3.420kg(34.5摩尔)、47.23质量%NaSH水溶液27.300kg(以NaSH计为230摩尔)、及49.21质量%NaOH水溶液18.533g(以NaOH计为228摩尔),边搅拌边在氮气气氛下用5小时升温至173℃,使水27.300kg馏出后,将高压釜密闭。对于在脱水时通过共沸而馏出的p-DCB,用倾析器进行分离而随时返回到高压釜内。脱水结束后的高压釜内为微粒状的无水硫化钠组合物分散于p-DCB中的状态。该组合物中的NMP含量为0.079kg(0.8摩尔),因此表示投入的NMP的98摩尔%(33.7摩尔)水解为NMP的开环体(4-(甲基氨基)丁酸)的钠盐(以下,简记为“SMAB”。)。高压釜内的SMAB量相对于存在于高压釜中的硫原子1摩尔为0.147摩尔。对于投入的NaSH和NaOH总量,在转变为无水Na2S时的理论脱水量为27.921g,因此表示:高压釜内的残余水量878g(48.8摩尔)内,609g(33.8摩尔)在NMP与NaOH的水解反应中被消耗,不以水的形式存在于高压釜内,剩余的269g(14.9摩尔)以水或结晶水的形式残留在高压釜内。高压釜内的水分量相对于存在于高压釜中的硫原子1摩尔为0.065摩尔。
[工序2]
在上述脱水工序结束后,将内温冷却至160℃,投入NMP 46.343kg(467.5摩尔),升温至185℃。高压釜内的水分量相对于工序2中投入的NMP 1摩尔为0.025摩尔。在表压到达至0.00MPa的时刻,开放连接精馏塔的阀,用1小时将内温升温至200℃。此时,通过冷却和阀的开度进行控制以使精馏塔出口温度为110℃以下。对于馏出的p-DCB与水的混合蒸气,用冷凝器进行冷凝、用倾析器进行分离,从而p-DCB返回到高压釜中。馏出水量为228g(12.7摩尔)。
[工序3]
工序3开始时的高压釜内水分量为41g(2.3摩尔),相对于工序2中投入的NMP 1摩尔为0.005摩尔、相对于存在于高压釜中的硫原子1摩尔为0.010摩尔。高压釜内的SMAB量与工序1相同,相对于存在于高压釜中的硫原子1摩尔为0.147摩尔。接着,用3小时使内温从200℃升温至230℃,在230℃搅拌1小时后,升温至250℃,搅拌1小时。内温200℃时刻的表压为0.03MPa、最终表压为0.40MPa。冷却后,将所得浆料内650g注入到3升水中,在80℃搅拌1小时后,进行过滤。将该滤饼再次在3升的温水中搅拌1小时、清洗后,进行过滤。重复4次该操作。向该滤饼中再次加入3升的温水和乙酸,调整至pH4.0后,搅拌1小时、清洗后,进行过滤。将该滤饼再次在3升的温水中搅拌1小时、清洗后,进行过滤。重复2次该操作。使用热风干燥机在120℃干燥一晩,得到白色粉末状的PPS树脂(A-1)。该聚合物在300℃下的熔融粘度为41Pa·s。非牛顿指数为1.07。
(制造例2)聚苯硫醚树脂(A-2)的制造
除了将设为“接着,用3小时使内温从200℃升温至230℃,在230℃搅拌1小时后,升温至250℃,搅拌1小时。”的部分设为“接着,用3小时使内温从200℃升温至230℃,在230℃搅拌1.5小时后,升温至250℃,搅拌1小时。”以外,与制造例1同样地操作,得到白色粉末状的PPS树脂(以下,记为A-2)。所得聚合物的熔融粘度为73Pa·s、非牛顿指数为1.07。
(制造例3)聚苯硫醚树脂(A-3)的制造
在连接有压力计、温度计、冷凝器的带搅拌叶片及底阀的150升高压釜中投入片状硫化钠(60.3重量%Na2S)19.413kg和NMP 45.0kg。边在氮气气流下搅拌边升温至209℃,使水4.644kg馏出(残存的水分量相对于硫化钠1摩尔为1.13摩尔)。其后,将高压釜密闭,冷却至180℃,投入对二氯苯22.185kg、1,2,4-三氯苯0.027kg及NMP 18.0kg。在液温150℃下使用氮气加压至表压0.1MPa,开始升温。在液温240℃保持2小时后,在液温260℃下搅拌3小时并且进行反应,通过洒水将高压釜上部冷却。接着降温的同时停止高压釜上部的冷却。以在冷却中液温不降低的方式保持高压釜上部恒定。反应中的最高压力为0.85MPa。反应后,冷却,在温度170℃的时刻将在NMP0.663kg中包含草酸·二水合物0.284kg(2.25摩尔)的溶液加压注入。搅拌30分钟后,冷却,在100℃打开底阀,将反应浆料移送到150升平板过滤机,在120℃进行加压过滤后,加入NMP 16kg,进行加压过滤。过滤后,使用带搅拌叶片的150升真空干燥机,在减压下在150℃搅拌2小时,将NMP去除,得到白色粉末状的PPS树脂(A-3)。该聚合物在300℃下的熔融粘度为77Pa·s。非牛顿指数为1.25。
(制造例4)聚苯硫醚树脂(A-4)的制造
在连接有压力计、温度计、冷凝器的带搅拌叶片及底阀的150升高压釜中投入片(フレーク)状硫化钠(60.3重量%Na2S)19.413kg和NMP 45.0kg。边在氮气气流下搅拌边升温至209℃,使水4.644kg馏出(残存的水分量相对于硫化钠1摩尔为1.13摩尔)。其后,将高压釜密闭,冷却至180℃,投入对二氯苯23.211kg及NMP 18.0kg。在液温150℃下使用氮气加压至表压0.1MPa,开始升温。在液温260℃下搅拌3小时并且进行反应,通过洒水将高压釜上部冷却。接着降温的同时停止高压釜上部的冷却。以在冷却中液温不降低的方式保持高压釜上部恒定。反应中的最高压力为0.85MPa。
反应后,冷却,冷却后,将所得浆料内的650g注入到3升的水中,在80℃搅拌1小时后,进行过滤。将该滤饼再次在3升的温水中搅拌1小时、清洗后,进行过滤。重复7次该操作。使用热风干燥机在120℃干燥一晩。
其后,用热风干燥机在240℃进行3小时热处理,得到PPS树脂(A-4)。所得聚合物的熔融粘度为28Pa·s、非牛顿指数为1.21。
(实施例1~8及比较例1~4)热塑性树脂组合物的制造
按照表1~4中记载的组成成分及配混量(全部为质量份),用桶混机将各材料均匀混合。其后,将前述配混材料投入到株式会社日本制钢所制带排气孔的双螺杆挤出机“TEX30α”中,将树脂成分挤出量设定为25kg/hr、将螺杆转速设定为250rpm、将设定树脂温度设定为330℃来进行熔融混炼,得到树脂组合物的粒料。使用该粒料进行以下的各种评价试验。试验及评价的结果示于表1~3。
(测定例2)密合强度
实验方法将实施了下述粗糙化处理的金属试验片(长度×宽度×厚度=50mm×10mm×2mm)设置在注射成形用模具(模具温度为140℃)上,以处理面(10mm×2mm)与树脂组合物垂直接合的方式成形为金属/树脂复合结构体(依据ISO19095、依据Type-A型)。实施相对于所得结构体的接合面垂直方向的拉伸试验(拉伸速度1mm/分钟),将所得最大应力值作为密合强度。
金属处理(S):从铝板(材质:A1050)以前述大小切出金属片,进而对接合面进行研磨(研磨纸粗糙度:1000号)。对研磨后的接合面进行电子显微镜观察,结果在数均内径100nm以下的凹部未观测到表面被覆盖的样子。在该铝片的与接合面处于相反侧的端部打孔,对十几个孔使由氯乙烯涂覆的铜线通过,以使铝片彼此互相不重叠的方式对铜线进行弯曲加工,使全部同时下垂。
在槽中将市售的铝合金用脱脂剂“NE-6(Meltex Inc.制)”7.5%投入到水中后,以75℃进行加热溶解,将前述铝片浸渍5分钟,充分进行水洗。接着在另一槽中准备设为50℃的10%苛性钠水溶液,使前述铝片在其中浸渍0.5分钟,充分进行水洗。
接着在另一槽中准备设为90℃的60%硝酸溶液,浸渍15秒,充分进行水洗。接着在另一槽中准备设为20℃的5%硫酸水溶液,将直流电源装置“ASR3SD-150-500(中央制作所制)”的阳极接线于前述铝片的孔部,将阴极接线于放入至槽中的铅板,以成为5A/dm2的电流密度的恒定电流控制进行阳极氧化。进行40分钟阳极氧化并进行水洗,在设为60℃的温风干燥机中放入1小时而干燥。1天后,用扫描型电子显微镜对其中1个接合面进行拍摄(倍率50万倍),从各图像中随机分别选择50个凹部后进行测定。在表面周期性地连续形成凹部,凸部间距以数均计为50nm、数均孔径为30μm、凹部的密度是平均100nm2为10个。
处理后迅速成形,测定密合强度(S1)。进而,在恒温高湿(80℃、湿度95%)环境下下放置200小时后测定密合强度(S2)。以n=3次进行评价,采用其平均值。
金属处理(T):对金属试验片使用YAG激光标记装置(SHIBAURA ELETECCORPORATION制“LAY-791DE”)实施激光槽加工。在金属片的端面以100μm间隔形成长度10mm、深度150μm、宽度100μm的连续的槽。
处理后迅速成形,测定密合强度(T1)。进而在恒温高湿(80℃、湿度95%)环境下放置200小时后测定密合强度(T2)。以n=3次进行评价,采用其平均值。
[表1]
[表2]
[表3]
[表4]
需要说明的是,表1~4中的配混树脂、材料的配混比率表示质量份,使用下述物质。
B-1:苯酚酚醛清漆DIC株式会社制“TD-2090”(羟基当量105g/当量、软化点117-123℃)
B-2:苯酚酚醛清漆DIC株式会社制“TD-2093”(羟基当量104g/当量、软化点98-102℃)
B-3:苯酚酚醛清漆DIC株式会社制“TD-2131”(羟基当量104g/当量、软化点78-82℃)
B-4:甲酚酚醛清漆DIC株式会社制“KA-1165”(羟基当量119g/当量、软化点117-130℃)
b-5:乙烯(88质量%)-二甲基丙烯酸缩水甘油酯(12质量%)的共聚物住友化学工业株式会社制“BONDFAST 7L”
※需要说明的是,对于酚醛树脂的软化点测定,使用MEIHO CO.,LTD.制环球式软化点测定装置ASP-M4SP,采用以3℃/分钟升温测定的值。另外,对于酚醛树脂的羟基当量的测定,采用依据JIS K 0070(1992)中规定的中和滴定法的方法测定的值。
C-1:玻璃纤维(短切纤维、E玻璃、平均纤维长度200μm、平均直径10μm、基于环氧系集束剂的表面处理品)
附图标记说明
x···从凸部的顶上部到邻接的凸部的顶上部为止的2点间的、金属构件表面的与微细凹凸面平行的方向的部分的长度
y···从凸部的顶上部到邻接的凹部的底面部为止的2点间的、金属构件表面的与微细凹凸面垂直的方向的部分的长度。
Claims (10)
1.一种金属/树脂复合结构体,其特征在于,其是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
所述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
所述聚芳硫醚树脂组合物是将下述树脂组合物成形而成的,所述树脂组合物以相对于聚芳硫醚树脂(A)100质量份、酚醛树脂(B)为0.05~20质量份的范围包含所述聚芳硫醚树脂(A)和所述酚醛树脂(B)。
2.根据权利要求1所述的金属/树脂复合结构体,其中,所述酚醛树脂(B)为酚醛清漆型酚醛树脂。
3.根据权利要求1或2所述的金属/树脂复合结构体,其中,所述酚醛树脂(B)具有80~200g/当量的范围的羟基当量。
4.根据权利要求1~3中任一项所述的金属/树脂复合结构体,其中,所述酚醛树脂(B)具有50~180℃的范围的软化点。
5.根据权利要求1~4中任一项所述的金属/树脂复合结构体,其中,所述树脂组合物为熔融混炼物。
6.根据权利要求1~5中任一项所述的金属/树脂复合结构体,其中,所述树脂构件是将聚芳硫醚树脂组合物熔融成形而得到的。
7.一种金属/树脂复合结构体的制造方法,其特征在于,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
所述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
所述制造方法中,对于金属构件,将包含聚芳硫醚树脂(A)和酚醛树脂(B)的聚芳硫醚树脂组合物在所述聚芳硫醚树脂(A)的熔点以上熔融成形。
8.根据权利要求7所述的金属/树脂复合结构体的制造方法,其中,相对于所述聚芳硫醚树脂(A)100质量份,所述聚芳硫醚树脂组合物以0.05~20质量份的范围包含所述酚醛树脂(B)。
9.一种聚芳硫醚树脂组合物,其特征在于,其用于金属/树脂复合结构体,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
所述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
所述聚芳硫醚树脂组合物是将聚芳硫醚树脂(A)和酚醛树脂(B)作为必需成分配混而成的,相对于所述聚芳硫醚树脂(A)100质量份以0.05~20质量份的范围包含所述酚醛树脂(B)。
10.一种树脂构件,其特征在于,其用于金属/树脂复合结构体,所述金属/树脂复合结构体是经表面粗糙化的金属构件与由聚芳硫醚树脂组合物构成的树脂构件接合而成的,
所述金属构件为铝、铜、镁、铁、钛或含有它们的合金,
所述聚芳硫醚树脂组合物是将聚芳硫醚树脂(A)和酚醛树脂(B)作为必需成分配混而成的,相对于所述聚芳硫醚树脂(A)100质量份,所述酚醛树脂(B)为0.05~20质量份的范围,
所述树脂构件是将聚芳硫醚树脂组合物熔融成形而得到的。
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US11911974B2 (en) | 2024-02-27 |
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WO2018139034A1 (ja) | 2018-08-02 |
US20190389146A1 (en) | 2019-12-26 |
JPWO2018139034A1 (ja) | 2019-11-07 |
EP3575077A1 (en) | 2019-12-04 |
KR20190111922A (ko) | 2019-10-02 |
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EP3575077A4 (en) | 2020-07-22 |
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