CN115667581A - 热塑性树脂组合物的镀敷成型体 - Google Patents
热塑性树脂组合物的镀敷成型体 Download PDFInfo
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- CN115667581A CN115667581A CN202180035408.0A CN202180035408A CN115667581A CN 115667581 A CN115667581 A CN 115667581A CN 202180035408 A CN202180035408 A CN 202180035408A CN 115667581 A CN115667581 A CN 115667581A
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Abstract
本发明提供一种对于1MHz以下的低频段电磁波具有优异的屏蔽性(遮蔽性)的成型体。根据本发明,提供一种镀敷成型体,其具有热塑性树脂组合物的树脂层、以及导电性金属的被覆层,该热塑性树脂组合物含有含Fe‑Si‑Al合金的软磁性粉末。
Description
技术领域
本发明涉及一种热塑性树脂组合物的镀敷成型体,该热塑性树脂组合物中调配有具有低频段电磁波屏蔽性能的软磁性粉末,该软磁性粉末屏蔽或吸收各种电子设备的装置内部,尤其是电动汽车上搭载的电力转换装置、数据处理装置等所产生的频率为1MHz以下的电磁波(以下,通常将其称为低频段电磁波),以抑制电磁波噪声。
背景技术
各种电子设备所产生的不必要电磁波会影响其他电子设备,成为导致误动作的原因。为了抑制这种不必要电磁波的有害影响,使用电磁波屏蔽材料。
作为这样的电磁波屏蔽材料,提出了软磁性材料。作为这样的软磁性材料,众所周知,坡莫合金类对频率为数百MHz~数GHz的电磁波展现优异的屏蔽性。
作为软磁性材料,还有1937年发现的Fe-Si-Al系合金的软磁性体。此外,Fe-Si系合金、Fe-Si-Cr系合金也是公知的软磁性体。已知有评价这些软磁性体对于频率300MHz~3GHz的电磁波的屏蔽性的示例。
另一方面,对于频率为1MHz以下的低频段电磁波的屏蔽材的研究例非常少,例如专利文献1中提出使用将软磁性粉末分散在有机溶剂中而得的磁屏蔽涂料,在两层以上的碳纤维强化树脂层之间形成磁性层的层叠体,专利文献2中提出通过在网状结构体涂布软磁性涂料并进行干燥,而使软磁性粉含浸并固定而得的磁场屏蔽片。
此外,也有人提出在树脂成型品的表面设置有镀敷层的成型品。专利文献3中记载有使用了维持镀敷性,同时各种机械特性及阻燃性优异的树脂组合物的成型物,专利文献4中记载有以在由热塑性弹性体组合物构成的成型体设置镀敷层为特征的镀敷成型体。
[现有技术文件]
[专利文献]
[专利文献1]日本特开2017-126644
[专利文献2]日本特开2018-85391
[专利文献3]国际公开WO2014/115475
[专利文献4]日本特开平11-29663
发明内容
发明要解决的问题
但是,至今为止,为了有效地屏蔽1MHz以下的低频段电磁波,通过将现有的软磁性材料厚板化、层叠化,或围成壳体状来采取应对。但是,这样的方法存在屏蔽部变得过重的课题。为了实现各种电子设备的轻薄短小化、电动汽车的轻量化,期望有效屏蔽低频段电磁波,且薄壁化、复杂部件形状的成型体。
即,本发明的目的在于提供一种对于1MHz以下的低频段电磁波具有优异的屏蔽性(遮蔽性)的成型体。
用于解决问题的方案
根据本发明,可提供一种镀敷成型体,其具有热塑性树脂组合物的树脂层、以及导电性金属的被覆层,该热塑性树脂组合物含有含Fe-Si-Al合金的软磁性粉末。
将本发明的软磁性粉末调配于热塑性树脂中而得的具有低频段电磁波屏蔽性能的树脂组合物,可通过使用公知的密闭混合机、挤出机等设定热塑性树脂加热熔融的适当温度范围并进行熔融混练而获得,通过使用适当的铸模、模具,可将该熔融混练物成型为片材、软管、其他形状而获得成型体。此外,利用公知的镀敷法,可获得在该成型体表面形成有镀敷层的镀敷成型体。
以下,例示本发明的各种实施方式。以下所示的实施方式可相互组合。
优选地,在镀敷成型体中,导电性金属为铜。
优选地,在镀敷成型体中,厚度1.0mm的镀敷成型体片材利用KEC法测得的于频率0.3MHz的磁场分量的衰减率为10dB以上,于1MHz的磁场分量的衰减率为15dB以上。
此外,通过将上述热塑性树脂组合物进行加热熔融成型加工,而提供成型体。
通过对该成型体实施镀敷处理,而提供在表面形成有被覆层(镀敷层)的镀敷成型体。
发明的效果
根据本发明,可提供一种对于低频段电磁波具有优异的电磁波屏蔽性的热塑性树脂组合物的镀敷成型体。
附图说明
图1是使用壳体模具成型而得的壳体成型体的概略剖视图。
图2是使用壳体模具成型而得的壳体成型体的概略俯视图。
具体实施方式
以下,针对用以实施本发明的方式进行详细地说明。此外,以下说明的实施方式是展示本发明的代表性实施方式的示例,本发明的范围不应由此狭义地解释。
本发明的镀敷成型体具有热塑性树脂组合物的树脂层、以及导电性金属的被覆层,该热塑性树脂组合物含有含Fe-Si-Al合金粉末作为主成分的软磁性粉末。被覆层是直接或经由其他层形成于树脂层上的导电性金属层。在一个示例中,是于将含有软磁性粉末的热塑性树脂组合物进行加热熔融成型而得的成型体(树脂层)实施导电性金属的镀敷(被覆层)。此外,成型体的示例有片材、壳体、软管等。
在本发明中,片材成型后,切取形成被覆层而获得的两面镀敷片材、或于图1、图2所示的壳体成型体进行两面镀敷而获得的镀敷壳体的方形片材部分(以下,将其称为镀敷片材),得到的厚度1.0mm的镀敷片材可用于KEC测定。
本发明的镀敷成型体,就于频率0.3MHz与1MHz的磁场分量的衰减率(使用作为镀敷成型体的厚度1.0mm的片材,对于频率0.3MHz及1MHz的电磁波,利用KEC法测得的电磁波的磁场分量的衰减率),优选于0.3MHz为10dB以上,于1MHz为15dB以上。本发明的镀敷成型体对于1MHz以下的低频段电磁波具有优异的屏蔽性。
作为镀敷成型体的厚度1.0mm的片材利用KEC法测得的于频率0.3MHz的磁场分量的衰减率优选为10dB以上,更优选为15dB以上,进一步优选为20dB以上。
作为镀敷成型体的厚度1.0mm的片材利用KEC法测得的于频率1MHz的磁场分量的衰减率优选为15dB以上,更优选为20dB以上,进一步优选为25dB以上。
此外,镀敷成型体优选除了对于1MHz以下的电磁波的屏蔽性外,还具有对于3MHz、10MHz的电磁波的屏蔽性。作为镀敷成型体的厚度1.0mm的片材利用KEC法测得的于频率3MHz的磁场分量的衰减率优选为20dB以上。作为镀敷成型体的厚度1.0mm的片材利用KEC法测得的于频率10MHz磁场分量的衰减率优选为30dB以上。
软磁性粉末是含有具有软磁性的Fe-Si-Al合金的粉末。
软磁性粉末优选以Fe-Si-Al合金粉末为主成分。在不损及本发明的效果的范围内,软磁性粉末可含有Fe-Si系合金粉末、Fe-Si-Cr系合金粉末、其他软磁性粉末。以Fe-Si-Al合金粉末为主成分时,优选软磁性粉末的50质量%以上为Fe-Si-Al合金粉末,更优选为软磁性粉末实质上仅由Fe-Si-Al合金粉末构成,特别优选软磁性粉末为Fe-Si-Al合金粉末。
Fe-Si-Al合金为含有Fe、Si、以及Al的合金。Fe-Si-Al合金的组成优选为Si:3~12原子%、Al:4~12原子%、余量由Fe构成。Fe-Si-Al合金的代表性组成的一个例子为Fe85Si10Al5、Fe84.7Si9.5Al5.8等。Fe-Si-Al合金中Si的组成具体而言例如为3、4、5、6、7、8、9、10、11、12原子%,也可为此处所例示的数值中任意两者之间的范围内。此外,Fe-Si-Al合金中Al的组成具体而言例如为4、5、6、7、8、9、10、11、12原子%,也可为此处所例示的数值中任意两者之间的范围内。此外,本说明书中,波浪线符号“~”是用于表示包含其前后记载数值的数值范围的符号。具体而言“X~Y”的记载(X、Y均为数值)表示“X以上且Y以下”。
软磁性粉末的形状可为球状、扁平状、无定形中的任一种,会展现类似的屏蔽效果。该软磁性粉末的最大径为500μm,优选为100μm,可利用公知的筛分操作获得。此外,粉末的最大径,在无定形、扁平粉的情况下,是指各粒子的最大径。粉末的最大径变大而超过500μm的话,会有电磁波屏蔽性在成型物内变得不均匀,或成为缺陷部位的疑虑,而不优选。
热塑性树脂组合物优选含有20体积%~80体积%的软磁性粉末,更优选含有30体积%~70体积%。软磁性粉末的含量低于20体积%的话,无法展现足够令人满意的电磁波屏蔽性,超过80体积%的话,会有混练时或成型时的流动性不足,无法成型为预定形状的情况,并且混练物变脆,而不优选。热塑性树脂组合物中软磁性粉末的含量,具体而言例如为20、25、30、35、40、45、50、55、60、65、70、75、80体积%,也可为此处所例示的数值中任意两者之间的范围内。
热塑性树脂组合物中含有的热塑性树脂只要是能进行无电解镀敷的树脂,则没有特别限定,为选自由聚乙烯(PE)、聚丙烯(PP)、聚苯乙烯(PS)、ABS树脂、聚氯乙烯(PVC)、聚偏二氯乙烯(PVDC)、乙烯-乙酸乙烯酯树脂(EVA)、聚氨酯(PU)、丙烯酸树脂(PMMA)、聚碳酸酯(PC)、聚酰胺(PA)、聚酰亚胺(PI)、聚苯硫醚(PPS)、聚偏二氟乙烯(PVDF)、聚四氟乙烯(PTFE)、聚对苯二甲酸丁二醇酯(PBT)、尼龙、聚苯醚(PPE)、液晶聚合物(LCP)、以及它们的改性物等构成的群组中的至少一种。此外,也可为多种树脂的聚合物合金。考量软磁性粉末容易分散,容易获得均匀的电磁波屏蔽性的观点,有时优选为ABS树脂、聚氯乙烯、丙烯酸树脂、乙烯-乙酸乙烯酯树脂等。
此外,在不明显损及本发明的低频段电磁波屏蔽性的范围内,可添加前述以外的成型加工助剂、各种调配剂。添加加工助剂时,相对于热塑性树脂与软磁性粉末的总量,优选含有0.1质量%~1质量%的加工助剂,更优选含有0.3~0.5质量%。加工助剂可列举聚乙二醇脂肪酸酯等。
混练方法可采用公知的密闭混合机、挤出机等熔融混练机。关于混练温度与混练时间,就每种热塑性树脂选择能够进行混练、成型的公知的适当条件。为了提高软磁性粉末的分散性,在热塑性树脂的劣化、软磁性粉末的破碎不明显发生的范围内,优选为高速旋转、高剪切条件。此外,软磁性粉末的混练顺序可以是与热塑性树脂同时一并添加,也可为在热塑性树脂加热熔融后或加热熔融途中添加软磁性粉末(后添加)的方法,考量提高分散性与抑制树脂劣化的观点来适当选择。
获得的调配有软磁性粉末的热塑性树脂组合物(成型原料),通过使用热压机、熔融挤出机等,并使用适当的铸模、模具等,来成型为期望的形状。形状例如有片材、软管、壳体状等,可通过选择模具来成型为各种形状。此外,可制作使用多个挤出成型机而得的层叠片材、使用粘接剂等而得的多层化层合片材等。
成型品可为用于屏蔽各种设备的低频段电磁波的成型部件,作为一个示例,可如上述加工成片材。此外,通过片材由多个层构成,即使厚度相同,也会有增大屏蔽效果的情况。本发明的一个实施方式中,当片材为多层时,也可期待高屏蔽效果。另一方面,在本发明中,即使是由单层构成片材等的实施方式,也可获得充分的屏蔽效果。
然后,对于由前述热塑性树脂组合物构成的成型体的镀敷方法没有特别限制,优选为无电解镀敷法。考量成本、稳定性、导电性的观点,镀敷层的金属成分优选为铜。铜镀敷层的厚度为0.05~20μm,优选为0.1~10μm,更优选为0.1~5μm。无电解镀敷法中,是将合金粉末进行清洗并使表面活性化,添加至含有络合剂与还原剂的水溶液中,并向其中滴加铜盐来实施。
作为络合剂,例如有氨水、乙二胺四乙酸(EDTA)、二亚乙基三胺五乙酸(DTPA)、三亚乙基四胺六乙酸(TTHA)、羟基乙基乙二胺三乙酸(HEDTA)、氨三乙酸(NTA)、亚氨基二乙酸(IDA)等氨基羧酸盐、乙二胺、四亚甲基二胺、六亚甲基二胺、二亚乙基三胺、四亚乙基五胺、五亚乙基六胺等多元胺类、单乙醇胺、二乙醇胺、三乙醇胺等氨基醇类、柠檬酸、酒石酸、乳酸、苹果酸等羟基羧酸盐、硫代乙醇酸、甘氨酸等。
还原剂有氢化硼化合物、胺硼烷类、次磷酸类、亚磷酸类、醛类、抗坏血酸类、肼类、多元酚类、多元萘酚类、苯酚磺酸类、萘酚磺酸类等。
可溶性铜盐有硫酸铜、氧化铜、氯化铜、焦磷酸铜、碳酸铜、或乙酸铜、草酸铜及柠檬酸铜等羧酸铜盐、或甲磺酸铜及羟基乙磺酸铜等有机磺酸铜盐等。
在本发明中,于作为基底的热塑性树脂组合物的成型体表面层形成前述镀敷层,考量整个成型体展现稳定的电磁波屏蔽性的观点,优选均匀地形成镀敷层。此外,如果需要也可在该镀敷层上层叠无电解镀敷层或电解镀敷层。
作为评价电磁波噪声屏蔽性(遮断性)的方法,已知有一般财团法人关西电子工业振兴中心(KEC)所开发的KEC法,例如在纤维制品消费科学(纤消杂志)vol.40、No.2(1999)、“https://www.kec.jp/testing-division/kec-method/”中有介绍。该KEC法是将近场产生的电磁波的屏蔽效果分为电场分量与磁场分量来进行测定的方法,从发射天线(发射用治具)发射的电磁波通过片材状测定试样而由接收天线(接收用治具)接收,测定衰减后的电磁波并以衰减率(测定单位:dB)的形式定量化。在本发明中,于室温条件下使用一定厚度的试样(两面镀敷后的厚度1.0mm),在频率0.1MHz~1000MHz的范围内测定磁场分量的衰减率。此外,本发明中重要的1MHz以下频率的电磁波屏蔽性(磁场分量),是通过比较0.3MHz与1MHz的衰减率测定值来判断优劣。
[实施例]
以下,列举本发明的实施例及比较例来说明本发明的效果。
[实施例1~3]
按照表1所示的组成,制作调配有Fe-Si-Al合金粉末的树脂组合物。合金粉末使用平均粒径50μm的Fe-Si-Al合金粉末(山阳特殊制钢制、FME3D-AH、比重6.9、Si为9.6原子%、Al为5.9原子%、余量为Fe)。热塑性树脂使用ABS树脂(Denka(股)公司制ABS树脂ME、比重1.04)。混练装置使用东洋精机制Laboplastomill(内容积60mL),以成为表1的进料组成的方式,首先仅将ABS树脂在210℃×3分钟、转速20rpm的条件下进行预混练,然后添加本发明的合金粉末,在转速50rpm、210℃×10分钟的条件下进行混练,得到含合金粉末的树脂组合物(以下,简称为组合物)。使用设定为210℃的热压机与厚度1mm的片材模具将该组合物进行熔融成型,制作厚度为1.0mm、纵横尺寸为120mm×120mm的正方形成型片材。
对厚度1.0mm的成型片材的铜镀敷按照以下的步骤实施。将以前述步骤制作的成型片材于50℃在5摩尔/L的氢氧化钾水溶液中浸渍5分钟,以纯水充分清洗。另外,用于铜的无电解镀敷的铜氨络合物溶液按照以下的步骤制作。称量浓度0.2摩尔/L的硫酸铜五水合物,将其暂时溶解于300ml的纯水中,然后加入25%氨水400ml,利用纯水定容至1L,由此调制含有10%氨水与0.2摩尔/L硫酸铜的铜氨络合物溶液。重复该操作3次,制作共计3L的铜氨络合物溶液。使前述厚度的正方形片材在该铜氨络合物溶液中浸渍5分钟而使铜离子吸附后,利用纯水清洗。然后,在25℃的0.05摩尔/L的硼氢化钠水溶液中浸渍5分钟,还原吸附于由含合金粉末的树脂组合物构成的成型片材表面的铜离子,在片材两面析出金属铜皮膜。之后,将形成有铜皮膜的成型片材在氮气气氛、110℃的条件下加热处理2小时,最终获得本发明的镀敷成型体。经成型片材的剖面SEM观察,铜镀敷厚度分别为0.40μm。
[实施例4~6]
是将实施例1~3中厚度1.0mm的正方形片材于铜氨络合物溶液中的浸渍时间变更为10分钟的情形。铜镀敷厚度均为0.57μm。
[比较例1~3]
是使用前述实施例1~3中铜镀敷前的厚度1.0mm、纵横120mm×120mm的正方形成型片材的情形。
前述实施例、比较例的成型片材的电磁波屏蔽性(磁场分量)由“一般社团法人KEC关西电子产业振兴中心(京都市相乐郡精华町)”进行测定。是于同处将前述成型片材夹在“纤维制品消费科学(纤消杂志)vol.40、No.2(1999)”所示的一对磁场屏蔽效果评价用单元(图6)之间,并利用图7所示的装置获得的测定值。此外,测定时的施加频率在0.1MHz~1000MHz的范围内连续变化,尤其采用由在0.3MHz及1MHz的发射/接收强度值算出的衰减率(相对值)作为本发明中的磁场屏蔽效果的代表值。其结果示于表1与表2。本发明的含软磁性粉的树脂组合物的铜镀敷成型体,频率0.3MHz的衰减率展现为10dB以上,1MHz的衰减率展现为15dB以上,可知具有优异的电磁波(磁场分量)屏蔽性。此外,表1与表2中也表示3MHz与10MHz的衰减率。本发明的镀敷成型体在超过1MHz的频段中衰减率也提高,具有优异的屏蔽性。与未进行铜镀敷的成型体(比较例1~3)相比可知,通过进行铜镀敷,电磁波屏蔽性(磁场分量)于0.3MHz提高3dB以上,于1MHz提高10dB以上。
[表1]
[表2]
[实施例7、比较例4]
使用桶径30mm、L/D=16的附有混练功能的单轴挤出机,于前端部安装狭缝1mm、宽度200mm的T型模,在桶设定温度170~210℃、转速35rpm的条件下,投入预定量的ABS树脂(Denka(股)公司制ME)、加工助剂(聚乙二醇脂肪酸酯(花王公司制、EMANON 1112))、以及同种作为软磁性粉末的平均粒径53μm的Fe-Si-Al合金粉末(山阳特殊制钢制),得到混练有软磁性粉末的树脂组合物的片材状成型物。此外,添加加工助剂,以使其在每单位合计重量的EVA树脂与Fe-Si-Al合金粉末中成为0.3重量%。然后,将该片材状成型物裁切成120mm×120mm,使用预先准备的加温至210℃的热压机与屏蔽壳体成型用模具,将前述裁切的片材状成型物插入模具上表面与下表面之间,静置3分钟后,使下表面缓慢上升以加压,最终在20MPa的条件下保持10分钟并进行成型。然后,取出该屏蔽壳体模具,移至另外准备的水冷方式的冷压机中,静置10分钟并冷却。冷却结束后,从模具取出屏蔽壳体成型体(图1、图2)。图1中,厚度t1为1mm。此外,该壳体成型体的高度如图1所示为10mm。
使用该成型体,以与实施例4~6相同的条件在成型体整个表面进行铜镀敷,得到本发明的镀敷成型体。切取该镀敷成型体的平面部分(100mm×100mm),供至以与实施例1相同的方法进行的电磁波屏蔽性测定。磁场分量的测定结果示于表1的实施例7。前述中,从实施铜镀敷之前的屏蔽壳体成型体切出平面部分(100mm×100mm),并测定电磁波屏蔽性而得的结果(磁场分量)示于表2的比较例4。本发明的镀敷成型体,频率0.3MHz的衰减率展现为10dB以上,1MHz的衰减率展现为15dB以上,表明对于低频段的电磁波具有优异的屏蔽性。
[比较例5~9]
比较例5是未调配本发明的Fe-Si-Al合金粉末,也未实施铜镀敷的情形。衰减率为0.1~0.2dB左右,几乎不显示电磁波屏蔽性。比较例6~7是对未调配本发明的Fe-Si-Al合金粉末的热塑性树脂片材实施铜镀敷的情形。虽然通过铜镀敷,电磁波屏蔽性提高了2~3dB左右,但未观察到屏蔽性的显著提高。比较例8是Fe-Si-Al合金粉末的调配量为10体积%,但未进行铜镀敷的情形。于0.3MHz与1MHz的衰减率为5dB左右。比较例9是调配了90体积%的Fe-Si-Al合金粉末的情形。成型物非常脆,无法保持片材状态,未能进行KEC法测定。由一系列结果可知,本发明的调配有Fe-Si-Al合金粉末的热塑性组合物的镀敷成型体,在1MHz以下的低频段具有优异的电磁波屏蔽性。
产业上的可利用性
在调配有软磁性粉末的热塑性树脂组合物的成型体镀敷导电性金属而得的本发明的镀敷成型体,对于频率为1MHz以下的低频段电磁波噪声具有优异的屏蔽性能,在工业上极为有用。
附图标记说明
P:平面部
Claims (4)
1.一种镀敷成型体,具有热塑性树脂组合物的树脂层、以及导电性金属的被覆层,所述热塑性树脂组合物含有含Fe-Si-Al合金的软磁性粉末。
2.根据权利要求1所述的镀敷成型体,其中,导电性金属为铜。
3.根据权利要求1或2所述的镀敷成型体,其中,厚度1.0mm的镀敷成型体片材利用KEC法测得的于频率0.3MHz的磁场分量的衰减率为10dB以上,于1MHz的磁场分量的衰减率为15dB以上。
4.根据权利要求1至3中任一项所述的镀敷成型体,其中,所述树脂层是将所述热塑性树脂组合物进行加热熔融成型加工而得的成型体。
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