CN103298601A - 制备用于碳纤维复合材料的接合构件的方法 - Google Patents

制备用于碳纤维复合材料的接合构件的方法 Download PDF

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CN103298601A
CN103298601A CN2011800569657A CN201180056965A CN103298601A CN 103298601 A CN103298601 A CN 103298601A CN 2011800569657 A CN2011800569657 A CN 2011800569657A CN 201180056965 A CN201180056965 A CN 201180056965A CN 103298601 A CN103298601 A CN 103298601A
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metal
carbon fibre
fibre composite
thermoplastic resin
engagement member
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竹内正基
金子徹
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Teijin Ltd
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Teijin Ltd
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
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    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • 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
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    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/44—Joining a heated non plastics element to a plastics element
    • B29C65/46—Joining a heated non plastics element to a plastics element heated by induction
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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
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
    • B29C66/7428—Transition metals or their alloys
    • B29C66/74283—Iron or alloys of iron, e.g. steel
    • 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
    • B29C66/80—General aspects of machine operations or constructions and parts thereof
    • B29C66/83—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools
    • B29C66/832—Reciprocating joining or pressing tools
    • B29C66/8322—Joining or pressing tools reciprocating along one axis
    • 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
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/919—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges
    • 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
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/94—Measuring or controlling the joining process by measuring or controlling the time
    • B29C66/949—Measuring or controlling the joining process by measuring or controlling the time characterised by specific time values or ranges
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20—Use of solutions containing silanes

Abstract

一种用于制备在含有热塑性树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法，其中：在金属的表面上形成含有三嗪硫醇衍生物的层；在含有三嗪硫醇衍生物的层与碳纤维复合材料之间设置热塑性树脂层；以及熔化热塑性树脂层，从而将金属接合到碳纤维复合材料。

Description

制备用于碳纤维复合材料的接合构件的方法
技术领域
本发明涉及制备在碳纤维复合材料与金属之间的接合构件的方法。
背景技术
碳纤维复合材料具有高比强度和高比刚度，并评价为极其出色的材料。然而，在将使用热固性树脂作为基质的常规碳纤维复合材料接合到不同种类特别是金属的构件中，它们使用螺栓/螺母、铆钉等机械接合件或胶粘剂接合。由螺栓/螺母等进行的机械接合一般涉及重量的增加。具体来说，在复合材料中，存在应力集中于接合点，并且在最坏情况下从第一应力集中点开始连续发生断裂的顾虑。在使用胶粘剂的接合中，一般必须确保具有一定厚度的胶粘剂层以便确保强度。具体来说，在接合大尺寸构件的情况下，需要相当大量的胶粘剂。结果，存在所获得构件的重量极大增加的顾虑，并且此外，还存在仅利用胶粘剂其强度不总是足够的缺点。此外，由于在胶粘剂形成总体实用强度之前需要许多时间，因此必须考虑到老化步骤。另一方面，在使用热塑性树脂作为基质的碳纤维复合材料（在后文中有时称为“热塑性碳纤维复合材料”）中，材料通过在树脂相容的范围内进行焊接而彼此接合，并且能够预期获得与基质树脂相当的接合强度。然而，在许多情况下，即使在热塑性碳纤维复合材料中也难以通过焊接与金属接合。
为了将热塑性碳纤维复合材料焊接到金属，要求用作基质的热塑性树脂本身能够焊接到金属。专利文献1描述了金属与树脂能够通过焊接接合的原因是由于通过将树脂注射成型到具有细小多孔表面的铝材所产生的锚固效应。专利文献2和3描述了通过对金属表面实施处理而接合树脂和金属。
此外，专利文献4描述了通过设置与热固性碳纤维复合材料和金属两者具有亲和性的中间树脂层的接合方法。
专利文献1：JP-A-2003-103563
专利文献2：JP-B-5-51671
专利文献3：WO2009/157445小册子
专利文献4：JP-A-2006-297927
发明内容
本发明待解决的问题
本发明的目的是提供一种制备在含有树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法，特别是提供一种制备在含有热塑性树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法，其特征在于，能够同时进行接合和成型。
热塑性碳纤维复合材料的优点在于其形状容易通过加热而改变，并且由于这一点，与热固性碳纤维复合材料相比，能够在极短时段内进行注射或压制成型。因此，如果使用含有热塑性树脂作为基质的碳纤维复合材料并且与成型同时或紧接成型之后，通过在模具中的热压接接合能够极为容易地进行接合，能够极为高效地获得带有金属材料的接合体。然而，尽管试图通过在专利文献2和3中所描述的热塑性树脂与金属的接合方法将热塑性碳纤维复合材料接合到金属，但热塑性碳纤维复合材料，其是热塑性树脂处于“浸入”在碳纤维束中的状态下。因此，树脂不总是均匀存在于材料的表面上，并且在某些情况下，存在“缺陷的”树脂部分。因此，存在无法形成足够接合强度并且接合强度显示出极大变化性的顾虑。此外，碳纤维引起对金属的所谓电解腐蚀。因此，当碳纤维已经与在树脂已经缺陷的部分中的金属进行接触时，接触部位已经引起金属的腐蚀。
解决问题的方案
作为对在热塑性碳纤维复合材料与金属之间的接合进行深入调查的结果，本发明人发现，通过在金属的表面上形成含有三嗪硫醇衍生物的层，在所述含有三嗪硫醇衍生物的层与热塑性碳纤维复合材料之间设置热塑性树脂层，并且熔化所述热塑性树脂层，从而将金属接合到所述碳纤维复合材料，能够将金属与热塑性碳纤维复合材料强力稳定地接合，并且完成本发明。本发明的构成如下所述。
1.一种用于制备在含有热塑性树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法，该方法包括：在所述金属的表面上形成含有三嗪硫醇衍生物的层；在含有所述三嗪硫醇衍生物的层与所述碳纤维复合材料之间设置热塑性树脂层；以及熔化所述热塑性树脂层以将所述金属接合到所述碳纤维复合材料。
2.根据上面第1项中所述的用于制备接合构件的方法，其中，利用电磁感应的方法加热所述金属以进行所述接合。
3.根据上面第1至2任一项中所述的用于制备接合构件的方法，其中，所述热塑性树脂层具有5μm至5mm的厚度。
4.根据上面第1至3任一项中所述的用于制备接合构件的方法，其中，构成所述金属的元素主要包含铁或铝。
5.根据上面第1至4任一项中所述的用于制备接合构件的方法，其中，在所述碳纤维复合材料中存在的所述热塑性树脂的量是每100重量份碳纤维50至1,000重量份。
6.一种接合构件，该接合构件包括以5MPa或以上的接合强度接合的热塑性碳纤维复合材料和金属，所述接合构件通过上面第1至5任一项中所述的制备方法而获得。
7.一种用于制备金属复合材料成型体的方法，所述成型体包括接合的含有热塑性树脂作为基质的碳纤维复合材料和金属，该方法包括：在所述金属的表面上形成含有三嗪硫醇衍生物的层；并且熔化设置在所述含有三嗪硫醇衍生物的层与所述碳纤维复合材料之间的热塑性层，以同时或连续地进行所述金属与所述碳纤维复合材料之间的接合以及其成型。
本发明的优点
根据本发明，能够通过简化方法将热塑性碳纤维复合材料和金属强力且稳定地接合。此外，经由热塑性树脂将热塑性碳纤维复合材料接合到金属，能够同时防止由碳纤维引起的电解腐蚀。此外，通过同时或连续地进行接合和成型步骤，能够在短时段内和较少数量的步骤中获得碳纤维复合材料与金属之间的接合构件。
附图简述
图1是示出了本发明的接合构件的一个实施例的示意图。
图2是示出了在实施例5中获得的成型体的形状的示意图。
图3是示出了在实施例5中获得的金属复合材料成型体的形状的示意图。在所述图中，圆形SPCC片由斜线示出。
参考标记列表
1热塑性碳纤维复合材料
2热塑性树脂层
3含有三嗪硫醇衍生物的层
4金属
具体实施方式
本发明涉及用于制备在含有热塑性树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法。在图1中示出了本发明的接合构件的一个实施例，并且本发明的实施例在下面描述。
[热塑性碳纤维复合材料]
在本发明中使用的热塑性碳纤维复合材料是含有作为基质的热塑性树脂和碳纤维的材料。热塑性碳纤维复合材料优选以每100重量份碳纤维50至1,000重量份的量含有热塑性树脂。更优选地，热塑性树脂的量为每100重量份碳纤维50至400重量份。还更优选地，热塑性树脂的量为每100重量份碳纤维50至100重量份。当热塑性树脂的量低于每100重量份碳纤维50重量份时，复合材料中的干碳纤维可能增加。另一方面，当该量超过1,000重量份时，碳纤维的量太少，并且碳纤维可能变得不适合作为结构材料。
热塑性树脂的实例包括：聚酰胺、聚碳酸酯、聚氧化甲烯、聚苯硫醚、聚苯醚、改性的聚苯醚、聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、聚萘二甲酸乙二酯、聚乙烯、聚丙烯、聚苯乙烯、聚甲基丙烯酸甲酯、AS树脂以及ABS树脂。具体地，从成本和性能的平衡的角度，优选为选自聚酰胺、聚丙烯、聚碳酸酯和聚苯硫醚中的至少一种。作为聚酰胺（有时简称为PA，有时称为尼龙），优选为选自下列组中的至少一种：PA6（称为聚己酰胺或聚己内酰胺，更准确来说称为聚ε-己内酰胺）、PA26（聚己二酰乙二胺）、PA46（聚己二酰丁二胺）、PA66（聚己二酰己二胺）、PA69（聚壬二酰己二胺）、PA610（聚癸二酰己二胺）、PA611（聚十一碳二酰己二胺）、PA612（聚十二碳二酰己二胺）、PA11（聚十一烷酰胺）、PA12（聚十二烷酰胺）、PA1212（聚十二碳二酰十二碳二胺）、PA6T（聚对苯二甲酰己二胺）、PA6I（聚间苯二甲酰己二胺）、PA912（聚十二碳二酰壬二胺）、PA1012（聚十二碳二酰癸二胺）、PA9T（聚对苯二甲酰壬二胺）、PA9I（聚间苯二甲酰壬二胺）、PA10T（聚对苯二甲酰癸二胺）、PA10I（聚间苯二甲酰癸二胺）、PA11T（聚对苯二甲酰十一碳二胺）、PA11I（聚间苯二甲酰十一碳二胺）、PA12T（聚对苯二甲酰十二碳二胺）、PA12I（聚间苯二甲酰十二碳二胺）以及聚酰胺MXD6（聚己二酰间苯二胺）。
对热塑性碳纤维复合材料中碳纤维的形式没有特别限制。可以使用包含连续纤维的机织物或具有单向排列纤维的织物。在单向排列纤维的情形中，通过改变层的方向将纤维层以多层堆叠。例如，层能够交替地堆叠。此外，优选情况下堆叠面在厚度方向上对称排列。
在热塑性碳纤维复合材料中，不连续的碳纤维可以被分散并且排列以便交叠。在这种情况下，纤维长度优选为5至100mm。在不连续碳纤维的情况下，碳纤维可以以碳纤维束的状态存在于复合材料中，并且优选情况下碳纤维束和单纤维混合在一起。此外，优选情况下，不连续碳纤维在复合材料中二维随机地排列。
作为热塑性碳纤维复合材料，可以使用长纤维粒料，即通过调整熔融树脂的粘度，将连续纤维的碳纤维用熔融树脂浸渍，并且然后切割的步骤获得的粒料，并通过注射成型机模制成形。
[金属]
在本发明中使用的金属的实例具体来说包括诸如铁、不锈钢、铝、铜、黄铜、镍和锌的金属。优选情况下，构成金属的元素主要包括铁或铝。在本文中使用的术语“主要”是指以重量计90%或以上。具体来说，优选使用铁例如SS钢、SPCC钢或高强度钢，不锈钢例如SUS304或316，1000-700号铝，及其合金。
对将要接合的金属的形状没有特别限制，并能够根据所需的接合构件适合地选择。
[含有三嗪硫醇衍生物的层]
含有三嗪硫醇衍生物的层形成在金属的待接合表面上，并用于接合。含有三嗪硫醇衍生物的层不需形成在金属的待接合的整个表面上，并且对其厚度没有特别限制，只要确保胶粘度即可。三嗪硫醇衍生物的优选实例包括：能够预期化学键合于金属的含有脱水硅醇的三嗪硫醇衍生物，以及含有烷氧基硅烷的三嗪硫醇衍生物。
含有烷氧基硅烷的三嗪硫醇衍生物优选为选自由下列通式（1）和（2），以及通式（3）所表示的化合物中的至少一种：
Figure BDA00003252753900071
（在上面的通式（1）和（2）中，R1是H-、CH3-、C2H5-、CH2=CHCH2-、C4H9-、C6H5-和C6H13-中的任一个。R2是-CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2CH2CH2CH2-、-CH2CH2SCH2CH2-和-CH2CH2NHCH2CH2CH2-中的任一个。R3是-(CH2CH2)2CHOCONHCH2CH2CH2-或-(CH2CH2)2N-CH2CH2CH2-，并且在这种情况下，N和R3形成环状结构。
在上面的通式（1）和（2）中，X是CH3-、C2H5-、n-C3H7-、i-C3H7-、n-C4H9-、i-C4H9-、t-C4H9-和C6H5-中的任一个，Y是CH3O-、C2H5O-、n-C3H7O-、i-C3H7O-、n-C4H9O-、i-C4H9O-、t-C4H9O-和C6H5O-中的任一个，n是1、2和3中的任一个，并且M是-H或碱金属）
Figure BDA00003252753900081
（在上面的通式（3）中，R4是-S-、-O-、-NHCH2C6H4O-、-NHC6H4O-、-NHC6H3(Cl)O-、-NHCH2C6H3(NO2)O-、-NHC6H3(NO2)O-、-NHC6H3(CN)O-、-NHC6H2(NO2)2O-、-NHC6H3(COOCH3)O-、-NHC10H6O-、-NHC10H5(NO2)O-、-NHC10H4(NO2)2O-、-NHC6H4S-、-NHC6H3(Cl)S-、-NHCH2C6H3(NO2)S-、-NHC6H3(NO2)S-、-NHC6H3(CN)S-、-NHC6H2(NO2)2S-、-NHC6H3(COOCH3)S-、-NHC10H6S-、-NHC10H5(NO2)S-以及-NHC10H4(NO2)2S-，M’是-H或碱金属，Z是烷氧基，并且优选为具有1至4个碳原子的烷氧基，并且j是1至6的整数）。
在上面的通式（1）至（3）中，碱金属为选自锂、钠、钾、铷以及铯中的至少一种。
在本发明中使用的三嗪硫醇衍生物的优选实例具体来说包括下面的三乙氧基硅烷基丙基氨基三嗪硫醇单钠盐，其是显示出出色效应的含有烷氧基硅烷的三嗪硫醇衍生物。
Figure BDA00003252753900082
用于形成含有三嗪硫醇衍生物的层的方法的优选实例，包括在WO2009/157445的小册子中描述的方法。具体来说，示例了浸泡在含有烷氧基硅烷的三嗪硫醇、水和乙醇溶液中，取出，进行热处理，完成反应和干燥的方法。在不损害本发明的目的的范围内，含有三嗪硫醇衍生物的层可以包含除了三嗪衍生物之外的物质。
[金属化合物层]
在含有三嗪硫醇衍生物的层与金属之间，可以形成金属化合物层例如氢氧化物、碳酸盐、磷酸盐或硫酸盐，并且这种形成预期能够进一步提高接合强度，这是优选的情形。形成金属化合物层的方法优选包括在WO2009/157445中描述的方法，并且具体来说包括浸泡在酸例如盐酸、硫酸或磷酸中的方法。
[热塑性树脂层]
本发明的特征在于，在热塑性碳纤维复合材料与设置在金属上的含有三嗪硫醇衍生物的层之间设置热塑性树脂层，并且熔化热塑性树脂层，从而将金属接合到碳纤维复合材料。热塑性树脂层不需设置在待接合的整个表面上，只要确保胶粘度即可。将热塑性树脂层以薄膜形式、机织物形式、非机织物形式或粉末形式排列，并施加热和压力以将热塑性树脂熔化至一定程度，使得热塑性碳纤维复合材料的纤维能够用热塑性树脂浸渍，从而将金属接合到碳纤维复合材料。
构成热塑性树脂层的热塑性树脂优选为与热塑性碳纤维复合材料的基质树脂相容的树脂，并且优选包括与构成热塑性碳纤维复合材料的基质树脂相同的树脂。更优选地，构成热塑性树脂层的热塑性树脂和构成热塑性碳纤维复合材料的热塑性树脂是相同类型的树脂。构成热塑性树脂层的热塑性树脂的优选实例，包括与在构成热塑性碳纤维复合材料的热塑性树脂中所描述的相同的树脂。
热塑性树脂层具有优选5μm至5mm、更优选20μm至4mm、还更优选40μm至3mm的厚度。当树脂层的厚度小于5μm时，焊接所需的树脂变得不足，并存在不能获得足够强度的情况。当树脂层的厚度超过5mm时，当对两者施加剪切负荷时，力矩作用在接合表面上，并且强度整体上可能降低。通过以5μm或以上的厚度设置树脂层，能够在焊接时提供足够树脂，并且能够防止碳纤维与金属接触。结果，能够预期防止电解腐蚀，这是优选的情况。
[焊接方法]
在本发明的用于制备接合构件的方法中，在金属表面上的含有三嗪硫醇衍生物的层与碳纤维复合材料之间设置热塑性树脂层，并且熔化热塑性树脂层，从而将金属牢固地接合到碳纤维复合材料。
用于熔化热塑性树脂层的方法优选为通过加热和加压的方法。加热方法优选为通过外部加热器的热传递、辐射等。通过电磁感应加热待接合金属的方法是极为优选的，因为能够直接加热与树脂的接合表面。从最大提高接合强度的立场来看，加热金属的时间优选与成型被加热树脂的时间相匹配。然而，在所述步骤中，可以在成型后加热金属，并且再次加压以进行接合。
加热温度优选从构成热塑性树脂层的热塑性树脂的熔点温度至其分解温度，并且更优选从（熔点温度+15℃）至（分解温度-30℃）。加压条件是对焊接表面施加0.01至2MPa、优选0.02至1.5MPa、更优选0.05至1MPa的压力。当压力低于0.01MPa时，可能无法获得良好的接合强度，并且存在复合材料在加热期间弹回，并且不能维持形状，从而降低材料强度的情况。另一方面，当压力超过2MPa时，加压部分被压碎，从而可能难以维持形状或材料强度可能降低。
设置在含有三嗪硫醇衍生物的层与碳纤维复合材料之间的热塑性树脂层，可以通过事先将树脂层粘附于它们的任一侧而形成。在任一侧上形成热塑性树脂层的情况下，优选通过粘附在其表面上形成有含有三嗪硫醇衍生物的层的金属层的侧面处，设置热塑性树脂层。此外，能够通过将热塑性树脂层和碳纤维复合材料堆叠在具有附着于其的含有三嗪硫醇衍生物的层的金属层上，并同时将整体热压接合，而制备接合构件。
形成热塑性树脂层的步骤的温度更优选为从（热塑性树脂的熔化温度+15℃）至（其分解温度-30℃）。能够通过使用薄膜形式、机织物形式、非机织物形式或薄片形式的热塑性树脂，并将其热压接合或通过注射成型以小的厚度粘附熔融树脂，而排列热塑性树脂层。
当接触熔融热塑性树脂时，金属的温度优选为从（热塑性树脂的熔化温度+15℃）至（其分解温度-30℃）。当金属的温度低于该范围时，存在树脂难以适应于表面的情况。另一方面，当温度超过所述范围时，可能发生树脂的分解。如果能够确保用于将金属与热塑性碳纤维复合材料基本上接合的时间，维持温度的时间最好尽可能短。金属表面上含有三嗪硫醇衍生物的层的亲和性对于热塑性树脂层与金属之间的接合强度来说是重要的，并且一般来说存在含有三嗪硫醇衍生物的层被高温改性的顾虑。因此，长时间高温是不优选的情况。作为一个实例，在275℃下的接合时间优选为10分钟或更短。
[金属复合材料成型体]
在将含有热固性树脂作为基质的碳纤维复合材料接合到金属的情况下，在将金属插入到预浸料坯中之后，被迫使用胶粘剂或在高压釜中长时间成型。然而，本发明使用含有热塑性树脂作为基质的碳纤维复合材料，并且因此，金属的接合能够与成型步骤例如压制同时或连续进行。也就是说，本发明包括一种制备金属复合材料成型体的方法，在所述方法中将碳纤维复合材料与金属接合，其特征在于，在模具中同时进行成型和接合。
因此，本发明还涉及一种用于制备金属复合材料成型体的方法，在所述方法中将含有热塑性树脂作为基质的碳纤维复合材料与金属接合，其特征在于，在金属表面上设置含有三嗪硫醇衍生物的层，并将设置在含有三嗪硫醇衍生物的层与碳纤维复合材料之间的热塑性树脂层熔化，从而同时或连续地进行金属和碳纤维复合材料的接合和成型。在金属复合材料成型体的制备中，能够在短时段内进行成型和接合。因此，本发明的方法与使用含有热固性树脂作为基质的现有碳纤维复合材料的情况相比，是工业上优越的方法。在制备本发明的金属复合材料成型体的方法中，术语“连续进行金属和碳纤维复合材料的接合和成型”不仅包括在将金属接合到碳纤维复合材料之后连续进行成型的实施方式，而且包括在将碳纤维复合材料成型为所需形状之后连续地接合金属的实施方式。
[接合构件]
获得了包含强力接合的碳纤维复合材料和金属的接合构件。接合构件的接合强度为5MPa或以上。接合强度能够通过抗拉测试来评估，并且接合强度的上限基本上约为50MPa。在本发明中获得的接合构件和金属复合材料成型体适合地用作需要强度的结构构件。结构构件的实例包括构成移动车辆例如汽车的部件。对接合构件的接合部分的数量没有限制，并能够根据单搭接或双搭接并根据接合环境进行随意地选择。双搭接是面积变为两倍的搭接，并且因此接合强度变为两倍。
实施例
下面在实施例的基础上对本发明进行具体描述，但是本发明不限于这些实施例。
在每个实施例和比较例中的物理性质测量和评估条件如下所述。
1）接合强度
制备在每个实施例中描述的5个接合构件，并且将利用通用测试机INSTRON5587以1mm/min的速率进行抗拉测试所获得的抗拉强度值定义为接合构件的接合强度。
[参比例1]
连续纤维0°和90°交替堆叠材料的碳纤维复合材料的制备
将连续碳纤维（TENAX STS40-24KS（纤维直径：7μm，抗拉强度：4,000MPa），由Toho Tenax Co.,Ltd.制造）以0°和90°的纤维方向交替堆叠成64层，同时堆叠尼龙6膜（UNITIKA EMBLEM ON，25μm厚）（碳纤维：64层，尼龙：65层），并将得到的组装体在260℃加热下在2MPa压力下压制20分钟。因此，制备了具有0°和90°交替纤维，对称堆叠，碳纤维体积比为47%（碳纤维以质量计的含量为57%）并且厚度为2mm的碳纤维复合材料。
[参比例2]
包含随机材料的平板碳纤维复合材料的制备
将切成平均纤维长度为16mm的碳纤维（TENAX STS40，平均纤维直径：7μm，由Toho Tenax Co.,Ltd.制造）随机排列，以制造平均密度为540g/m2的纤维片，并且夹在10片UNITIKA KE435-POG（尼龙6）布之间。将得到的组装体在260℃和2.5MPa下压制，以制备碳纤维体积比为35%（碳纤维以质量计的含量为45%）并且厚度为2mm的平板碳纤维复合材料。
[金属表面处理]
将长度为100mm、宽度为25mm、并且厚度为1.6mm的金属片，在浓度为15.0g/L的氢氧化钠水溶液中，在60℃温度下脱脂60秒。然后将金属片用水清洗60秒，在烘箱中在80℃下干燥30分钟。将金属片在浓度为30至50g/L的磷酸水溶液（除了水之外，90%或以上的组分是磷酸）中浸泡300秒，然后用热水（60℃）清洗60秒，并且用水清洗60秒，以在金属片的表面上形成包含金属磷酸盐和氢氧化物作为主要组分的金属化合物涂层膜。将具有金属化合物涂层膜的金属片，在浓度为0.7g/L的三乙氧基硅烷基丙基氨基三嗪硫醇单钠盐的乙醇/水（体积比：95/5）溶液中，在室温下浸泡30分钟。将金属片在烘箱中，在160℃下热处理10分钟。将金属片在含有浓度为1.0g/L的N,N’-间苯二马来酰亚胺和浓度为2g/L的过氧化二异丙苯的丙酮溶液中，在室温下浸泡10分钟，并在烘箱中在150℃下热处理10分钟。将浓度为2g/L的过氧化二异丙苯的乙醇溶液在室温下喷洒到金属片的整个表面，并且空气干燥，以在金属片的整个表面上设置三嗪硫醇衍生物层。
[实施例1]
将上述的金属表面处理应用于长度为100mm、宽度为25mm、并且厚度为1.6mm的SPCC（冷轧碳钢片）的两个表面，并在其两个表面上设置两个尼龙6膜（UNITIKA EMBLEM ON，25μm厚，熔点：225℃）。通过电磁感应加热将SPCC片加热至250℃，并且然后立即冷却至常温。将尼龙膜熔化并紧密附着，并且然后固化，以在SPCC表面上形成尼龙6的层。将在参比例2中获得的碳纤维复合材料切割成100mm的长度和25mm的宽度，通过单搭接堆叠在具有尼龙层的SPCC片上25mm×25mm的范围内，并且使用模具在250℃加热下在0.2MPa下加压5分钟，以在热塑性碳纤维复合材料与SPCC片之间制备接合构件。制备5个接合构件，并利用通用测试机INSTRON5587以1mm/min的速率进行抗拉测试。结果，接合强度的平均值为12MPa。
[实施例2]
将上述的金属表面处理应用于长度为100mm、宽度为25mm、并且厚度为1.6mm的590MPa类型的高强度钢的两个表面，并在其两个表面上设置两个尼龙6膜（UNITIKA EMBLEM ON，25μm厚）。通过电磁感应加热将高强度钢加热至250℃，并且然后立即冷却至常温。将尼龙膜熔化，紧密附着并且固化，以在高强度钢表面上形成尼龙6的层。将在参比例2中获得的包含随机材料的平板切割成100mm的长度和25mm的宽度，通过单搭接堆叠在具有尼龙层的高强度钢上25mm×25mm的范围内，将热塑性碳纤维复合材料在250℃下加热，并且将高强度钢加热至140℃，然后使用模具在加热下在0.2MPa下加压1分钟。随后，通过电磁感应加热将在堆叠的材料中的高强度钢加热至250℃，并且在加热下在0.2MPa下加压1分钟，以在热塑性碳纤维复合材料与高强度钢之间制备接合构件。制备5个接合构件，并利用通用测试机INSTRON5587以1mm/min的速率进行抗拉测试。结果，接合强度的平均值为17MPa。
[实施例3]
在与实施例1中相同的步骤中经历过金属表面处理的长度为100mm、宽度为25mm、并且厚度为1.6mm的SPCC片的两个表面上，设置两个尼龙6膜（UNITIKA EMBLEM ON，25μm厚）。将在参比例1中获得的碳纤维复合材料切割成100mm的长度和25mm的宽度，加热至250℃，通过单搭接堆叠在具有尼龙6层的SPCC片上25mm×25mm的范围内，并使用模具在加热下与之前通过电磁感应加热法加热至250℃的SPCC片一起，在0.2MPa下加压5分钟，以在热塑性碳纤维复合材料与SPCC之间制备接合构件。制备5个接合构件，并利用通用测试机INSTRON5587以1mm/min的速率进行抗拉测试。结果，接合强度的平均值为7.4MPa。
[实施例4]
除了使用厚度为1mm的5052铝片代替SPCC片，以与实施例1中相同的方式在铝片的表面上形成尼龙6的层。将在参比例2中获得的包含随机材料的平板切割成100mm的长度和25mm的宽度，通过单搭接堆叠在具有尼龙层的铝片上25mm×25mm的范围内，然后使用模具在250℃加热下在0.2MPa下加压5分钟，从而在热塑性碳纤维复合材料与5052铝片之间制备接合构件。制备了5个接合构件，并利用通用测试机INSTRON5587以1mm/min的速率进行抗拉测试。结果，铝片部断裂。从铝片的断裂强度计算，发现接合强度为7.1MPa或以上。
[比较例1]
进行与实施例1中相同的操作，区别在于没有在经历过金属表面处理的长度为100mm、宽度为25mm、并且厚度为1.6mm的SPCC片上设置尼龙6层，并且代替在参比例2中获得的碳纤维复合材料，将具有相同尺寸的尼龙6片进行接合。然而，作为试图测量获得的接合构件的接合强度的结果，尼龙6片脱落。
[实施例5]
将在参比例1中获得的碳纤维复合材料加热至250℃，并且在140℃下使用模具在20MPa压力下压制，以获得图2中所示的长度为1,200mm、宽度为150mm、并且高度为50mm的近似U-形的成型体。如图2中所示，在成型体中形成直径为10mm的5个孔。在其中心处具有直径为10mm的孔，并且已在与实施例1中相同的步骤中经历金属表面处理的直径为100mm，厚度为1.6mm的SPCC片，经由具有相同尺寸的两个尼龙6膜（UNITILA EMBLEM ON，25μm厚）置于5个孔的每一个上。通过电磁感应加热将得到的组装体加热至250℃，并且通过20kgf（196N）的力对SPCC片进行加压直至达到约100℃，从而接合到成型体。因此，获得了金属复合材料成型体。所述金属复合材料成型体能够用作座椅横档的一部分，并且其形状示出在图3中。
工业实用性
本发明的接合构件具有出色的接合强度，并能够用于例如构成诸如汽车的移动车辆的部件的各种用途中。

Claims (7)

1.一种用于制备在含有热塑性树脂作为基质的碳纤维复合材料与金属之间的接合构件的方法，该方法包括：
在所述金属的表面上形成含有三嗪硫醇衍生物的层；
在所述含有三嗪硫醇衍生物的层与所述碳纤维复合材料之间设置所述热塑性树脂层；以及
熔化所述热塑性树脂层以将所述金属接合到所述碳纤维复合材料。
2.根据权利要求1所述的用于制备接合构件的方法，其中，利用电磁感应的方法加热所述金属以进行所述接合。
3.根据权利要求1至2任一项所述的用于制备接合构件的方法，其中，所述热塑性树脂层具有5μm至5mm的厚度。
4.根据权利要求1至3任一项所述的用于制备接合构件的方法，其中，构成所述金属的元素主要包含铁或铝。
5.根据权利要求1至4任一项所述的用于制备接合构件的方法，其中，在所述碳纤维复合材料中存在的所述热塑性树脂的量为每100重量份碳纤维50至1,000重量份。
6.一种接合构件，该接合构件包括以5MPa或以上的接合强度接合的热塑性碳纤维复合材料和金属，所述接合构件通过权利要求1至5任一项的制备方法而获得。
7.一种用于制备金属复合材料成型体的方法，所述成型体包括接合的含有热塑性树脂作为基质的碳纤维复合材料和金属，所述方法包括：在所述金属的表面上形成含有三嗪硫醇衍生物的层，并且熔化设置在所述含有三嗪硫醇衍生物的层与所述碳纤维复合材料之间的所述热塑性层，以同时或连续地进行所述金属与所述碳纤维复合材料之间的接合以及其成型。
CN2011800569657A 2010-11-30 2011-11-25 制备用于碳纤维复合材料的接合构件的方法 Pending CN103298601A (zh)

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