CN1906027A - 两面导体聚酰亚胺积层体的连续制造方法 - Google Patents

两面导体聚酰亚胺积层体的连续制造方法 Download PDF

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Publication number
CN1906027A
CN1906027A CNA2004800404673A CN200480040467A CN1906027A CN 1906027 A CN1906027 A CN 1906027A CN A2004800404673 A CNA2004800404673 A CN A2004800404673A CN 200480040467 A CN200480040467 A CN 200480040467A CN 1906027 A CN1906027 A CN 1906027A
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laminate
conductive metal
polyimide
hot pressing
roller
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CN1906027B (zh
Inventor
宫本和弥
德光明
井伊正一
重松义浩
日笠山伊知郎
菅野胜浩
中川雄次郎
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Nippon Steel Chemical and Materials Co Ltd
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Nippon Steel Chemical Co Ltd
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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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/02—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
    • 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
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/1429—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface
    • B29C65/1432—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface direct heating of the surfaces to be joined
    • 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
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/1429—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface
    • B29C65/1454—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface scanning at least one of the parts to be joined
    • B29C65/1458—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface scanning at least one of the parts to be joined once, i.e. contour welding
    • 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
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/1429—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface
    • B29C65/1464—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the way of heating the interface making use of several radiators
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C65/78—Means for handling the parts to be joined, e.g. for making containers or hollow articles, e.g. means for handling sheets, plates, web-like materials, tubular articles, hollow articles or elements to be joined therewith; Means for discharging the joined articles from the joining apparatus
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    • B29C65/7888—Means for handling of moving sheets or webs
    • B29C65/7894—Means for handling of moving sheets or webs of continuously moving sheets or webs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
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    • B29C66/1122—Single lap to lap joints, i.e. overlap joints
    • 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
    • B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
    • B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
    • B29C66/45—Joining of substantially the whole surface of the articles
    • 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
    • B29C66/71—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 characterised by the composition of the plastics material of the parts to be joined
    • 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
    • B29C66/72—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 characterised by the structure of the material of the parts to be joined
    • B29C66/723—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 characterised by the structure of the material of the parts to be joined being multi-layered
    • B29C66/7232—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 characterised by the structure of the material of the parts to be joined being multi-layered comprising a non-plastics layer
    • B29C66/72321—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 characterised by the structure of the material of the parts to be joined being multi-layered comprising a non-plastics layer consisting of metals or their alloys
    • 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
    • B29C66/73—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 characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—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 characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7392—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 characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
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    • B29C66/83—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools
    • B29C66/834—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools moving with the parts to be joined
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • 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
    • B29C66/914—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux
    • B29C66/9141—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature
    • B29C66/91411—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature of the parts to be joined, e.g. the joining process taking the temperature of the parts to be joined into account
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/90—Measuring or controlling the joining process
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    • B29C66/9141—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/90—Measuring or controlling the joining process
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/90—Measuring or controlling the joining process
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    • H—ELECTRICITY
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Abstract

本发明的课题是提供在辊卷绕状态下连续制造没有纵向皱褶等外观缺陷、质量稳定的两面导体聚酰亚胺类积层体的两面导体聚酰亚胺积层体的连续制造方法，该两面导体聚酰亚胺积层体的连续制造方法将在导电性金属箔(M1)上具有底层、中间主层、顶层至少三层聚酰亚胺类树脂层的单面导体积层体和包括导电性金属箔(M2)的基材连续导入到一对热压辊之间，在上述顶层上通过热压使导电性金属箔(M2)积层一体化，其特征在于：将导入热压辊间之前的单面导体积层体和导电性金属箔(M2)分别在惰性气体气氛下预加热到大于等于200℃～小于等于顶层的聚酰亚胺类树脂的玻璃化转变温度，然后使它们与热压辊表面接触。

Description

两面导体聚酰亚胺积层体的连续制造方法
技术领域
本发明涉及对于作为与电子设备类的小型化、轻量化要求相适应的配线材料的柔性印刷电路板等适合采用的两面导体聚酰亚胺积层体的连续制造方法，特别是涉及利用了热压辊、可以稳定生产不产生皱褶、而且也无质量偏差的辊卷绕产品的两面导体聚酰亚胺积层体的连续制造方法。
技术背景
近年来，随着高功能化的移动电话、数码相机、导航仪、其他各种电子设备类的小型化、轻量化的发展，作为其中使用的电子配线材料的柔性印刷电路板(配线基板)的小型高密度化、多层化、精密化、低介电化等要求高涨。关于该柔性印刷配线基板，以前是用可低温固化的粘接剂贴合聚酰亚胺膜和金属箔以进行制造，但存在粘接剂层使作为配线基板的特性下降，特别是有损聚酰亚胺基膜的优异耐热性、阻燃性等问题。而且作为具有粘接剂层的其他问题，还有配线的电路加工性变差的问题。
具体而言，可以列举通孔加工时钻孔引起的树脂污点的产生、导体通孔加工时的尺寸变化率大等问题。特别是两面通孔结构的场合(以绝缘体层即基膜为中心，在其两面上通过粘接剂贴合导体的铜箔等而形成的结构等)，存在与单面结构的柔性印刷电路板相比，通常其柔软性低的问题。另一方面，随着IC的高密度化、印刷电路的微细化、高密度化，存在发热增大，需要与热的良导体贴合的场合。另外，也存在为了更加紧凑而使外壳和配线一体化的方法。还存在需要电容不同的配线，需要更加耐高温的配线材料的情况。因此，提出了不使用粘接剂，在铜箔等导体上直接涂布固化前的聚酰胺酸溶液，加热使其固化的各种柔性印刷电路板的制造方法。
例如，可以列举将固化物的线膨胀系数小于等于3.0×10-5的由二胺和四羧酸酐合成的聚酰胺酸涂布在金属箔上、加热使其固化(参照例如专利文献1)，将含有具有特定结构单元的聚酰胺酰亚胺前体化合物的树脂溶液涂布在导体上、使其酰亚胺化(参照例如专利文献2)，将具有由包含二氨基-N-苯甲酰苯胺或其衍生物的二胺类和芳香族四羧酸反应得到的结构单元的绝缘材料的前体溶液直接涂布在导体上并使其固化(参照例如专利文献3)等。而且还提出了为了提高与金属箔的密合性，通过在导体上使用多种聚酰亚胺前体树脂溶液，进行多次涂布和干燥，制造具有多个聚酰亚胺树脂层的柔性印刷配线用基板的方法(参照例如专利文献4)。
这些柔性印刷配线基板涉及仅在导电性金属箔的单面侧，不用粘接剂而是利用加热固化使绝缘体层粘接的单面结构。另一方面，应对电子设备类的小型化、轻量化，本发明人等提出首先使用在导电性金属箔(M1)的单面上具有至少三层聚酰亚胺层的单面导体积层体，在该聚酰亚胺层上在加热加压下积层导电性金属箔(M2)的两面导体聚酰亚胺积层体的制造方法(参照例如专利文献5)。该两面导体积层体特别是可以在基板的两面上形成配线电路，为了进行高密度安装，已经实用化，近年来在各种领域中广泛采用。
在上述专利文献5的两面导体聚酰亚胺积层体的制造方法中，公开了利用了热压装置等的分批方式的具体例子。在该分批方式的热压装置等中，在称为热板的基座上，同时载置多层单面导体积层体和导电性金属箔的组合并加热压接。通常加热由配置在热板内的电加热器进行，压力则是利用油压将基座推起，通过板材使压力传递到上部基座以维持规定压力。在该热板中，因为加热器的温度偏差大，所以即使进行各种校正，也存在由于加热不足、加热过剩而局部产生不良部位的场合。
而且在同时对多层进行处理的场合，由于长时间的加热而促进了积层树脂层的劣化，是每一件号的最佳条件窄、非常不稳定的方法。而且，因为反复进行从常温加热加压、到达一定温度后冷却的分批方式的循环以生产积层基材，所以不仅生产效率低，而且需要积层基材的切断操作，此时容易卷入异物，在附着异物的场合，积层的物质上全部转印异物的形状，引起外观缺陷的情况多。因此，强烈要求采用连续方式的质量稳定的两面导体聚酰亚胺积层体的制造方法。
专利文献1：特开昭62-212140号公报
专利文献2：特开昭63-84188号公报
专利文献3：特开昭63-245988号公报
专利文献4：特公平6-49185号公报
专利文献5：特开平10-323935号公报
发明内容
本发明人等取代在先提出的专利文献5中的两面导体聚酰亚胺积层体的制造方法中的利用了热压装置等的分批方式，对通过采用一对热压辊的加热压接连续制造两面导体聚酰亚胺积层体的方法进行了研究，其结果得知存在各种应该解决的问题，即如果在装入压辊间之前的基材传送条件和预热方法与从压辊出口的传送条件和冷却方法不适合，则发现基材在通过中产生近10种热胀·冷缩引起的格子皱褶、集束皱褶等皱褶，而且在辊面的平滑度太高的状态下，基材和辊面的密合度变强，在移动中容易产生很多由于卷绕导致的复杂皱褶(以下称为皱折(torare))和杂质引起的凹痕(产品表面上几十微米的冲击痕)等。
因此，本发明的目的是提供在聚酰亚胺类树脂层的两面上不通过粘接剂而积层导电性金属层的没有纵皱褶等外观缺陷的品质稳定的两面导体聚酰亚胺类积层体的连续制造方法。而且，本发明的其他目的是提供在辊卷绕状态下制造两面导体聚酰亚胺积层体的方法，该两面导体聚酰亚胺积层体具有用户需求特别强的优异的配线电路加工性，而且作为配线电路板具有优异的耐热性、挠性。
本发明人等对上述问题进行了刻苦研究，结果发现通过将就要导入热压辊间的单面导体积层体和导电性金属箔(M2)预加热到特定温度，通过使用对压辊表面进行了表面粗糙化处理到特定表面粗糙度(Ra)的压辊，实现了上述目的，从而完成本发明。
即本发明涉及：
(1)两面导体聚酰亚胺积层体的连续制造方法，将在导电性金属箔(M1)上具有底层、中间主层、顶层至少三层聚酰亚胺类树脂层的单面导体积层体和包括导电性金属箔(M2)的基材连续导入一对热压辊之间，在上述顶层上通过热压使导电性金属箔(M2)积层一体化，其特征在于：在将就要导入热压辊间的单面导体积层体和导电性金属箔(M2)分别预加热到大于等于200℃～小于等于顶层的聚酰亚胺类树脂的玻璃化转变温度之后，使它们与热压辊表面接触。
(2)将上述本发明的一对压辊表面的平均表面粗糙度(Ra)表面粗糙化处理到0.01～5μm，优选在惰性气体气氛下，在使压辊表面温度为340～390℃、压辊间的线压为50Kg/cm～300Kg/cm(490～2940N/cm)、通过时间为2～5秒的条件下进行热压。
(3)将上述本发明的单面导体积层体和导电性金属箔(M2)从辊卷绕状态拉出，经由中心轴高度各不相同的多个导辊，优选在氮气气氛下使平面性提高的状态下对它们进行预加热。
(4)优选上述本发明的预加热由配置在基材与热压辊表面接触的位置上的内置加热装置的导辊进行。
(5)优选在上述本发明的辊表面上热喷涂陶瓷被膜，形成表面粗糙度(Ra)。
根据本发明，通过在惰性气体气氛下将导入热压辊之间之前的单面导体积层体和导电性金属箔(M2)在大于等于200℃～小于等于玻璃化转变温度的温度(优选200～350℃)下分别进行预加热，然后使它们与热压辊表面接触，从而使热压时急剧的温度上升得到缓和，结果是防止两面导体积层体的表面上纵向条纹等外观缺陷。而且通过将热压辊的表面粗糙度保持在特定条件，基材和辊表面的密合度减小，从而也防止了移动中卷绕导致的复杂皱褶(以下称为皱折)、凹痕(产品表面上几十微米的冲击痕)等的发生。
附图说明
图1是表示本发明的两面导体聚酰亚胺积层体的制造方法的简要流程。
图2是表示预加热用导辊的一个例子的简要纵截面图。
图3是表示热压辊的一个例子的简要纵截面图。
符号说明
1   单面导体积层体
2   导电性金属箔
3   导辊
3′ 预加热用导辊
4   导辊
4′ 预加热用导辊
5   热压辊
6   热压辊
7   两面导体聚酰亚胺积层体
8   导辊
9   辊卷绕产品
10  氮气气氛的处理室
11  氮密封机构
12  中心轴
13  利用轴承等的旋转支撑部件
14  加热装置
17  加热管
具体实施方式
以下，对用于实施本发明的最佳方式进行详细说明。首先，作为在本发明中使用的导电性金属箔(M1和M2)，可以列举厚度5～150μm的铜、铝、铁、银、钯、镍、铬、钼、钨、锌及它们的合金等，优选铜。特别是，也适合使用由于刚性低、采用热压的压力控制困难而避免使用的轧制铜箔产品。为了提高粘接力，也可以在其表面上实施siding、镀镍、镀铜-锌合金或者利用醇化铝、铝螯合物、硅烷偶联剂等的化学或机械表面处理。
其中，作为使绝缘体层即聚酰亚胺类树脂在不用粘接剂的情况下加热固化、粘接在导电性金属箔(M1)的单面上的单面导体积层体，可以采用由上述专利文献1～4和5公开的公知的积层体。作为绝缘体层使用的聚酰亚胺类树脂是具有酰亚胺环结构的树脂的总称，可以列举例如聚酰亚胺、聚酰胺酰亚胺、聚酯酰亚胺等。作为聚酰亚胺类树脂层，能够利用上述专利文献1～4中所述的低热膨胀性物质、加热时熔融或软化的热塑性聚酰亚胺等，不作特别限定。但是特别优选的绝缘体层是包含由专利文献5中所述的由聚酰亚胺前体树脂溶液的加热固化得到的热塑性聚酰亚胺类树脂形成的底层、由低热膨胀性聚酰亚胺类树脂形成的中间主层、以及由热塑性聚酰亚胺类树脂形成的顶层至少三层聚酰亚胺类树脂层的绝缘体层。
其中，作为形成中间主层的低热膨胀聚酰亚胺类树脂，其线膨胀系数优选小于等于30×10-6(1/℃)，在薄膜的耐热性、挠性方面具有优异的性能。其中，线膨胀系数是使用酰亚胺化反应充分完成后的试料，利用热机械分析仪(TMA)，求出升温到250℃后，以10℃/分钟的速度冷却，在240～100℃的范围内的平均线膨胀系数。作为具有这样的性质的低热膨胀聚酰亚胺类树脂的具体例子，优选是上述专利文献5中所述的具有由下述通式(I)所示单元结构的聚酰亚胺类树脂。
(式中R1～R4表示低级烷基、低级烷氧基、卤素基或氢)。
而且，作为底层和顶层使用的热塑性聚酰亚胺类树脂，只要其玻璃化转变温度小于等于350℃，可以为任何结构，优选在加热加压下压接时其界面的粘接强度足够的热塑性聚酰亚胺类树脂。这里所说的热塑性聚酰亚胺类树脂也包含在大于等于玻璃化转变温度的通常状态下不一定显示出充分的流动性，可以通过加压进行粘接的树脂。作为具有这样的性质的热塑性聚酰亚胺类树脂的具体例子，具有由上述专利文献5所述的下述通式(II)、通式(III)表示的单元结构。
(式中Ar1是2价的芳香族基团，其碳原子数大于等于12)。
(式中Ar2是2价的芳香族基团，其碳原子数大于等于12)。
其中，作为2价的芳香族基团Ar1或Ar2的具体例，可以列举例如：
等，优选
Figure A20048004046700094
此外，作为单面导体积层体的制造方法，如上述专利文献5中所述的那样，在聚酰亚胺前体溶液或聚酰亚胺溶液中添加公知的酸酐类、胺类固化剂等固化剂，硅烷偶联剂、钛酸酯偶联剂、环氧化合物等粘接性赋予剂，橡胶等挠性赋予剂等各种添加剂和催化剂，涂布到导电性金属箔(M1)上，然后通过热处理使之热固化，能够得到单面导体积层体。而且，优选单面导体积层体是在导电性金属箔(M1)上积层热塑性聚酰亚胺类树脂层作为底层，积层低热膨胀性聚酰亚胺类树脂层作为中间主层，再积层热塑性聚酰亚胺类树脂层作为顶层(最表面层)。其中，在中间主层中不包含低热膨胀性聚酰亚胺类树脂层的场合，由加热固化工序得到的单面导体积层体的弯曲、卷曲变大，以后工序中的操作性显著下降。而且，如果顶层(最表面层)中不包含热塑性聚酰亚胺类树脂层，则热压辊工序中与导电性金属箔的热压接产生的粘接力没有被充分发挥，所以不优选。
此时，低热膨胀性聚酰亚胺类树脂层的厚度t1和热塑性聚酰亚胺类树脂层的厚度t2的厚度比(t1/t2)在2～100的范围内，优选5～20的范围内。如果该厚度比(t1/t2)比2小，则与金属箔的热膨胀系数相比，聚酰亚胺类树脂层整体的热膨胀系数变得过高，由该第一工序得到的单面导体积层体的弯曲、卷曲变大，在接下来的第二工序中的操作性显著下降。而且，如果热塑性聚酰亚胺类树脂层的厚度t2过小，厚度比(t1/t2)增大到超过100，则会产生第二工序的热压接产生的粘接力没有被充分发挥的情况。
将这些多种聚酰亚胺类树脂涂布到导电性金属箔(M1)上能够以其树脂溶液的形式进行，但优选如上述专利文献4、5中所述的那样，以其前体溶液的形式，在一起或依次涂布多种前体溶液或者在小于等于酰亚胺闭环温度的脱溶剂处理后，一起进行前体向聚酰亚胺的加热转换。如果在完全转换成聚酰亚胺的层上进一步涂布别的聚酰亚胺类前体溶液，进行热处理使其进行酰亚胺闭环，则存在各聚酰亚胺类树脂层之间的粘接力没有充分被发挥的情形，成为使制品的两面积层体的质量下降的原因。
作为在导电性金属箔(M1)上涂布聚酰亚胺类树脂溶液或其前体溶液(聚酰胺酸溶液)的方法，能够使用例如刮板式涂布机、压模涂布机、辊式涂布机、帘式涂布机等，采用公知的方法进行，特别是在进行厚涂的场合，适合采用压模涂布机、刮板式涂胶机。而且，涂布时使用的聚酰亚胺类前体溶液的聚合物浓度还取决于聚合物的聚合度，但通常为5～30重量％，优选10～20重量％。如果聚合物的浓度低于5重量％，则一次涂布不能得到足够的膜厚，如果高于30重量％，则溶液粘度过高，不容易涂布。
接着对在导电性金属箔上以均一厚度涂布的聚酰胺酸溶液进行热处理，除去溶剂，进而使其进行酰亚胺闭环。此时，如果在高温下快速进行热处理，则在树脂表面生成表层，溶剂难以蒸发，或者起泡，所以优选在从低温缓缓上升到高温的同时进行热处理。此时最终的热处理温度通常优选为300～400℃，在大于等于400℃时，慢慢产生聚酰亚胺的热分解，如果小于等于300℃，则聚酰亚胺被膜在导电性金属箔上没有充分取向，不能得到平面性好的单面导体积层体。这样形成的作为绝缘体的聚酰亚胺类树脂层的整体厚度通常为10～150μm。
下面，根据附图进行详细说明。图1是表示将本发明的单面导体积层体和导电性金属箔(M2)导入到一对压辊之间，通过加热压接使其积层一体化的两面导体聚酰亚胺积层体的制造方法的简要流程。图2是表示预加热用导辊的一个例子的简要纵截面图。图3是表示压辊的一个例子的简要纵截面图。
在图1中，使由聚酰亚胺类树脂形成的绝缘体层加热固化而粘接在上述导电性金属箔(M1)的单面上的单面导体积层体1和导电性金属箔(M2)2都从辊卷绕状态被连续拉出，经过中心轴高度不同的多个导辊3、3′、4、4′等，在提高了平面性的状态下被预加热后，在与一对热压辊5、6的表面接触的状态下，通过压辊之间产生的加压点，从而形成通过加热压接使导电性金属箔(M2)在上述单面导体积层体1的顶层上积层一体化的两面导体聚酰亚胺积层体7，然后，利用适宜用于冷却的喷射惰性气体等的冷却装置c进行预冷却，然后，经过多个导辊8、8′，在外部空气中进一步被冷却，同时形成辊卷绕产品9。
其中，优选的是，为了防止导电性金属箔氧化，将多个导辊3、3′、4、4′、8、8′等和一对热压辊5、6配置在保持在大于等于大气压的氮气等惰性气体气氛下的处理室10内，而且在基材导入口以及积层体的排出口设置密封机构(迷宫式密封)11。其中，虽然没有示出，但优选从辊卷绕状态被连续拉出的单面导体积层体1和导电性金属箔(M2)2在导入到处理室10内之前，分别经由中心轴高度不同的多个导辊，在张紧状态下提高平面性。而且，虽然没有示出，但优选从处理室10拉出后的两面导体聚酰亚胺积层体在成为辊卷绕制品9之前，也在外部空气中分别在张紧状态下经过中心轴高度不同的多个导辊，进一步降低表面温度。
特别地，作为本发明中在平面性提高的状态下进行预加热的装置，可以使热压辊5、6之前与其最接近的导辊3′(4′)为加热装置内置型，或者就在热压辊之前设置加热灯或放出辐射能的加热器h1、h2等进行预加热，或者同时使用两种预加热装置。这里，利用图2说明特别优选的加热装置内置型的预加热用导辊的一个例子。在图2中，在导辊3′(4′)中，内部为空腔的外周部和从空腔两端突出的中心轴12通过配置在辊外周部的两端内部的轴承等旋转支撑部件13而成为一体，而且辊外周部的结构是利用该旋转支撑部件13在中心轴12的周围自由旋转。
而且，在辊内部的中心轴12上，分离地或一体化地适当固定从利用介电加热的加热线圈、红外线加热器、电阻加热线圈等中选择的利用辐射热的加热控制装置14，通过改变流向这些加热装置的电流值，控制向辊的内壁面照射的辐射热能。而且，在辊外表面附近，埋入配置填充有导热性良好的有机加热介质的称为夹套或加热管的传热元件17。在该加热管中，因为热量从上述中心轴12的加热装置14瞬间传送到辊的整个外表面，所以表面温度精度高，几乎不产生轴向的温度差。
其中，导入热压辊之间之前的单面导体积层体1和导电性金属箔(M2)2的预加热温度为200℃～顶层树脂即热塑性聚酰亚胺类树脂的玻璃化转变温度，优选200～350℃。优选该预加热辊外表面温度由埋入辊表面的温度传感器监视，以使该温度始终保持规定温度的方式，控制向加热控制装置14供给的电流值。在不进行预加热的场合，或者预加热温度小于等于200℃时，极薄的金属箔在通过热压辊之间时急剧升温并被压接，结果在积层体的表面产生很多纵向条纹、横向皱褶和集束皱褶等，从而不仅导致外观缺陷，而且粘接性降低，所以不优选。另外，在玻璃化转变温度以上时，聚酰亚胺类树脂劣化，所以也不优选。
下面，如图3所示，一对热压辊5(6)在结构上与图2说明的加热装置内置型的导辊3′(4′)相同，与图2中赋予的符号相同的符号表示的含义和图2中说明的相同，不同点在于其直径大，并且加热装置被分割为14、15、16这3部分，而且由未图示的搅拌动力机构使其强制旋转。在压辊外表面附近，埋入填充了传热性良好的有机加热介质的被称为夹套或加热管的传热元件17，从而设置使表面温度均一化的装置。优选压辊外表面温度大于等于热塑性聚酰亚胺类树脂的玻璃化转变温度，更优选控制为360～390℃的范围内的设定值。优选该压辊外表面温度由埋入辊表面的温度传感器监视，以控制向加热控制装置14、15、16供给的电流值。
虽然未示出，但上述一对热压辊5、6在氮气气氛下上下配置，将至少一个压辊保持在中心轴12的两侧，由利用油压或齿轮的加压装置使其移动到规定位置，对两者的间隙进行调整，从而最佳压力从压辊向导入的基材1、2相互传送。此时，优选在热压辊间的线压50～500Kg/cm(490N/cm～4900N/cm)、优选100～300Kg/cm(980N/cm～2940N/cm)、通过时间2～5秒的条件下进行热压。
而且，优选所使用的一对热压辊是在使压辊的平均表面粗糙度(Ra)为0.01～5μm、优选0.1～3μm的表面粗糙化状态下使用。压辊的表面粗糙度(Ra)小于等于0.01μm时，从加热辊之间出来的两面导体聚酰亚胺积层体由于与辊密合而产生皱折，在移动中产生皱褶，不能避免附着铜箔粉等异物而引起的凹痕(制品表面上几十微米的冲击痕，或者凹陷)等的产生。另外，在大于等于5μm时，因为辊表面的凹凸转印到积层体表面上，所以不优选。为了使辊表面为上述范围内的粗糙面，能够通过热喷涂陶瓷被膜进行调整。由利用金刚石针的触针式表面粗糙度计求出表面粗糙度(Ra)。
而且，优选的是，在图1中，在形成由热压辊5和6通过热压使导电性金属箔(M2)在单面导体积层体1的顶层上积层一体化的两面导体聚酰亚胺积层体7后，利用喷射用于冷却的惰性气体等的冷却装置c进行预冷却，但因为在冷却装置c产生的冷却温度过于急剧地冷却的场合，在积层体7上产生弯曲而不优选，所以优选与上述预加热温度相同的200℃～顶层树脂即热塑性聚酰亚胺类树脂的玻璃化转变温度，优选200～300℃。
由本发明得到的两面导体型聚酰亚胺积层体在作为绝缘体的聚酰亚胺类树脂层的两面上具有作为导体的导电性金属层，是外观良好、没有产生皱褶、而且不存在质量偏差的辊卷绕制品，随着高功能化的移动电话、数码相机、导航仪、其他各种电子设备类的小型化、轻量化的发展，适合于作为使用的电子配线材料。
实施例
以下，基于实施例和比较例，对本发明的实施方式进行具体说明。在以下的实施例和比较例中，用下述方法测定线膨胀系数、单面覆铜产品的卷曲和粘接力。
即，线膨胀系数利用精工电子工业株式会社制造的热机械分析仪(TMA100)，升温到250℃后以10℃/分的速度冷却，计算在240℃～100℃之间的平均线膨胀系数而求出。单面覆铜产品的卷曲是测定热处理、酰亚胺化后尺寸100mm×100mm的覆铜产品的曲率半径。
单面覆铜产品的粘接力是根据JIS C5016：7.1项，使用导体宽度3mm的图案，求出在180°的方向将铜箔以50mm/分的速度剥离时的值。
另外，在实施例和比较例中，使用以下的缩写。
PMDA：均苯四甲酸酐
BTDA：3，3′，4，4′-二苯甲酮四甲酸酐
DDE：4，4-二氨基二苯醚
MABA：2′-甲氧基-4，4′-二氨基-N-苯甲酰苯胺
(合成例1)
在玻璃制反应器中边通入氮气边放入2532g的N，N-二甲基乙酰胺，接着在搅拌的情况下加入0.5mol的DDE和0.5mol的MABA，然后使其完全溶解。将该溶液冷却到10℃，一点一点地添加1mol PMDA使反应液保持在小于等于30℃的温度，在添加结束之后，继续在室温下搅拌2小时，使聚合反应完成。得到的聚酰亚胺前体溶液具有15重量％的聚合物浓度，利用B型粘度计在25℃下测得的表观粘度为1000mPa·s。
(合成例2)
除了使用1mol的DDE作为二胺成分，使用1mol的BTDA作为酸酐成分之外，与合成例1同样地调制聚酰亚胺前体溶液。得到的聚酰亚胺前体溶液具有15重量％的聚合物浓度，利用B型粘度计在25℃下测得的表观粘度为300mPa·s。
(积层体的制作)
在35μm辊状的电解铜箔(Nikko Gould社制)的粗糙化表面上，利用压模涂布机以12μm的厚度均匀涂布在合成例2中调制的聚酰亚胺前体溶液2，然后用120℃的热风干燥炉进行连续处理以除去溶剂。接着在该聚酰亚胺前体层上，利用反转式辊式涂布机以200μm的厚度均匀涂布在合成例1中调制的聚酰亚胺前体溶液1，然后用120℃的热风干燥炉进行连续处理以除去溶剂，再以15μm的厚度均匀涂覆在合成例2中调制的聚酰亚胺前体溶液2，接下来在热风干燥炉中用30分钟从120℃升温到360℃，热处理使其酰亚胺化，得到聚酰亚胺树脂层的厚度为25μm、没有弯曲和卷曲的平面性良好的单面覆铜产品a。测定该单面覆铜产品a的铜箔层和聚酰亚胺树脂层之间的180°剥离强度(JIS C-5016)，结果为0.8kg/cm，蚀刻后薄膜的线膨胀系数为23.5×10-6(1/℃)。
(实施例1)
在分别经由氮气气氛下的导辊，将制造例调制的单面绝缘体层的覆铜产品的宽度500mm的辊卷绕片材的树脂面与相同宽度尺寸的35μm的辊卷绕片材即轧制铜箔的粗糙化表面导入一对热压辊(外径300mm，宽800mm，在表面附近埋入封入萘的夹套式加热管作为均匀加热装置，在内部的中心轴上内置介电加热线圈的结构)之间之前，由加热装置内置型的导辊3′(4′)预加热，然后在热压辊表面温度360～390℃、压辊间的线压150～170kg/cm、通过时间2～5秒的范围内进行热压。此时，对相同的基材材料、相同的热压辊条件下没有预加热的场合和将预加热温度改变到150℃、250℃和340℃的场合，通过目视调查得到的双面覆铜产品的表面状态，在表1中示出结果。
                     表1
  预加热温度(℃)   两面覆铜产品的表面状态
  没有预加热   差(产生许多纵向条纹、横向皱褶)
  150   差(产生皱褶)
  250   外观良好(没有皱褶)
  340   外观良好(没有皱褶)
(实施例2)
在上述实施例1中，对于设定为热压辊表面的设定温度360℃、压辊间的线压150kg/cm、通过时间3秒，而且导入到热压辊之间的基材没有预加热的场合，和使预加热温度为250℃和340℃的场合，通过目视调查使热压辊的表面粗糙度(Ra)变化为小于等于0.01、0.05、0.20、10.0μm这4段的场合得到的两面覆铜产品的表面状态，在表2中示出结果。
                              表2
温度(℃)     Ra(μm)     两面覆铜产品的表面状态
没有预加热     小于等于0.01     差(产生皱折引起的皱褶和凹痕)
    0.05     差(产生许多纵向条纹和横向皱褶)
    0.20     差(产生许多纵向条纹和横向皱褶)
    10.0     产生凹凸
250     小于等于0.01     差(产生皱折引起的皱褶和凹痕)
    0.05     外观良好
    0.20     外观良好
    10.0     产生凹凸
340     小于等于0.01     差(产生皱折引起的皱褶和凹痕)
    0.05     外观良好
    0.20     外观良好
    10.0     产生凹凸
本发明的两面导体聚酰亚胺积层体的制造方法是能够在辊卷绕状态下连续制造不存在纵皱褶等外观缺陷、质量稳定的两面导体聚酰亚胺类积层体，产业上的可利用性高的制造方法。

Claims (5)

1.一种两面导体聚酰亚胺积层体的连续制造方法，将在导电性金属箔(M1)上具有底层、中间主层、顶层至少三层聚酰亚胺类树脂层的单面导体积层体和包括导电性金属箔(M2)的基材连续导入到一对热压辊之间，在上述顶层上通过热压使导电性金属箔(M2)积层一体化，其特征在于：将导入热压辊间之前的单面导体积层体和导电性金属箔(M2)分别在惰性气体气氛下预加热到大于等于200℃～小于等于项层的聚酰亚胺类树脂的玻璃化转变温度，然后使它们与热压辊表面接触。
2.权利要求1所述的两面导体聚酰亚胺积层体的连续制造方法，其中，将上述一对热压辊的平均表面粗糙度(Ra)表面粗糙化处理到0.01～5μm，并且在使其表面温度为340～390℃、压辊间的线压为50Kg/cm～300Kg/cm、通过时间为2～5秒的条件下进行热压。
3.权利要求1或2所述的两面导体聚酰亚胺积层体的连续制造方法，其中，将上述单面导体积层体和导电性金属箔(M2)从辊卷绕状态拉出，经过中心轴高度各不相同的多个导辊，在平面性提高的状态下进行预加热。
4.权利要求1～3的任一项所述的两面导体聚酰亚胺积层体的连续制造方法，其中，上述预加热由内置加热装置的导辊进行。
5.权利要求2所述的两面导体聚酰亚胺积层体的连续制造方法，其中，在上述辊表面上热喷涂陶瓷被膜以形成表面粗糙度(Ra)。
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