CN108778736B - 芳族聚酰胺纸与聚酰亚胺膜的层合体及其制造方法 - Google Patents

芳族聚酰胺纸与聚酰亚胺膜的层合体及其制造方法 Download PDF

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CN108778736B
CN108778736B CN201780017607.2A CN201780017607A CN108778736B CN 108778736 B CN108778736 B CN 108778736B CN 201780017607 A CN201780017607 A CN 201780017607A CN 108778736 B CN108778736 B CN 108778736B
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polyimide film
laminate
aramid paper
aramid
paper
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CN108778736A (zh
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浮谷孝一
藤森龙士
成濑新二
近藤千寻
田中康纪
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DuPont Teijin Advanced Papers Japan Ltd
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DuPont Teijin Advanced Papers Japan 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • 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
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/10—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of paper or cardboard
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
    • 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
    • B32B29/00—Layered products comprising a layer of paper or cardboard
    • B32B29/002—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B29/005—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material next to another layer of paper or cardboard layer
    • 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
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • 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
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
    • 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
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • 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
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/10—Organic non-cellulose fibres
    • D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/26—Polyamides; Polyimides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
    • D21H25/04—Physical treatment, e.g. heating, irradiating
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/30—Multi-ply
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
    • B29C65/18—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using heated tools
    • 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
    • B29C65/44—Joining a heated non plastics element to a plastics element
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • 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
    • B29C66/112—Single lapped joints
    • B29C66/1122—Single lap to lap joints, i.e. overlap joints
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • 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
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    • B29C66/45—Joining of substantially the whole surface of the articles
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Abstract

提供层合体的制造方法，其包含通过在温度275~320℃、压力50~400kgf/cm的条件下的加热加压加工来层合芳族聚酰胺纸与聚酰亚胺膜。根据本发明，将芳族聚酰胺纸与聚酰亚胺膜利用简便的手法、且在不损及两者特性的情况下层合，可以制造耐热性、电特性、耐化学性、机械特性等优异的芳族聚酰胺纸‑聚酰亚胺膜层合体。

Description

芳族聚酰胺纸与聚酰亚胺膜的层合体及其制造方法
技术领域
本发明涉及耐热性、电特性(电绝缘特性)、耐化学性、机械特性等优异的芳族聚酰胺纸-聚酰亚胺膜层合体及其制造方法，特别是涉及作为旋转装置、变压器和电气、电子设备的绝缘材料有用的芳族聚酰胺纸-聚酰亚胺膜层合体及其制造方法。
背景技术
以往，在要求耐热性的电绝缘领域中，使用以耐热性高分子作为原材料的成形体。特别是使用芳香族聚酰胺(以下称为芳族聚酰胺，aramid)的成形品，其是具备来源于芳族聚酰胺分子结构的耐热性、耐化学性、阻燃性的优异的工业材料。其中，由聚间苯二甲酰间苯二胺的纤条体和纤维所构成的纸(商品名称NOMEX纸(注册商标))，被广泛用作耐热性优异的电绝缘纸。
另外，前述成形品与材质不同的树脂膜等片材层合而成的层合体，也同样地被广泛用于电绝缘用途。这样的层合体，通过将不同材质的片材层合，可以将各片材所具有的特性有效利用于作为层合体的特性。例如将耐热性较高的材料配置于与热源相接的层合体的表层，由此可提高层合体整体的耐热性。
专利文献1公开了：在层合片材时，对粘接面进行等离子体处理，将各种树脂片与芳族聚酰胺纸层合的手法。然而，等离子体处理需要专用的处理装置，且不适合对大型片进行连续处理。
现有技术文献
专利文献
专利文献1：日本特开2013-223962号公报。
发明内容
本发明的目的是提供耐热性、电特性、耐化学性、机械特性等优异的芳族聚酰胺纸-聚酰亚胺膜层合体及其制造方法，其将芳族聚酰胺纸与聚酰亚胺膜利用简便的手法、且在不损及两者特性的情况下层合。
本发明是根据将芳族聚酰胺纸与聚酰亚胺膜在特定温度且特定压力下进行加热加压加工而使其层合，由此可以解决上述课题的见解而完成的。即，本发明包含下述方案。
1. 层合体的制造方法，其特征在于：通过在温度275~320℃、压力50~400kgf/cm的条件下的加热加压加工来层合芳族聚酰胺纸与聚酰亚胺膜。
2. 上述1所述的层合体的制造方法，其中，加热加压加工使用砑光辊来进行。
3. 上述1或2所述的层合体的制造方法，其中，将以2层聚酰亚胺膜夹持1层芳族聚酰胺纸而得的预层合片进行加热加压加工，由此形成具有聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层结构的层合体。
4. 上述1或2所述的层合体的制造方法，其中，将1层芳族聚酰胺纸与1层聚酰亚胺膜层合而得的预层合片进行加热加压加工，由此形成具有聚酰亚胺膜-芳族聚酰胺纸的二层结构的层合体。
5. 上述1~4中任一项所述的层合体的制造方法，其中，将前述芳族聚酰胺纸与前述聚酰亚胺膜未隔着粘接层，而直接进行层合。
6. 上述1~5中任一项所述的层合体的制造方法，其中，在加热加压加工前，不对芳族聚酰胺纸和聚酰亚胺膜的粘接面实施等离子体处理。
7. 上述1~6中任一项所述的层合体的制造方法，其中，前述芳族聚酰胺纸的厚度为20~1000μm，前述聚酰亚胺膜的厚度为3~200μm。
8. 上述1~7中任一项所述的层合体的制造方法，其中，前述层合体的厚度为20~1500μm。
9. 层合体，其是通过将芳族聚酰胺纸与聚酰亚胺膜在温度275~320℃、压力50~400kgf/cm的条件下进行加热加压加工而形成的层合体。
10. 上述9所述的层合体，其具有聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层结构。
11. 上述9所述的层合体，其具有聚酰亚胺膜-芳族聚酰胺纸的二层结构。
具体实施方式
(芳族聚酰胺)
本发明中，芳族聚酰胺是指酰胺键的60%以上与芳香环直接键合的线状高分子化合物。作为这样的芳族聚酰胺，例如可举出：聚间苯二甲酰间苯二胺及其共聚物、聚对苯二甲酰对苯二胺及其共聚物、共聚对亚苯基·3,4’-二苯基醚对苯二甲酰胺等。
这些芳族聚酰胺，通过例如利用芳香族酸二氯化物与芳香族二胺的缩合反应所进行的溶液聚合法、两阶段界面聚合法等进行工业性地制造，可以作为市售品获取，但并不限定于此。这些芳族聚酰胺之中，聚间苯二甲酰间苯二胺具备良好的成型加工性、阻燃性、耐热性等特性，在该方面优选。
(芳族聚酰胺纤条体)
本发明中，芳族聚酰胺纤条体是由芳族聚酰胺构成的膜状微小粒子，有时也称为芳族聚酰胺浆粕。关于制造方法，例如可例示：日本特公昭35-11851号、日本特公昭37-5732号公报等中记载的方法。关于芳族聚酰胺纤条体，因为与通常的木材浆粕相同地具有造纸性，因此在水中分散之后，可以在造纸机中成形为片状。该情况下，基于保持适用于造纸的品质的目的，可以实施所谓的打浆处理。可以通过盘式磨浆机、打浆机、其他带来机械切割作用的造纸原料处理设备，来实施该打浆处理。该操作中，可通过JIS P8121所规定的滤水度(游离度)监测纤条体的形态变化。
本发明中，实施打浆处理之后的芳族聚酰胺纤条体的滤水度，优选处于10~300cm3(加拿大标准游离度)的范围内。通过将滤水度控制在300cm3以下，可提高其后成形的片的强度。通过使滤水度为10cm3以上，可以提高所投入的机械动力的利用效率，并可以提高每单位时间的处理量。而且，可实现纤条体适度的微细化，从而可抑制粘合剂功能的降低。
(芳族聚酰胺短纤维)
本发明中，芳族聚酰胺短纤维是指将以芳族聚酰胺为原料的纤维裁切为规定的长度所得物，作为这样的纤维，例如可以例示：杜邦公司的“NOMEX(注册商标)”，“KEVLAR (注册商标)”，帝人(株)的“CONEX(注册商标)”，“TECHNORA(注册商标)”等，但并不限于这些。
芳族聚酰胺短纤维可以具有优选0.05dtex以上且不足25dtex的范围内的纤度。纤度为0.05dtex以上的纤维，在通过湿式法的制造(后述)中，不易发生凝集，另外，纤度不足25dtex的纤维，纤维直径成为适当的大小。例如，正圆形状下将密度设为1.4g/cm时，在直径为45微米以上的情况下，可能产生纵横比降低、力学的补强效果降低、芳族聚酰胺纸的均匀性不良。
芳族聚酰胺短纤维的长度优选选自1mm以上且不足25mm的范围。短纤维的长度若为1mm以上，则芳族聚酰胺纸的力学特性变得充分，若不足25mm，则可以抑制后述的通过湿式法制造芳族聚酰胺纸时发生“交缠”、“结成束”等。
(芳族聚酰胺纸)
本发明中，芳族聚酰胺纸是指以前述芳族聚酰胺纤条体和芳族聚酰胺短纤维为主所构成的片状物，通常具有20μm~1000μm的厚度，优选具有70μm~800μm的厚度，更优选具有300μm~600μm的厚度。
而且，芳族聚酰胺纸通常具有10g/m2~1000g/m2的单位面积重量，优选具有30g/m2~400g/m2的单位面积重量，更优选具有50g/m2~200g/m2的单位面积重量，进一步优选具有80g/m2~180g/m2的单位面积重量。在此，芳族聚酰胺纤条体与芳族聚酰胺短纤维的混合比例可以为任意比例，不过优选使芳族聚酰胺纤条体/芳族聚酰胺短纤维的比例(质量比)为1/9~9/1，更优选为2/8~8/2，但并不限定于该范围。
芳族聚酰胺纸的玻璃化转变温度没有特别限定，通常为255~275℃，优选为260~270℃。
本申请中，玻璃化转变温度是指：将试验片从室温以3℃/分钟的比例进行升温，通过差示扫描量热计测定发热量，从吸热曲线引出2条延长线，从延长线间的1/2直线与吸热曲线的交点所求得的值。可使用差示扫描量热计作为玻璃化转变温度的测定装置。
芳族聚酰胺纸通常可通过将前述的芳族聚酰胺纤条体与芳族聚酰胺短纤维混合之后进行片化的方法来制造。具体而言，例如可以适用：将上述芳族聚酰胺纤条体和芳族聚酰胺短纤维进行干式混合之后，利用气流形成片的方法；将芳族聚酰胺纤条体和芳族聚酰胺短纤维在液体介质中分散混合之后，排出至液体透过性的支撑体、例如网或带上来进行片化，并去除液体而干燥的方法等；但这些之中，优选选择将水用作介质的所谓的湿式造纸法。
在湿式造纸法中，通常的方法如下：将至少含有芳族聚酰胺纤条体、芳族聚酰胺短纤维的单一或混合物的水性浆料送液至造纸机并分散之后，通过脱水、榨水和干燥，而作为片进行卷取的方法。作为造纸机，可利用长网造纸机、圆网造纸机、倾斜型造纸机和将这些组合的联合造纸机等。在以联合造纸机制造的情况下，通过使掺混比例不同的浆料成形为片并合而为一，可以得到由多个纸层构成的复合体片。造纸时，根据需要，可使用分散性改善剂、消泡剂、纸力增强剂等的添加剂。
(砑光加工)
如上所得的芳族聚酰胺纸，通过在一对辊间以高温高压进行加热加压加工，可以提升密度、机械强度。关于加热加压加工的条件，例如，使用金属制辊时，可以例示275℃~320℃的温度、50~400kg/cm的线压，但并不限于这些。热压时还可以将多个芳族聚酰胺纸层合。
(聚酰亚胺膜)
聚酰亚胺膜由于横跨从极低温区域到高温区域的宽温度范围发挥优异的机械、电、化学特性，因此被广泛用于部件安装用挠性电路基板的补强材(stiffener)或电绝缘材料。聚酰亚胺膜的厚度，通常而言为3μm~200μm，优选为5μm~150μm，更优选为10μm~25μm。作为这样的聚酰亚胺膜，可以例示东丽杜邦(株)的Kapton(注册商标)，但并不限定于此。
而且，作为聚酰亚胺膜，优选具有3g/m2~300g/m2的单位面积重量，更优选具有4g/m2~150g/m2的单位面积重量，进一步优选具有5g/m2~50g/m2的单位面积重量为宜。
(芳族聚酰胺纸-聚酰亚胺膜层合体)
通过将前述的芳族聚酰胺纸与聚酰亚胺膜进行加热加压加工，制造芳族聚酰胺纸-聚酰亚胺膜层合体。芳族聚酰胺纸-聚酰亚胺膜层合体是指，将芳族聚酰胺纸与聚酰亚胺膜层合而得的、形成至少2层以上的层结构的层合体。层合体的厚度没有特别限定，但优选为20μm~1500μm，更优选为50μm~800μm，进一步优选为200μm~400μm。厚度可根据用途进行选择。
而且，作为芳族聚酰胺纸-聚酰亚胺膜层合体，优选具有10g/m2~2000g/m2的单位面积重量，更优选具有30g/m2~700g/m2的单位面积重量，进一步优选具有80g/m2~400g/m2的单位面积重量。
芳族聚酰胺纸和聚酰亚胺膜的尺寸没有特别限定。可考虑层合体被使用的用途、生产成本、既有设备等的各种主要因素，来确定所使用的尺寸。从生产率的观点出发，准备辊状的芳族聚酰胺纸和聚酰亚胺膜，通过连续的加热加压加工来制造层合体。在试制品的制造或特订品的制造中，使用小尺寸的芳族聚酰胺纸和聚酰亚胺膜较为简便。
加热加压加工是指，对层合体施加热和压力两者的加工处理。实施加热加压加工的装置没有特别限定，但在一个实施方案中，使用砑光装置。砑光装置是指，在产业界中被广泛使用的、将多条砑光辊组合而成的装置，其是将片状对象物通过辊间，由此施加压缩力的装置。通过使对象物通过砑光辊，对象物可高密度化或改善平滑度。根据施加于对象物的压力或温度条件，可从钢辊、弹性辊等选择具有适当材质和尺寸的辊。砑光辊的构成也无特别限制。使多个片状的对象物通过砑光辊，由此可制造将不同材料层合而成的层合体。可根据要层合的片尺寸，选择适当的砑光装置。例如，在要被叠合的芳族聚酰胺纸和聚酰亚胺膜为长条的卷状的情况下，可以使用具备2辊以上的送纸功能的砑光装置。
一个实施方案中，芳族聚酰胺纸与聚酰亚胺膜未隔着粘接层，而直接层合。通过设为这样的形态，可降低制造成本，且可提升生产率。本发明中，可制造无粘接层但具有充分粘接性的层合体。
一个实施方案中，关于芳族聚酰胺纸与聚酰亚胺膜，在加热加压加工前，未对芳族聚酰胺纸和聚酰亚胺膜的粘接面实施等离子体处理。通过实施等离子体处理可改善粘接性，但本发明中可制造不经等离子体处理而具有充分粘接性的层合体。通过采用不经等离子体处理而制造层合体的工艺，可降低制造成本，而且提升生产率。
使加热加压加工时的温度为构成层合体的芳族聚酰胺纸的玻璃化转变温度以上的温度。需说明的是，在2片以上的芳族聚酰胺纸被层合的情况下，以与聚酰亚胺膜相接的芳族聚酰胺纸的玻璃化转变温度为本发明中的玻璃化转变温度。使用砑光辊实施加热加压加工的情况下，使砑光辊的温度为构成层合体的芳族聚酰胺纸的玻璃化转变温度以上。
本发明中，作为加热加压加工时的温度，必须采用275~320℃的温度范围。作为该温度，优选为280~315℃，进一步优选为285~310℃。加热加压加工时的温度通常可经由所使用的装置的控制机构进行调整。例如，砑光辊等的加热加压装置的温度，可作为砑光辊的设定温度得到控制。
本发明中，除了采用上述特定的温度以外，必须采用50~400kgf/cm的压力范围作为加热加压加工时的压力。作为该温度，优选为75~350kgf/cm、更优选为100~350kgf/cm、进一步优选为150~330kgf/cm。加热加压加工时的压力通常可经由所使用的装置的控制机构进行调整。例如，砑光辊等的加热加压装置的压力通常可经由装置的控制机构来控制。
本发明中，通过加热加压加工形成芳族聚酰胺纸与聚酰亚胺膜的层合体时，可同时进行上述芳族聚酰胺纸的高密度化。因此，根据情况，可在芳族聚酰胺纸的制造中简化或省略砑光加工，此情况下，可更进一步谋求工艺效率的提升。
在一个实施方案中，层合体是具有聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层结构的层合体。该层合体可通过如下制造：形成以2层聚酰亚胺膜夹持1层芳族聚酰胺纸而得的预层合片，并对预层合片进行加热加压加工。
以聚酰亚胺膜夹持芳族聚酰胺纸的层合体的优点是在厚度方向上的均匀性和尺寸稳定性。另外，由于在两侧配置有耐热性高的聚酰亚胺，因此成为高耐热性的层合体。作为有效利用这种特性的用途，例如可举出：片两面与高温部位相接那样的耐热间隔物、或要求焊接耐热性的挠性电路基板的补强材。
在另一实施方案中，层合体是具有聚酰亚胺膜-芳族聚酰胺纸的二层结构的层合体。该层合体可通过如下制造：形成1层芳族聚酰胺纸与1层聚酰亚胺膜层合而得的预层合片，并对预层合片进行加热加压加工。
在1层芳族聚酰胺纸与1层聚酰亚胺膜层合而得的层合体中，芳族聚酰胺纸露出于一侧的表面，而聚酰亚胺膜露出于另一侧的表面。这种层合体的优点在于将聚酰亚胺膜的高绝缘性赋予芳族聚酰胺纸的方面，适合于例如单一的芳族聚酰胺纸无法确保绝缘性的绝缘用途。
实施例
以下，根据实施例更具体地说明本发明。需说明的是，这些实施例仅为例示，并不用于对本发明的内容作任何限定。
[实施例1]
(原料调制)
使用日本特开昭52-15621号公报记载的定子与转子的组合所构成的浆粕粒子制造装置(湿式沉淀机)，制造了聚间苯二甲酰间苯二胺的纤条体。将其在解磨机、打浆机中进行处理，以将长度加权平均纤维长度调整为0.9mm。另一方面，将杜邦公司制间位芳族聚酰胺纤维(meta-aramid fiber，NOMEX(注册商标)，单丝纤度2.2dtex)裁切为长度6mm，作为造纸用原料。
(芳族聚酰胺纸的制造)
将如上调制的芳族聚酰胺纤条体与芳族聚酰胺短纤维各自分散于水中，制作了浆料。将这些浆料混合，使芳族聚酰胺纤条体与芳族聚酰胺短纤维成为1/1的混合比率(重量比)，之后送液至长网造纸机(FOURDRINIER)型造纸机，进行脱水、榨水、干燥并卷取，得到了芳族聚酰胺纸。
(芳族聚酰胺纸-聚酰亚胺膜层合体的制造)
将通过上述方法制造的芳族聚酰胺纸(DuPont Teijin Advanced Papers(株)制“NOMEX(注册商标)纸型号411、标称厚度15mil、玻璃化转变温度275℃”)和聚酰亚胺膜(东丽杜邦(株)制“Kapton(注册商标)50H”、玻璃化转变温度=300℃)分别裁切为A4尺寸并叠合，准备了预层合体。通过具有金属制砑光辊的砑光装置，在温度设定300℃，线压设定300kgf/cm下，对该预层合体进行加热加压加工，得到了芳族聚酰胺纸-聚酰亚胺膜的二层层合体。
将利用下述方法评价由此所得的层合体的主要特性的结果示于表1中。
[测定方法]
(1) 单位面积重量、厚度、密度
依照JIS C 2323-2实施，通过(单位面积重量/厚度)算出密度。
(2) 外观
观察层合体的外观，将表面平滑且均匀者判断为“良好”，将产生气泡或明显可见凹凸者判断为“不良”。
(3) 粘接性
将芳族聚酰胺纸与聚酰亚胺膜粘接者判断为“良好”，将未粘接者判断为“不良”。
[实施例2]
将通过实施1所得的芳族聚酰胺纸和2片聚酰亚胺膜分别裁切为A4尺寸，并以2片聚酰亚胺膜夹持芳族聚酰胺纸的形态进行叠合，准备了预层合体。通过具有金属制砑光辊的砑光装置，在温度设定300℃、线压设定300kgf/cm下，对该预层合体进行加热加压加工，得到了聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层层合体。与实施例1同样地评价了由此所得的绝缘构件的主要特性值。将结果示于表1中。
[比较例1]
将通过实施1所得的芳族聚酰胺纸和聚酰亚胺膜分别裁切为A4尺寸，并进行叠合，准备了预层合体。通过具有金属制砑光辊的砑光装置，在温度设定250℃、线压设定300kgf/cm下，对该预层合体进行加热加压加工，得到了芳族聚酰胺纸-聚酰亚胺膜的二层层合体。与实施例1同样地评价了由此所得的绝缘构件的主要特性值，将结果示于表1中。
[比较例2]
将通过实施1所得的芳族聚酰胺纸和聚酰亚胺膜分别裁切为A4尺寸，并进行叠合，准备了预层合体。通过具有金属制砑光辊的砑光装置，在温度设定330℃、线压设定300kgf/cm下，对该预层合体进行加热加压加工，得到了芳族聚酰胺纸-聚酰亚胺膜的二层层合体。与实施例1同样地评价了由此所得的绝缘构件的主要特性值，将结果示于表1中。
表1
Figure DEST_PATH_IMAGE002
如表1所示，判明了：通过在加热加压加工时选择芳族聚酰胺纸的玻璃化转变温度以上的适当温度，可得到粘接性、外观均良好的芳族聚酰胺纸-聚酰亚胺膜层合体。另一方面，加热加压加工的温度在250℃以下的情况下，确认产生来源于芳族聚酰胺纸所含的水分的气泡，加热加压加工的温度为330℃以上的情况下，确认由于芳族聚酰胺纸与聚酰亚胺膜的热收缩率的差异而产生贴合皱纹，因此芳族聚酰胺纸-聚酰亚胺膜间的粘接并不充分。
根据上述结果判明了：如实施例1和2所例示，作为挠性电路基板的补强材或绝缘材料有用的耐热性、电特性、机械特性等优异的芳族聚酰胺纸-聚酰亚胺膜层合体，使用在芳族聚酰胺纸的玻璃化转变温度即275℃以上、且芳族聚酰胺纸不会发生过度热收缩的320℃以下的温度实施加热加压加工所得的芳族聚酰胺纸-聚酰亚胺膜层合体是有效的。

Claims (10)

1.层合体的制造方法，其特征在于：通过使用砑光辊在温度275~320℃、压力50~400kgf/cm的条件下的加热加压加工来层合芳族聚酰胺纸与聚酰亚胺膜。
2.权利要求1所述的层合体的制造方法，其中，将以2层聚酰亚胺膜夹持1层芳族聚酰胺纸而得的预层合片进行加热加压加工，由此形成具有聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层结构的层合体。
3.权利要求1所述的层合体的制造方法，其中，将1层芳族聚酰胺纸与1层聚酰亚胺膜层合而得的预层合片进行加热加压加工，由此形成具有聚酰亚胺膜-芳族聚酰胺纸的二层结构的层合体。
4.权利要求1~3中任一项所述的层合体的制造方法，其中，将前述芳族聚酰胺纸与前述聚酰亚胺膜未隔着粘接层，而直接进行层合。
5.权利要求1~3中任一项所述的层合体的制造方法，其中，在加热加压加工前，不对芳族聚酰胺纸和聚酰亚胺膜的粘接面实施等离子体处理。
6.权利要求1~3中任一项所述的层合体的制造方法，其中，前述芳族聚酰胺纸的厚度为20~1000μm，前述聚酰亚胺膜的厚度为3~200μm。
7.权利要求1~3中任一项所述的层合体的制造方法，其中，前述层合体的厚度为20~1500μm。
8.层合体，其是通过将芳族聚酰胺纸与聚酰亚胺膜使用砑光辊在温度275~320℃、压力50~400kgf/cm的条件下进行加热加压加工而形成的层合体。
9.权利要求8所述的层合体，其具有聚酰亚胺膜-芳族聚酰胺纸-聚酰亚胺膜的三层结构。
10.权利要求8所述的层合体，其具有聚酰亚胺膜-芳族聚酰胺纸的二层结构。
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TW201801894A (zh) 2018-01-16
JP6722480B2 (ja) 2020-07-15
KR102603103B1 (ko) 2023-11-20
KR20180121912A (ko) 2018-11-09
US10836112B2 (en) 2020-11-17
WO2017159131A1 (ja) 2017-09-21
CN108778736A (zh) 2018-11-09
US20190061270A1 (en) 2019-02-28

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