CN102189733B - 层压复合物及其制造方法 - Google Patents

层压复合物及其制造方法 Download PDF

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Publication number
CN102189733B
CN102189733B CN201110024020.9A CN201110024020A CN102189733B CN 102189733 B CN102189733 B CN 102189733B CN 201110024020 A CN201110024020 A CN 201110024020A CN 102189733 B CN102189733 B CN 102189733B
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fiber
face shield
nano
laminated composites
graphite plate
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CN201110024020.9A
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CN102189733A (zh
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C.夸
C-S.王
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GM Global Technology Operations LLC
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GM Global Technology Operations LLC
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
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Abstract

本发明涉及层压复合物及其制造方法。层压复合物包括多个堆叠预浸料体，所述预浸料体具有在每对相邻的预浸料体之间形成的界面。每个预浸料体包括基体材料和散置在其中的增强纤维。至少一个纤维面罩被层压到所述界面中的至少一个的至少一部分上，所述至少一个纤维面罩具有附连到其至少一个表面上的石墨纳米板。

Description

层压复合物及其制造方法
相关申请的交叉引用
本申请是于2008年12月2日提交的、题为“Laminated Composites and Methods of Making the Same”的同在审查中的美国专利申请序列号12/326362的部分延续，上述申请的公开内容在此作为参考全文引入。
技术领域
本发明总体上涉及层压复合物及其制造方法，且更具体地涉及制造成具有预浸料体和纤维面罩的层压复合物，所述纤维面罩上附连有石墨纳米板（nano-platelet）。
背景技术
用碳纤维环氧树脂预浸料体制成的层压复合物已经用于许多应用。这种层压复合物的增强碰撞属性对于某些机动车和工程应用来说可能是特别期望的。改进层压复合物的碰撞属性的努力包括改变基体树脂属性或层压结构。前者主要通过使用合适的韧化材料韧化预浸料体树脂系统完成。后者通过使用较小尺度纤维在层之间引入各种界面来尝试。
发明内容
本发明涉及层压复合物及其制造方法。层压复合物包括多个堆叠预浸料体，所述预浸料体具有在每对相邻的预浸料体之间形成的界面。每个预浸料体包括基体材料和散置在其中的增强纤维。至少一个纤维面罩被层压到所述界面中的至少一个的至少一部分上，所述至少一个纤维面罩具有附连到其至少一个表面上的石墨纳米板。
方案1. 一种层压复合物，包括：
多个堆叠预浸料体，所述预浸料体具有在每对相邻的预浸料体之间形成的界面，每个预浸料体包括基体材料和散置在其中的增强纤维；和
至少一个纤维面罩，所述至少一个纤维面罩被层压到所述界面中的至少一个的至少一部分上，所述至少一个纤维面罩具有附连到其至少一个表面上的石墨纳米板。
方案2. 根据方案1所述的层压复合物，其中，具有附连到其上的石墨纳米板的所述至少一个纤维面罩给复合物增加预定厚度。
方案3. 根据方案2所述的层压复合物，其中，所述预定厚度在从大约0.01 mm至大约0.1 mm的范围内。
方案4. 根据方案1所述的层压复合物，其中，石墨纳米板是片状石墨纳米板。
方案5. 根据方案1所述的层压复合物，其中，增强纤维是碳纤维，基体材料是树脂，其中，预浸料体中的每个包括至多35％重量的树脂和至少65％重量的碳纤维，其中，碳纤维选自包括12K碳纤维、24K碳纤维及其组合物的组。
方案6. 根据方案1所述的层压复合物，其中，所述至少一个纤维面罩是玻璃纤维面罩。
方案7. 根据方案1所述的层压复合物，其中，在层压复合物中石墨纳米板的量小于层压复合物的总wt％的2.5wt％。
方案8. 根据方案1所述的层压复合物，其中，所述层压复合物展现了最大负荷、能量-最大负荷以及穿孔能量中的至少一个的增加。
方案9. 根据方案1所述的层压复合物，其中，i）多个预浸料体和ii）至少一个纤维面罩中的每个都包括纤维，其中，这些纤维的平均直径范围从大约7000 nm至大约9000 nm。
方案10. 根据方案1所述的层压复合物，其中，所述多个预浸料体中的每个包括：i）选自碳纤维、玻璃纤维、硼纤维和聚合物纤维的纤维；ii）选自单向结构、编织织物和多个轴向织物的结构；以及iii）选自环氧树脂、酚醛树脂、聚酯树脂、乙烯基酯树脂、 聚酰亚胺树脂、热塑性树脂的树脂。
方案11. 一种制造抗碰撞层压复合物的方法，所述方法包括：
用石墨纳米板涂布至少一个纤维面罩的表面；
将所述至少一个纤维面罩层压到多个预浸料体之间的界面的至少一部分上，每个预浸料体包括在基体材料中的增强纤维；和
将层压的多个预浸料体和至少一个纤维面罩模制成复合物。
方案12. 根据方案11所述的方法，其中，增强纤维是碳纤维，基体材料是树脂，其中，预浸料体中的每个包括至多35％重量的树脂和至少65％重量的碳纤维，其中，碳纤维选自包括12K碳纤维、24K碳纤维及其组合物的组。
方案13. 根据方案11所述的方法，其中，石墨纳米板是片状石墨纳米板。
方案14. 根据方案11所述的方法，其中，用石墨纳米板涂布至少一个纤维面罩的表面通过以下步骤完成：
将所述至少一个纤维面罩浸渍在含有分散在其中的石墨纳米板的溶液中；以及
干燥具有附连到其上的石墨纳米板的所述至少一个纤维面罩。
方案15. 根据方案14所述的方法，其中，所述溶液包括异丙基醇、分散剂、以及胶状纳米二氧化硅和异丙醇的混合物。
方案16. 一种纤维面罩，包括：
基体，所述基体包括多个纤维，所述多个纤维中的每个的平均直径在从大约7000 nm至大约9000 nm的范围内；和
石墨纳米板，所述石墨纳米板在没有聚合物粘结剂的情况下附连到所述多个纤维中的至少一些上。
附图说明
本发明的特征和优点将通过参照下面的详细描述和附图变得显而易见。
图1A、1B和1C是示出了以下步骤的一系列示意图：分散片状石墨纳米板（xGnP）（在图1A中标记为“xGnP分散”）、用片状石墨纳米板涂布面罩（在图1B中标记为“xGnP涂布”）、以及执行层压模制（在图1C中标记为“层压模制”）；
图2是示出了来自于本文公开的层压复合物的样品和多个对比样品（即，没有面罩和未涂布面罩）的负荷（kN）对比位移（mm）的对比碰撞负荷-位移曲线的曲线图；和
图3是示出了来自于本文公开的层压复合物的样品和包括碳纳米纤维涂布面罩的对比样品的负荷（kN）对比位移（mm）的对比碰撞负荷-位移曲线的曲线图。
具体实施方式
在与其他已知层压复合物相比时，本文公开的层压复合物展现了优良的碰撞属性。本文公开的示例的复合物包括有策略地设置在多个预浸料体层之间的界面处的少量石墨纳米板。这些少量石墨纳米板附连到薄纤维面罩上，其用作纳米板的载体。因而，石墨纳米板不添加到最终复合物中存在的所有纤维（例如，预浸料体纤维）上，而是添加到位于预浸料体层之间的界面处的纤维面罩上。石墨纳米板涂布的纤维面罩有利地增加碰撞属性且增强得到的复合物的弱界面，而不显著增加复合物的重量或体积（例如，厚度）或者增加制造成本。
如本文使用的，术语“预浸料体”是基体树脂和纤维增强物的组合，以便用于在热和压力下的本文公开的制造工艺。在一个示例中，预浸料体纤维已经用预催化基体树脂浸渍且部分固化（B级）。“层叠”指的是将预浸料体（已经用树脂预先浸渍）铺放到模具外侧或者有时直接铺放到模具上的工艺。应当理解的是，在本文公开的方法中，层叠工艺也包括将石墨纳米板涂布的面罩（下文进一步讨论）铺放在预浸料体之间。
在制备本文公开的层压复合物时，在层叠工艺期间，发生纳米板涂布的面罩层压到预浸料体上。该技术的一个益处在于不需要现有预浸料体的任何化学或物理改性。改性商业预浸料体通常是困难和昂贵的，至少部分因为这些材料在其固化速率、粘度-温度性能和处理特性方面精密平衡。应当理解的是，制造本文公开的层压复合物的方法可以与任何预浸料体一起使用。因为其需要常规预浸料体和/或层叠工艺的细微（如果有的话）的变化，因而该技术被认为是便于实施的。
与将纳米纤维结合到整个预浸料体树脂基体中的常规方法相比，本文公开的方法的另一个益处在于其使用显著更少量的石墨纳米板。例如，在文献（参见Quaresimin et al., “Understanding the effect of nano-modifier addition upon the properties of fibre reinforced laminates,” Composites Science and Technology, Volume 68, Issues 3-4, March 2008, Pages 718-726中的图12）中已知的先前研究报道了通过将7.5 wt％的碳纳米纤维（CNF）添加到预浸料体本身而引起碰撞能量的20％改进。本发明的技术用少于3 wt％的片状石墨纳米板产生超过20％的改进，而不用将片状石墨纳米板结合到预浸料体成分中，如下文示例中的表1所示。
本文公开的方法的又一个益处在于由本文公开的工艺引起的从层压复合物模制的部件的厚度和重量的任何增加是微小的且可能是可忽略的。例如，通过包括已涂布面罩，模制复合物的厚度可以增加大约0.01 mm至大约0.1 mm。因而，本文公开的方法能在不改变现有部件设计和制造工具及工艺的情况下应用。通过使用较轻重量的碳纤维面罩，最终部件的重量增加还可进一步最小化。
通常，如图1A所示，方法通过将少量的合适片状石墨纳米板分散到期望溶剂或溶液中开始。片状石墨纳米板（xGnP）是由石墨制成的纳米颗粒。xGnP的尺寸由沿横向尺寸测量的平均板直径表示，例如1、5、10、15、25微米等。颗粒尺寸分布通常符合具有大约±35％标准偏差的正态分布。在一些情况下，纳米颗粒包括厚1 nm至15 nm且直径在亚微米至100微米范围内的小堆石墨烯。在一个非限制性示例中，石墨纳米板的平均直径在约5微米至约15微米的范围内。在一些实施例中，还可以使用不同尺寸的石墨纳米板的混合物（例如，1：1重量比的5微米xGnP和15微米xGnP）。可以理解的是，至少部分由于尺寸分布，混合物可能更容易分散在选定溶剂中。
通常，石墨纳米板的量被选择使得石墨纳米板分散实现期望溶液且使得得到的溶液利于石墨纳米板大致均匀地分布到纤维面罩上。此外，应当理解的是，至少部分取决于碰撞属性的期望增强水平，所使用的石墨纳米板的量可以变化。在一个实施例中，分散在溶剂中的石墨纳米板的量总体上在溶剂总重量的从大约0.5 wt％至大约2 wt％的范围内。
此外，期望在最终模制复合物中石墨纳米板的总量很小，从而不会显著地增加最终产品的重量和体积。在一个非限制性示例中，石墨纳米板的总量小于最终模制复合物的2 wt％。例如，如果在复合物树脂基体中，三个涂布面罩包括2 wt％的总石墨纳米板，那么每个面罩包含大约0.7 wt％的石墨纳米板。
合适的石墨纳米板的非限制性示例包括片状石墨纳米板。这种纳米板由具有强粘附多层结构的天然石墨制成。所述层可以使用各种类型的插入剂（如，碱金属、金属卤化物、酸碱金属（acid alkali metal）等）插入。通过快速加热，插入石墨可以被剥离以形成可以进一步分离的膨胀层。膨胀石墨被粉碎以制成石墨烯的片状纳米板。
期望将石墨纳米板分散到选定溶剂或溶液中。石墨纳米板本质上是疏水性的，因而可以使用添加剂以利于板分散在选定溶剂中。在一个非限制性示例中，异丙基醇（isopropyl alcohol）被选择为溶剂且胶状纳米二氧化硅/异丙醇（isopropanol）溶液被选择为分散剂。可以使用的其他溶剂包括氯化烃和/或芳烃溶剂。可以使用的其他分散添加剂/制剂/助剂包括二甲亚矾、N-甲基吡咯烷酮、聚乙二醇单[4-(1,1,3,3-)甲基丁基]苯醚（polyethylene glycol mono [4-(1,1,3,3-tetramethylbutyl) phenyl] ether）、聚乙二醇单乙醚等。
石墨纳米板分散到选定溶剂/溶液中可通过将石墨纳米板添加到溶剂/溶液（包括分散助剂）中且将混合物暴露于超声波处理预定时间来完成。应当理解的是，超声波处理时间至少部分取决于所使用的石墨纳米板和溶剂/溶液以及石墨纳米板到溶剂/溶液中的可分散性。超声波处理槽的温度未被严格控制，但是溶液保持相对冷以防止由超声波处理引起的过热。这种过热会导致溶剂快速蒸发和分散效率的恶化。超声波处理时间还可取决于在相位分离开始之前可保持分散状态的最大持续时间。
现在参考图1B，薄的干燥纤维面罩浸渍到分散有石墨纳米板的溶液中，从而用石墨纳米板涂布面罩。纤维面罩的一个非限制性示例是玻璃、碳或聚合纤维面罩。面罩被允许在分散有石墨纳米板的溶液中浸泡预定时间，使得石墨纳米板粘附到面罩的一个或多个暴露表面上。该涂布工艺在没有任何上浆材料/上浆剂（如，聚合粘结剂）的情况下完成。
已涂布面罩然后被干燥。干燥可以通过在预定温度（其非限制性示例是室温）下蒸发溶剂预定时间来完成。
干燥后的已涂布面罩使用标准层叠工艺被层压在相邻预浸料体之间的界面处。如前文所述，可以使用任何期望预浸料体。在一个非限制性示例中，预浸料体是包括至多35 wt％环氧树脂和至少65 wt％碳纤维的单向碳纤维/环氧树脂预浸料体。关于纤维结构，可以使用由编织纤维（例如，平纹、缎纹、斜纹等）或者多个轴向纤维（如，未卷曲）制成的预浸料体。合适的预浸料体纤维材料的非限制性示例包括碳、玻璃、硼和聚合物。预浸料体中的碳纤维可以例如是12K碳纤维或24K碳纤维。合适的预浸料体基体树脂的非限制性示例包括环氧树脂、酚醛树脂、聚酯树脂、乙烯基酯树脂、聚酰亚胺树脂、热塑性树脂等。
在层压在一起之后，在界面之间具有已涂布面罩的预浸料体模制成复合部件，例如使用压缩模制技术（例如，参见图1C）。合适的模制技术的其他非限制性示例包括真空袋工艺和压热器法。
简而言之，图1A至1C示出了以下三个示意图：a）石墨纳米板（xGnP）通过超声波处理分散到酒精中；b）纤维面罩浸渍在xGnP分散体中且然后干燥；以及c）xGnP涂布面罩放置在多层单向（UD）预浸料体之间的界面中且UD预浸料体/面罩结构随后在热下被压缩。
在本文公开的示例中，构成纤维面罩（不要与附连的石墨纳米板混淆）的纤维的平均直径与构成预浸料体的纤维的平均直径相同或类似。在一个示例中，面罩和预浸料体中的纤维的平均直径在从大约7000 nm至大约9000 nm的范围内。这种纤维通常是商业可获得的，且在一些情况下可能是更期望的。应当理解的是，纤维面罩可以由较小纤维制成，而在一些情况下，这种面罩可能更难于制备且更昂贵。
为了进一步示出本文公开的示例，给出了以下示例。应当理解的是，这些示例提供用于说明目的，而不应理解为限制本文公开的示例的范围。
示例
模制面板样品根据本文公开的方法制备（一些具有5微米片状石墨纳米板（样品1a、1b和1c）、一些具有15微米片状石墨纳米板（样品2a、2b和2c）且一些具有1：1重量比的5和15微米片状石墨纳米板（样品3a和3b）），制备了三个对比模制面板样品，其中一个没有包括面罩（对比示例1）、其中另一个包括未涂布面罩（对比示例2）、其中另外一个包括碳纳米纤维涂布面罩（对比示例3）。
根据本文公开的方法的样品复合物如下制成。片状石墨纳米板具有不同级别，均分别具有5微米和15微米的标称尺寸，且由XG Sciences供应。为了制备含有面罩的片状石墨纳米板（xGnP），通过在冰水冷却槽中超声波处理1小时，高达2g的各种xGnP（5微米xGnP、15微米xGnP或两者的混合物）分别分散到125 ml至175 ml的异丙基醇中。在超声波处理之前，0.2 g至1 g的由Nissan Chemical制造的IPA-ST胶状纳米二氧化硅/异丙醇溶液（30 wt%的二氧化硅）添加到异丙基醇中，以便利于xGnP的分散。
分散溶液传输到相应方形槽，纤维面罩（由TFP供应的Optimat 20103A（玻璃纤维，17 g/m2））被浸渍到相应槽中且然后被取出。湿面罩通过在室温下蒸发乙醇大约30分钟而干燥。干燥的含有xGnP的面罩然后被称重。
在这些示例中使用的单向碳纤维环氧树脂预浸料体包括35 wt％的树脂和65 wt％的24K T700碳纤维（由Patz Materials and Technologies供应）。预浸料体的空气重量是300 g/m2。
应用标准层叠工艺，且层叠设置对于对比示例1是0/90/0/0/90/0，对于包括面罩的样品（V＝面罩）（样品1a至3b以及对比示例2和3）是0/V/90/0/V/0/90/V/0。层叠复合物样品中的每个在1.4 MPa和157℃下在画框（254 mm×254 mm）以及两个平板中压缩模制10分钟。具有面罩的模制面板复合物（即，样品1a至3b以及对比示例2和3）的标称厚度是大约1.85 mm，没有面罩的模制面板复合物（即，对比示例1）的标称厚度是大约1.80 mm。通过添加面罩和xGnP引起的重量增加小于复合物面板的2.2 wt％。
然后从层压复合物面板切出方形样品（100 mm×100 mm）以用于碰撞试验。碰撞试验使用配备有半球形碰撞塞（直径20 mm）的高速率Instron机器执行。选择0.5 m/秒的碰撞速度以提供足以使得样品在初步试验之后穿孔的能量。根据负荷-位移曲线，通过在每个样品的曲线下数值积分，可知最大负荷且计算相应能量。穿孔能量通过积分到穿孔点获得，超过穿孔点，仍存在负荷振动，但是表示铰链效应。碰撞试验使用高速视频照相机在样品的背侧录像，以确认负荷-位移曲线的解释。
从碰撞试验获得的三个典型负荷-位移曲线在图2中示出。曲线图示出了没有面罩的样品（对比示例1）、仅包括面罩的样品（对比示例2）以及带有具有5微米xGnP的面罩的样品（1.2 wt％，样品1a）的负荷（单位，千牛顿）对比位移（单位，毫米）。用于样品和对比示例的数量平均为2至3个相同或类似样品，每个样品执行至少两次试验。没有纤维面罩的样品（对比示例1）的碰撞曲线被稍微调高，以考虑在其他示例中通过添加面罩引起的厚度增加（0.05 mm或3％）。可以发现，与对比示例2（未涂布面罩）相比，将xGnP添加到面罩中不会引起任何可测量厚度变化。数据显示，添加面罩（具有或不具有xGnP）不改变样品的总碰撞性能。然而，最大负荷和碰撞能量对于仅含有未涂布纤维面罩的对比示例2显著增加，且对于含有用xGnP涂布的纤维面罩的样品（例如，样品1a）进一步增加。
在表1（下文）中概括了层压复合物（包括各种量的xGnP）的碰撞属性的改进，按照最大负荷的百分比增加、能量-最大负荷、以及穿孔能量（energy to penetration）。xGnP的浓度计算为在复合物样品中总树脂基体的重量百分比。结果表明，本文公开的方法成功地实现了使用不同类型xGnP和xGnP混合物中的每一种的层压复合物的碰撞属性的显著增强。
表1：层压复合物（12K， T700碳纤维预浸料体）的碰撞属性：不包括面罩的对比示例1；包括未涂布面罩的对比示例2；包括具有5微米xGnP的面罩的样品1（包括a、b和c）；包括具有15微米xGnP的面罩的样品2（包括a、b和c）和包括具有1：1重量比的5微米xGnP和15微米xGnP的面罩的样品3（包括a和b）。
在碰撞属性改进中添加xGnP的效果与在预浸料体之间包括碳纤维涂布面罩的层压复合物进行比较。该比较在图3中示出。除了石墨纳米板比碳纳米纤维总体上更便宜之外，样品1a和对比示例3的碰撞属性的提高类似。
虽然已经详细描述了多个示例，但是本领域技术人员将清楚，所公开示例可以变型。因而，前述说明被认为是示例性的而不是限制性的。

Claims (16)

1.一种层压复合物，包括：
多个堆叠预浸料体，所述预浸料体具有在每对相邻的预浸料体之间形成的界面，每个预浸料体包括基体材料和散置在其中的增强纤维；和
至少一个纤维面罩，所述至少一个纤维面罩被层压到所述界面中的至少一个的至少一部分上，所述至少一个纤维面罩具有附连到其至少一个表面上的石墨纳米板。
2.根据权利要求1所述的层压复合物，其中，具有附连到其上的石墨纳米板的所述至少一个纤维面罩给复合物增加预定厚度。
3.根据权利要求2所述的层压复合物，其中，所述预定厚度在从0.01 mm至0.1 mm的范围内。
4.根据权利要求1所述的层压复合物，其中，石墨纳米板是片状石墨纳米板。
5.根据权利要求1所述的层压复合物，其中，增强纤维是碳纤维，基体材料是树脂，其中，预浸料体中的每个包括至多35％重量的树脂和至少65％重量的碳纤维，其中，碳纤维选自包括12K碳纤维、24K碳纤维及其组合物的组。
6.根据权利要求1所述的层压复合物，其中，所述至少一个纤维面罩是玻璃纤维面罩。
7.根据权利要求1所述的层压复合物，其中，在层压复合物中石墨纳米板的量小于层压复合物的总wt％的2.5wt％。
8.根据权利要求1所述的层压复合物，其中，所述层压复合物展现了最大负荷、最大负荷的能量以及穿孔能量中的至少一个的增加。
9.根据权利要求1所述的层压复合物，其中，i）多个预浸料体和ii）至少一个纤维面罩中的每个都包括纤维，其中，这些纤维的平均直径范围从7000 nm至9000 nm。
10.根据权利要求1所述的层压复合物，其中，所述多个预浸料体中的每个包括：i）选自碳纤维、玻璃纤维、硼纤维和聚合物纤维的纤维；ii）选自单向结构、编织织物和多个轴向织物的结构；以及iii）选自环氧树脂、酚醛树脂、聚酯树脂、乙烯基酯树脂、 聚酰亚胺树脂、热塑性树脂的树脂。
11.一种制造抗碰撞层压复合物的方法，所述方法包括：
用石墨纳米板涂布至少一个纤维面罩的表面；
将所述至少一个纤维面罩层压到多个预浸料体之间的界面的至少一部分上，每个预浸料体包括在基体材料中的增强纤维；和
将层压的多个预浸料体和至少一个纤维面罩模制成复合物。
12.根据权利要求11所述的方法，其中，增强纤维是碳纤维，基体材料是树脂，其中，预浸料体中的每个包括至多35％重量的树脂和至少65％重量的碳纤维，其中，碳纤维选自包括12K碳纤维、24K碳纤维及其组合物的组。
13.根据权利要求11所述的方法，其中，石墨纳米板是片状石墨纳米板。
14.根据权利要求11所述的方法，其中，用石墨纳米板涂布至少一个纤维面罩的表面通过以下步骤完成：
将所述至少一个纤维面罩浸渍在含有分散在其中的石墨纳米板的溶液中；以及
干燥具有附连到其上的石墨纳米板的所述至少一个纤维面罩。
15.根据权利要求14所述的方法，其中，所述溶液包括异丙基醇、分散剂、以及胶状纳米二氧化硅和异丙醇的混合物。
16.一种纤维面罩，包括：
基体，所述基体包括多个纤维，所述多个纤维中的每个的平均直径在从7000 nm至9000 nm的范围内；和
石墨纳米板，所述石墨纳米板在没有聚合物粘结剂的情况下附连到所述多个纤维中的至少一些上。
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