CN117412862A - 复合材料以及用于形成该复合材料的方法 - Google Patents

复合材料以及用于形成该复合材料的方法 Download PDF

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CN117412862A
CN117412862A CN202280018348.6A CN202280018348A CN117412862A CN 117412862 A CN117412862 A CN 117412862A CN 202280018348 A CN202280018348 A CN 202280018348A CN 117412862 A CN117412862 A CN 117412862A
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pfa
mold
layer
composite
composite material
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宫内卓也
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Dupont Specialty Products Usa Ltd
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Dupont Specialty Products Usa Ltd
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Abstract

公开了一种复合材料，其具有(A)含有全氟烷氧基烷烃和碳纤维的基层、(B)中间层以及(C)聚四氟乙烯覆盖层，其中该中间层含有全氟烷氧基烷烃。

Description

复合材料以及用于形成该复合材料的方法
技术领域
本发明涉及一种具有全氟烷氧基烷烃(PFA)基层和聚四氟乙烯(PTFE)覆盖层的复合材料，这些层通过PFA中间层彼此结合。
背景技术
已知纤维增强的PFA是用于半导体制造设备的结构材料。可以将这种纤维增强的PFA模制以获得对设备有用的任何形状。在WO 2011/002883A中公开了一种获得纤维增强的PFA的实用方法，其公开了一种包含氟聚合物和碳纤维的复合制品，以及一种用于制造该复合制品的方法。
虽然纤维增强的PFA因其机械性能、耐热性和耐化学性是优异的材料，但是当材料暴露于强酸时，裸露在材料表面上的增强纤维被强酸氧化并降解。这导致材料性能劣化。降解的增强纤维可以容易地从材料上脱落并导致污染问题。此外，通过氧化产生的气体在高温下使材料的表面膨胀。
WO 2009/110341A公开了一种由包含碳粉或碳纤维作为增强材料的PFA和PTFE制成的构件，其中通过使构件与氧化气体接触，与构件的内部相比，构件表面上的碳粉/纤维被去除。然而，该方法在零件加工后需要若干个附加的步骤，如浸入氧化气体中并重新加热材料至软化温度或超过软化温度。
因此，在半导体技术中仍然需要纤维增强的PFA材料就耐酸性而言的进一步改进。
发明内容
因此，本发明的一个方面是一种复合材料，其包含(A)包含全氟烷氧基烷烃和碳纤维的基层、(B)中间层以及(C)聚四氟乙烯覆盖层，其中该中间层包含全氟烷氧基烷烃。
本发明的其他方面是两种用于制备以上所公开的复合材料的方法。第一种方法包括以下步骤：(a)制备包含PFA和碳纤维的固结垫，(b)在模具中放置覆盖层、中间层以及该多个固结垫，然后(c)在该模具中热压这三个组成部分以形成复合材料。
第二种用于制备以上所公开的复合材料的方法包括以下步骤：(d)制备包含PFA和碳纤维的固结垫，(e)在模具中放置多个固结垫，(f)热压该多个固结垫以形成模制的材料，(g)在模具中放置覆盖层、中间层和通过步骤(f)获得的该模制的材料，然后(h)在该模具中热压这三个组成部分以形成复合材料。
本发明的另外的方面是一种由以上所描述的复合材料形成的制品。
具体实施方式
本发明涉及一种复合材料，其包含：(A)包含全氟烷氧基烷烃(PFA)和碳纤维的基层、(B)中间层以及(C)聚四氟乙烯(PTFE)覆盖层，其中该中间层包含全氟烷氧基烷烃。
(A)PFA基层
PFA基层包含PFA和碳纤维。它还被称为碳纤维增强的PFA。这种材料在本领域中是已知的并且可以用于本发明。例如，WO 2011/002883A公开了一种包含氟聚合物和碳纤维的固结复合制品。在该公开中，首先制备含有碳纤维的PFA垫，然后将PFA垫堆叠，然后模制以形成复合制品。
可以使用任何种类的PFA。一般地，PFA具有通过ASTM E831的120至200×10-6/摄氏度的线膨胀系数，以及通过ASTM D1238的2至17g/分钟的熔体流动指数(MFI)。PFA可以在商业上获得，例如由科慕-三井氟产品有限公司(Chemours-Mitsui Fluoroproducts Co.,Ltd.)提供的具有2至15g/分钟的MFI的TeflonTMPFA。
在本发明中，碳纤维用作PFA基层的增强材料。碳纤维比由无机化学材料如SiC制成的其他纤维材料具有优势，由于与这种无机纤维相比，它的更柔软的特性并且更容易在商业上获得。
碳纤维可以在商业上获得，例如由东丽公司(Toray)提供的TORAYCATM或由帝人公司(Teijin)提供的TenaxTM。典型的短切碳纤维具有3至25mm的长度以及500至5,000的纵横比。
PFA基层中的碳纤维的含量是基于PFA基层的总重量优选从5至50wt％、更优选从10至30wt％。
PFA基层可以进一步含有任何其他添加剂，如碳纳米管、石墨粉和纳米金刚石。
PFA基层的厚度例如是从1至50mm、优选从15至35mm。
通过ASTM E831，PFA基层的垂直于模制方向的平面内线膨胀系数优选是从1至20×10-6/摄氏度、更优选从2至10×10-6/摄氏度，温度范围为从25至260摄氏度。
(B)中间层
基层和覆盖层通过中间层相互附着，并且中间层是本发明的关键。中间层包含全氟烷氧基烷烃(PFA)。
用作本发明的中间层的PFA可以是与PFA基层中使用的相同的PFA，但可以是不同的PFA，其具有数十万的分子量，通过ASTM D1238的2至17g/分钟的MFI。
中间层可以进一步含有本领域已知的添加剂，但不需要含有其他添加剂。
中间层的厚度优选是从10至2,000微米、更优选100至2,000微米。
(C)PTFE覆盖层
本发明所用的PTFE具有数百万至一千万的分子量作为模制等级。
在本说明书中，PTFE包括改性的PTFE。改性的PTFE的实例是例如用全氟(烷基乙烯基醚)(PAVE)改性的PTFE、用六氟丙烯(HFP)改性的PTFE等。
一般地，通过ASTM E831，PTFE覆盖层的线膨胀系数为从120至220×10-6/摄氏度。
PTFE覆盖层的厚度优选是从0.1至10mm、更优选从0.5至5mm。
制备复合材料的方法
有两种制备本发明的复合材料的方法。第一种方法是一步热压法，而第二种方法是两步热压法。第一种方法还公开为同时模制法。
第一种方法(方法1)具有在下文中公开的以下步骤(a)至(c)。
(a)制备包含PFA和碳纤维的固结垫：
首先，制备包含PFA和碳纤维的固结垫。可以通过将包含PFA和碳纤维的垫加热至高于两者的软化温度的温度，然后将其冷却至低于所述软化温度的温度来制备固结垫。可以根据WO 2011/002883A、WO 1993/011450和US 5506052A中公开的方法获得包含PFA和碳纤维的固结垫。
(b)在模具中放置覆盖层、中间层以及多个固结垫。
在下一步骤中，将固结垫切成模具形状并在模具中按特定数量堆叠。然后将中间层和覆盖层按顺序放置在模具中的堆叠的固结垫的顶部上。在模具中放置这三层的顺序可以颠倒。
(c)在模具中热压这三个组成部分以形成复合材料。
下一步骤是热压步骤以形成复合材料。对模具施加热量和压力持续足够量的时间以形成最终的复合材料。这样做所需的温度、压力和时间将随MFI、厚度和纤维负载量等因素而变化。示例性地，将模具在低于0.5MPa的压力下加热至高于327摄氏度(高于PTFE的熔融温度)，持续30至60分钟。然后将模具在比初始压力更高的压力下冷却至室温，并且获得复合材料。
第二种方法(方法2)具有在下文中公开的以下步骤(d)至(h)。
(d)制备包含PFA和碳纤维的固结垫，如以上所提及的与步骤(a)相同的方法，
(e)在模具中放置多个固结垫，与以上所提及的步骤(b)相同，除了中间层和覆盖层不放置在堆叠的固结垫上之外。
(f)热压以上所公开的多个固结垫以形成模制的材料。以与以上所公开的(c)相同的方式热压堆叠的固结垫。该步骤后，获得模制的材料，即模制的PFA-碳纤维材料，没有上层和中间层。
(g)在模具中放置覆盖层、中间层以及该模制的材料。
然后在模具中放置通过步骤(f)获得的该模制的材料。在模具中放置之前，可以将该模制的材料加工成适合模具尺寸的特定形状。然后，将中间层和覆盖层按顺序放置在模具中的该模制的材料的顶部上。
(h)在模具中热压这三个组成部分以形成复合材料。
与提及的步骤(C)相同的条件适用于复合材料的模制。这样做所需的温度、压力和时间将随复合材料的形状而变化。
(D)制品
该复合材料的显著特性是优异的耐酸性与良好的抗热冲击性结合，尽管层状结构的多种材料具有各自的线膨胀系数。
该复合材料可用作用于半导体制造设备、尤其是用于暴露于酸性液体的这些设备的部件，例如晶片清洗机、泵和阀门。并且它还可以用于化学加工工业如CPL生产、HF生产、TiO2生产以及用于金属精炼的高压酸浸，其中在这些方法中使用了硫酸。
实例
US2011/0001082 A、WO 2011/002867A、WO 2011/002877A和WO 2011/002883A中详述了与以下类似的材料，以及用于制造类似的材料和制品的方法，所有这些专利都以其全文通过援引并入。
原料
PFA(片状)
使用具有约305摄氏度的熔点、通过ASTM D1505约2.12至2.17的比重以及通过ASTM D882约31.4至41.2MPa的拉伸强度的片状的PFA。
PTFE(片状)
使用具有约327摄氏度的熔点、通过ASTM D1505约2.13至2.20的比重以及通过ASTM D882约20至35MPa的拉伸强度的片状的PTFE。
改性的PTFE(片状)
使用具有约327摄氏度的熔点、通过ASTM D1505约2.13至2.20的比重以及通过ASTM D882约20至35MPa的拉伸强度的片状的改性的PTFE。
实例1至33(同时模制法、一步模制法)
根据WO 2011/002883 Al的方法制备固结垫，切割的直径为91.5mm。一个固结垫的厚度约为0.3mm，并且它由20重量％的CF和80重量％的PFA制成。
在模具中一个接一个地堆叠约60个固结垫。然后，将表1中公开的PFA和PTFE或改性的PTFE按顺序放置在堆叠的固结垫上。之后，将堆叠件(即堆叠的固结垫、PFA和PTFE)放入模具中。
将基本上在环境温度下的模具放置在温度受控的压板式压机中并加热，以使整个堆叠件的温度大于327摄氏度，同时在小于0.5MPa的压力下沿厚度方向最低程度地压缩堆叠件，而在长度和宽度方向上不受任何附加压力的约束。保持该温度和压力持续大于30分钟。然后在结束加热的同时沿厚度方向进一步压缩完全加热的模具。然后在2.3至6.0MPa的压力下冷却模具。因此，堆叠件被固结成约16mm厚度的基层，并且整个制品的温度降低至低于290摄氏度。然后将堆叠件的温度和压力降低至环境条件，以获得复合材料。模制的复合材料具有91.5cm的直径，约16.0mm的堆叠的固结垫(基层)厚度，0.1至1.0mm的PFA(中间层)厚度，以及0.5至5.0mm的PTFE或改性的PTFE(覆盖层)厚度。
实例34至66(两步模制法)
除了PFA(中间层)和PTFE或改性的PTFE(覆盖层)没有放入模具中之外，进行与实例1至33相同的方法。在与实例1至33中公开的相同条件下热压(模制)堆叠的固结垫。获得没有中间层和覆盖层的模制的固结垫。
将表2中公开的PTFE或改性的PTFE(覆盖层)和PFA(中间层)按顺序放入模具中。然后将获得的模制的固结垫放置在PFA上。在与实例1至33中公开的相同条件下热压堆叠件(即PTFE或改性的PTFE、PFA和模制的固结垫)。
模制的复合材料具有91.5cm的直径，约16.0mm的堆叠的固结垫(基层)厚度，0.1至1.0mm的PFA(中间层)厚度，以及0.5至5.0mm的PTFE或改性的PTFE(覆盖层)厚度。
分析方法
1.热冲击试验
通过切片和切割从获得的模制的复合材料制备测试件。将模制的复合材料的基层切成4.0mm的厚度。然后，从10mm的宽度切割模制的材料，并在测试件的平面的中心钻两个孔(直径为3mm)。
热冲击试验，也称为温度冲击试验，将产品暴露于交替的冷和热温度循环。热冲击试验用于评估物品是否能够承受周围环境温度的突然变化，而不会出现物理损伤或性能劣化。测试件反复浸入热硅油中加热，并且拿起用风扇冷却。使用50摄氏度为冷和200摄氏度为热的温度设置，持续2,000个循环，以评估基层、中间层与覆盖层之间的附着性。
荧光渗透探伤用于评估热冲击试验前后的附着情况。在评估中，将荧光渗透剂粘贴在测试件上并用溶剂(乙醇)擦拭。然后使用黑光，评估测试件的层之间是否存在任何间隙。结果在表1和2中示出。
外观
〇：良好(无剥离)
△：一般(部分剥离)
×：不好(剥离)
荧光渗透探伤
〇：良好(无间隙)
△：一般(约10至100微米的微小间隙)
×：不好(显著的间隙)
表1
表2
结果表明，如果不施加中间层，则覆盖层可以容易地剥离，并且与在模制的复合材料上附加的模制相比，与固结垫同时模制显示出优异的附着性。

Claims (9)

1.一种复合材料，其包含：
(A)包含全氟烷氧基烷烃和碳纤维的基层，
(B)中间层以及
(C)聚四氟乙烯覆盖层，
其中所述中间层包含全氟烷氧基烷烃。
2.如权利要求1所述的复合材料，其中所述基层(A)的线膨胀系数为从3至15×10-6/摄氏度，并且所述PTFE覆盖层的线膨胀系数为120至220×10-6/摄氏度。
3.如权利要求1所述的复合材料，其中在热冲击试验后，即通过将所述复合材料置于50摄氏度下，然后在200摄氏度下加热作为一个循环，重复2,000次后，所述基层与PTFE覆盖层是结合的。
4.如权利要求1所述的复合材料，其中层(B)的厚度为从10至2,000微米。
5.一种用于制备如权利要求1所述的复合材料的方法，所述方法包括以下步骤：
(a)制备包含PFA和碳纤维的多个固结垫，以及
(b)在模具中放置覆盖层、中间层以及所述多个固结垫，然后
(c)在所述模具中热压这三个组成部分以形成复合材料。
6.一种用于制备如权利要求1所述的复合材料的方法，所述方法包括以下步骤：
(d)制备包含PFA和碳纤维的固结垫，
(e)在模具中放置多个固结垫，
(f)热压所述多个固结垫以形成模制的材料，
(g)在模具中放置覆盖层、中间层以及所述模制的材料，
(h)在所述模具中热压这三个组成部分以形成复合材料。
7.一种制品，其由如权利要求1所述的复合材料形成。
8.如权利要求7所述的制品，其用于半导体制造方法。
9.如权利要求7所述的制品，其用于化学加工方法。
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