CN113047059A - 一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用 - Google Patents

一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用 Download PDF

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CN113047059A
CN113047059A CN202110276295.5A CN202110276295A CN113047059A CN 113047059 A CN113047059 A CN 113047059A CN 202110276295 A CN202110276295 A CN 202110276295A CN 113047059 A CN113047059 A CN 113047059A
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titanium carbide
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杨伟
刘俊杰
卫春祥
朱三娥
鲁红典
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Hefei University
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Abstract

一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用，属于电磁干扰屏蔽复合面料制备的技术领域，由基底、屏蔽层以及保护层复合而成，将Ti3C2/CMC混合溶液涂覆到基底上，加热涂覆机通过相转化法制备出屏蔽层，然后将聚合物溶解在溶剂中，待静止脱泡后，将溶液涂覆在屏蔽层上，烘干形成聚合物保护层，从而得到疏水耐折碳化钛/聚合物复合面料。本发明通过将Ti3C2/CMC混合溶液涂覆到聚酯无纺布上，解决了纯Ti3C2耐折性能差的问题。CMC的加入使得屏蔽层表面形貌更好，屏蔽效果更强。通过在Ti3C2屏蔽层表面涂覆一层疏水致密的保护层来提升其疏水性能和耐折性能，从而极大提升了面料的应用前景和使用范围。

Description

一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用
技术领域
本发明属于电磁干扰屏蔽复合面料制备的技术领域，涉及一种利用涂覆法制备复合面料的方法，具体是涉及一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用。
背景技术
过去十年中，智能手机、平板电脑和便携式计算机等电子产品已广泛应用于日常生活中。电子产品产生的电磁干扰(EMI)大幅增加，从而造成电子设备故障和性能下降，甚至会影响人类健康。因此，需要开发具有优异EMI屏蔽性能的材料来解决电磁污染问题。目前，常见的用于EMI屏蔽的材料主要是金属材料。由于其易于成型，具有出色的EMI屏蔽能力而被广泛应用于电子工业和实际生活中。但是，这种材料也有自身无法避免的缺陷，如密度高、容易被腐蚀等。碳材料，尤其是二维层状材料，例如石墨烯纳米片和还原型氧化石墨烯，也可用于制备轻质EMI材料。然而，具有出色电导率的石墨烯制备工艺复杂，从而增加了制作成本，限制了其应用。碳化钛(Ti3C2)作为一种新型二维纳米材料，由于其独特的层状结构、良好的导电性、大的比表面积、超轻的重量、易于加工等特点，具有作为EMI屏蔽材料和产业化生产的巨大潜力。但也存在固有的缺陷，如机械性能差、亲水、易于氧化等。因此，研发一种疏水性能、耐折性能和电磁干扰屏蔽性能优异的柔性复合面料，值得本领域技术人员深入研究。
发明内容
本发明要解决的技术问题为克服现有技术的不足，提供一种疏水耐折碳化钛/聚合物复合面料及其制备方法与应用。具体是将具有良好EMI屏蔽性能的Ti3C2与无纺布和聚合物相结合，在保证有效屏蔽的前提下，提高耐折性能和疏水性能。
为了实现上述目的，本发明所采用的技术方案为：一种疏水耐折碳化钛/聚合物复合面料，是由基底、屏蔽层以及保护层复合而成，所述屏蔽层选自碳化钛Ti3C2。
作为本发明的进一步优选技术方案，疏水耐折碳化钛/聚合物复合面料中，所述屏蔽层由碳化钛Ti3C2和羧甲基纤维素钠CMC共同组成。一定量的CMC溶液作为粘结剂和交联剂滴加到Ti3C2溶液中，既可以增加溶液的粘度，还可以减少涂覆过程中Ti3C2溶液透过基底(如无纺布)下渗的问题。因此相比较纯的Ti3C2溶液涂覆到无纺布上，添加CMC之后Ti3C2溶液制备的面料表面形貌更好，电磁屏蔽效率更高。
作为本发明的进一步优选技术方案，疏水耐折碳化钛/聚合物复合面料中，基底可以是正常的高分子膜材料，其作为支撑层存在。例如，基底可以使用无纺布以及高分子膜等物质，优选采用聚酯无纺布。
作为本发明的进一步优选技术方案，保护层材料可以选自柔性、耐折及疏水的聚合物材料，优选采用聚氨酯TPU、聚羟基脂肪酸酯PHA、聚苯乙烯PS中的一种或多种。
作为本发明的另一目的，本发明提供了一种疏水耐折碳化钛/聚合物复合面料的方法，步骤如下：
1)、提供基底；
2)、在基底的表面涂覆屏蔽层；
3)、在屏蔽层上涂覆保护层。
作为该制备方法的优选技术方案，首先将Ti3C2/CMC混合溶液涂覆到基底上，加热涂覆机通过相转化法制备出屏蔽层，然后将聚合物溶解在溶剂中，待静止脱泡后，将溶液涂覆在屏蔽层上，烘干形成聚合物保护层，从而得到疏水耐折碳化钛/聚合物复合面料。
作为本发明的进一步优选技术方案，制备方法中所述溶剂选自于四氢呋喃、N，N-二甲基甲酰胺、二氯甲烷中的一种或多种。
与现有技术相比，本发明的疏水耐折碳化钛/聚合物复合面料的有益效果表现在：
本发明通过将Ti3C2/CMC混合溶液涂覆到聚酯无纺布上，解决了纯Ti3C2耐折性能差的问题。CMC的加入使得屏蔽层表面形貌更好，屏蔽效果更强。通过在Ti3C2屏蔽层表面涂覆一层疏水致密的保护层来提升其疏水性能和耐折性能，从而极大地提升了面料的应用前景和使用范围。
附图说明
图1(a)、(b)分别是Ti3C2面料、Ti3C2/CMC面料的表面SEM图，图1(c)～(f)分别是100μm Ti3C2/CMC2.5％面料、200μm Ti3C2/CMC2.5％面料、300μm Ti3C2/CMC2.5％面料、400μm Ti3C2/CMC2.5％面料的屏蔽层截面SEM图。
图2(a)～(d)分别是不同屏蔽层厚度的Ti3C2/CMC-PHA、Ti3C2/CMC、Ti3C2/CMC-TPU、Ti3C2/CMC-PS面料的EMI屏蔽性能图。
图3分别是不同屏蔽层厚度的Ti3C2/CMC、Ti3C2/CMC-TPU、Ti3C2/CMC-PHA、Ti3C2/CMC-PS面料的接触角性能图。
具体实施方式
以下结合实施例和附图对本发明疏水耐折碳化钛/聚合物复合面料及其制备方法与应用做出进一步的说明。
实施例1
1、屏蔽层的制备
1.1Ti3C2粉末的制备
首先通过向试管中加入2.5mL蒸馏水，然后加入7.5mL 9M盐酸来制备稀HCl。将0.5g LiF和0.5g Ti3AlC2添加到HCl溶液中，在40℃下反应，磁力搅拌48h，以除去中间层的Al。然后将反应混合物在9500rpm下离心5min，倒出上清液收集沉淀物，用新鲜的去离子水重复离心过程，直到混合物的pH值变为中性为止。通过将最后一个洗涤周期的沉淀物与120mL去离子水混合进行回收，超声处理30min进行剥离。随后将悬浮液在4000rpm下再次离心5min以除去未剥离的层状Ti3C2。最后，获得了包含单层或少层Ti3C2纳米片的悬浮液。将Ti3C2纳米片的悬浮液冷冻干燥后得到Ti3C2粉末。
1.2屏蔽层的制备
首先配制3wt％Ti3C2去离子水悬浮液、2.5wt％CMC的去离子水悬浮液。然后在磁力搅拌的条件下，将2.5wt％CMC悬浮液缓慢滴加到3wt％Ti3C2悬浮液中。搅拌2.5h后，再静止2.5h，得到铸膜液。
使用不同刻度的涂膜器(100μm、200μm、300μm、400μm)将铸膜液均匀地涂覆到聚酯无纺布基底上，烘干铸膜液，形成不同厚度的屏蔽层。由此得到未复合保护层的面料分别记为：100μm Ti3C2/CMC2.5％；200μmTi3C2/CMC2.5％；300μmTi3C2/CMC2.5％；400μm Ti3C2/CMC2.5％。
2、高分子聚合物保护层的制备：
将TPU高分子聚合物材料溶解于四氢呋喃中，使用机械搅拌器搅拌溶解，静置脱泡。用涂膜器(刻度为150μm)将铸膜液刮涂在屏蔽层上，加热烘干溶液得到复合面料。本实施例制备得到的面料在后续命名分别为：100μm Ti3C2/CMC2.5％-TPU；200μmTi3C2/CMC2.5％-TPU；300μmTi3C2/CMC2.5％-TPU；400μm Ti3C2/CMC2.5％-TPU。
实施例2
1、屏蔽层的制备：
同实施例1。
2、高分子聚合物保护层的制备：
将PHA高分子聚合物材料溶解于二氯甲烷中，使用机械搅拌器搅拌溶解，静置脱泡。用涂膜器(刻度为150μm)将铸膜液刮涂在屏蔽层上，加热烘干溶液得到复合面料。本实施例制备得到的面料在后续命名分别为：100μm Ti3C2/CMC2.5％-PHA；200μmTi3C2/CMC2.5％-PHA；300μmTi3C2/CMC2.5％-PHA；400μm Ti3C2/CMC2.5％-PHA。
实施例3
1、屏蔽层的制备：
同实施例1。
2、高分子聚合物保护层的制备：
将PS高分子聚合物材料溶解于N，N-二甲基甲酰胺中，使用机械搅拌器搅拌溶解，静置脱泡。用涂膜器(刻度为150μm)将铸膜液刮涂在屏蔽层上，加热烘干溶液得到复合面料。本实施例制备得到的面料在后续命名为：100μm Ti3C2/CMC2.5％-PS；200μmTi3C2/CMC2.5％-PS；300μmTi3C2/CMC2.5％-PS；400μm Ti3C2/CMC2.5％-PS。
对照例1
与实施例1的区别在于，将3wt％Ti3C2的去离子水悬浮液直接涂覆到无纺布上作为屏蔽层，溶液中没有添加粘结剂CMC去离子水悬浮液，也没有涂覆高分子聚合物保护层。本对照例制备得到的面料在后续命名为Ti3C2。
对照例2
与实施例1的区别在于，没有涂覆高分子聚合物保护层，无纺布基底上仅有2.5％Ti3C2/CMC作为屏蔽层。本对照例制备得到的面料在后续命名为：100μm Ti3C2/CMC2.5％；200μmTi3C2/CMC2.5％；300μmTi3C2/CMC2.5％；400μm Ti3C2/CMC2.5％。
表征实验：
1、SEM表征
利用扫描电镜(SU8010，Hitachi)来研究Ti3C2面料和2.5％Ti3C2/CMC面料屏蔽层表面形貌和微观结构，如图1所示。从图中可以观察到，没有添加CMC的Ti3C2屏蔽层表面形貌较差，表面孔洞大且密集。相比较而言，2.5％Ti3C2/CMC表面形貌较好，屏蔽层能有效地、完整地涂覆在无纺布表面。此外，还可以观察到各种屏蔽层的厚度，100μm Ti3C2/CMC2.5％、200μmTi3C2/CMC2.5％、300μmTi3C2/CMC2.5％、400μm Ti3C2/CMC2.5％的屏蔽层厚度分别为0.9μm、1.8μm、2.7μm、3.6μm。
2、EMI屏蔽表征
在EMI屏蔽测试中，样品的S参数是根据美国材料试验标准D 4935-89在8.2-12.4GHz区域(X波段)，利用矢量网络分析仪(AV3672，中国电子技术仪器有限公司)进行测试，测试结果如图2所示。可以观察到以下规律：
同一实施例下，屏蔽层越厚，EMI屏蔽效果越好；屏蔽层厚度保持一致的前提下，EMI屏蔽性能最好的是Ti3C2/CMC、其次是Ti3C2/CMC2.5％-PHA、再次一点的是Ti3C2/CMC2.5％-TPU，最差的是Ti3C2/CMC2.5％-PS。在所有面料中，满足EMI屏蔽商用需求(20dB)有：所有厚度的Ti3C2/CMC面料、所有厚度的Ti3C2/CMC2.5％-PHA面料、200μmTi3C2/CMC2.5％-TPU、300μmTi3C2/CMC2.5％-TPU、400μm Ti3C2/CMC2.5％-TPU以及400μm Ti3C2/CMC2.5％-PS。
3、接触角表征
水接触角(WCA)通过接触角计(JC2000DM，中国上海中晨数字技术设备有限公司)进行测量，测试结果如图3所示。可以观察到，整体来看，Ti3C2/CMC2.5％-PHA和Ti3C2/CMC2.5％-PS疏水性最好，其次是Ti3C2/CMC2.5％-TPU，Ti3C2/CMC最差。且Ti3C2/CMC面料亲水性会随着屏蔽层厚度的增加而增加。
4、耐折度表征
在耐折度测试中，根据中华人民共和国GB/T 457-2008，利用电脑测控耐折度仪(DCP-MIT135，四川长江造纸仪器有限责任公司，测试条件为施加4.9N的力)，进行测试，测试结果如表1所示。可以观察到，耐折性能最好的是：Ti3C2/CMC2.5％-TPU，耐折次数超过65000次，耐折性极好。其次是PHA保护层、PS保护层。而耐折性能最差的是无保护层的Ti3C2/CMC面料。
表1耐折度数据
Figure BDA0002976772580000051
以上内容仅仅是对本发明的构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (8)

1.一种疏水耐折碳化钛/聚合物复合面料，其特征在于，是由基底、屏蔽层以及保护层复合而成，所述屏蔽层选自碳化钛Ti3C2。
2.如权利要求1所述的疏水耐折碳化钛/聚合物复合面料，其特征在于，所述屏蔽层由碳化钛Ti3C2和羧甲基纤维素钠CMC共同组成。
3.如权利要求1或2所述的疏水耐折碳化钛/聚合物复合面料，其特征在于，所述基底选自聚酯无纺布。
4.如权利要求1或2所述的疏水耐折碳化钛/聚合物复合面料，其特征在于，所述保护层选自聚氨酯TPU、聚羟基脂肪酸酯PHA、聚苯乙烯PS中的一种或多种。
5.一种制备如权利要求2～4任一项所述疏水耐折碳化钛/聚合物复合面料的方法，其特征在于，步骤如下：
1)、提供基底；
2)、在基底的表面涂覆屏蔽层；
3)、在屏蔽层上涂覆保护层。
6.如权利要求5所述的方法，其特征在于，首先将Ti3C2/CMC混合溶液涂覆到基底上，加热涂覆机通过相转化法制备出屏蔽层，然后将聚合物溶解在溶剂中，待静止脱泡后，将溶液涂覆在屏蔽层上，烘干形成聚合物保护层，从而得到疏水耐折碳化钛/聚合物复合面料。
7.如权利要求6所述的方法，其特征在于，所述溶剂选自于四氢呋喃、N，N-二甲基甲酰胺、二氯甲烷中的一种或多种。
8.如权利要求2～4任一项所述疏水耐折碳化钛/聚合物复合面料在电磁干扰屏蔽材料中的应用。
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