CN113025032B - 一种高介电性能自愈合聚氨酯复合材料及其制备的方法和制动应用 - Google Patents
一种高介电性能自愈合聚氨酯复合材料及其制备的方法和制动应用 Download PDFInfo
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Abstract
本发明公开了一种高介电性能自愈合聚氨酯复合材料及其制备的方法和制动应用,一种高介电性能自愈合聚氨酯复合材料,所述高介电性能自愈合聚氨酯复合材料是由M/TiC复合填料与自愈合介电弹性体材料组成的混合材料,所述M/TiC复合填料重量含量为0.02‑0.1%,M/TiC复合填料为纳米颗粒材料,M为Au、Al、Ti、Zr、Fe、Co、Ni、Cu、Ag和Zn中的任意一种。本发明通过M/TiC复合填料的填入一方面提高了弹性体薄膜的介电性能;另一方面,开辟了提高弹性体制动器制动性能的新方法;与传统陶瓷填料相比,M/TiC参杂量更少,而且具有高介电性,低介电损耗的优异性能,制动器器件表现出更高的机电稳定性。
Description
技术领域
本发明属于自愈合弹性体材料和介电弹性体微制动器领域,具体涉及一种高介电性能自愈合聚氨酯复合材料及其制备的方法和制动应用。
背景技术
目前大多数机器人依靠刚性部件,在结构化的环境中出色完成重复性工作。相比之下,生物则通过其柔软结构来适应外界环境,这种差异促使软机器人的发展,及由柔性材料制成,可以适应周围环境的新型软机器人。在各种软机器人驱动结构中,电制动器由于其柔软性、高能量密度、无声操作和类似肌肉的性能优点被认为是最有前途的制动方式。迄今为止,已经报道了许多介电弹性体微制动器,也被用于各种设备,例如传感器、平板扬声器、微型飞行器和尺蠖机器人。然而,介电弹性体微制动器在制动的过程中通常需要在介电弹性体微制动器上施加高电压(高达数千伏),高电压易击穿电介质而导致介电弹性体微制动器寿命损害。电介质被击穿时电极之间的电压会突然释放,在此过程中会产生大量的热量,这将导致介电弹性体燃烧,从而损坏整个介电弹性体微制动器。同时,介电弹性体微制动器在运行过程中容易磨损或部分损坏,这些缺点严重限制了它的发展。
为了提高介电弹性体微制动器的可靠性,制造在损坏或击穿后能够自愈并保持原有的性能运行的器件是该领域的研究趋势。如果介电弹性体微制动器具有自愈合的能力,它不仅可以修复材料本身的内部缺陷,还可以修复由磨损或击穿引起的裂纹,以保持结构和功能的完整性,从而增加安全性和寿命。
近年来介电弹性体微制动器明显的发展态势是逐步趋向集成软功能电子设备的研究,而功能化集成意味着要适应更为复杂的工作环境,这对器件稳定性是一个极大的考验,也对弹性体材料的要求更为苛刻。近5年研究自愈合弹性体材料的热度大幅上升,自愈合性能可以很大程度的提高电子皮肤和制动器的工作稳定性,进而适应更多功能集成应用。
发明内容
本发明的目的在于:针对上述存在的问题,本发明提供一种高介电性能自愈合聚氨酯复合材料及其制备的方法和制动应用,旨在填加Au/TiC复合材料到自愈合介电弹性体材料中形成高介电性能自愈合聚氨酯复合材料,实现在低含量填料下介电常数的明显提升,获得较好的机械稳定性。
本发明采用的技术方案如下:
一种高介电性能自愈合聚氨酯复合材料,所述高介电性能自愈合聚氨酯复合材料是由M/TiC复合填料与自愈合介电弹性体材料组成的混合材料,所述M/TiC复合填料重量含量为0.02-0.1%,M/TiC复合填料为纳米颗粒材料,M为Au、Al、Ti、Zr、Fe、Co、Ni、Cu、Ag和Zn中的任意一种。
优选的,所述自愈合介电弹性体材料为PU-UPy、PDMS-Upy和PDMS-PANI中的任意一种。
优选的,所述高介电性能自愈合聚氨酯复合材料是由Au/TiC复合填料与自愈合介电弹性体材料PU-UPy组成的混合材料,所述Au/TiC复合填料重量含量为0.02wt%-0.1wt%,Au/TiC为纳米颗粒材料。
本发明的第二个目的是提供基于一种高介电性能自愈合聚氨酯复合材料的制备方法,包括如下步骤:
步骤1:将PTMEG(聚四亚甲基醚二醇)在真空下110-130℃搅拌1.5-3h,除水后冷却至65-75℃;
步骤2:将HDI(六亚甲基二异氰酸酯)加入烧瓶中搅拌0.5-1.5h,后加入催化就DBTDL(二月桂酸二丁基锡)升温75-85℃搅拌2.5-3.5h;
步骤3:降温至65-75℃后,加入UPy-NCO(嘧啶酮)并加入DMF(N,N-二甲基甲酰胺)作为溶剂在75-85℃反应2.5-3.5h;
步骤4:将M纳米颗粒和TiC按照质量比1:(0.8-1.2)混合在DMF溶剂中,并超声分散;
步骤5:将表面改性的M/TiC复合填料按重量比0.02-0.1%与PU-UPy混合,并搅拌30min;
步骤6:将产物放入烘箱干燥,即得到高介电性能自愈合聚氨酯复合材料。
优选的,所述PTMEG、HDI、UPy-NCO的用量摩尔比为1:1.5:0.5,其中DBTDL的用量为1到2滴的催化剂的用量。
本发明的第三个目的是一种自愈合介电弹性体微制动器,其结构为电容式结构,由柔性电极和夹在柔性电极中间的介电层组成,所述介电层为前述的高介电性能自愈合聚氨酯复合材料制备而成。
优选的,所述介电层的厚度为90-110μm。
优选的,所述柔性电极为导电碳脂、碳润滑脂、石墨、银纳米线、碳纳米管中的任意一种。
优选的,所述自愈合介电弹性体微制动器的制备方法为:将步骤5制备的产物倒入模具中,放入烘箱干燥成介电薄膜,即得到介电层;再将所述介电层上下两侧均匀涂覆、喷涂或旋涂覆柔性电极,即得到自愈合介电弹性体微制动器。
优选的,所述介电薄膜通过旋涂、刮涂、滴膜、印刷中的任意一种方法制备而成。
自愈合介电弹性体材料的自愈合机理源于侧链(例如UPy)产生的多重氢键作用力;由于自愈合介电弹性体材料(例如PU-UPy、PDMS-Upy和PDMS-PANI)薄膜制动性能较差,制动电压过高,所以本发明在合成反应结束后加入少量表面改性的M/TiC(M为Au、Al、Ti、Zr、Fe、Co、Ni、Cu、Ag或Zn)复合填料,较少的参杂下可以提高薄膜的介电性能,并获得较好的机械稳定性;根据麦克斯韦压应力公式,介电常数的提高可以降低制动所需的电压。因此本发明一方面可以避免制动器应用时所需高压带来的安全隐患;另一方面,该复合材料集成自愈合特性,可以为多领域应用开辟新的前景,如人工肌肉、机器人和微制动器等。
与现有的技术相比本发明的有益效果是:
本发明通过M/TiC(M为Au、Al、Ti、Zr、Fe、Co、Ni、Cu、Ag或Zn)复合填料的填入一方面提高了弹性体薄膜的介电性能;另一方面开辟了提高弹性体制动器制动性能的新方法;与传统陶瓷填料相比,M/TiC参杂量更少,而且具有高介电性,低介电损耗的优异性能,制动器器件表现出更高的机电稳定性。
附图说明
图1是本发明的介电弹性体微制动器结构示意图。
图中标记为:1-介电层,2-柔性电极,3-铜箔导线连接电源正极,4-微型光谱仪一,5-铜箔导线连接电源负极。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明,即所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。
实施案例1
如图1所示为本发明的介电弹性体微制动器的基础结构,其为电容式结构,由中间的介电层和上下两侧的柔性电极组成,柔性电极材料为导电碳脂,柔性电极两极分别通过导电铜箔连接高压电源的正负极;介电层为填入Au/TiC复合填料的自愈合聚氨酯(PU-UPy),其中Au/TiC重量含量为0.02wt%混合构成,厚度为100μm。一种高介电性能自愈合性能的介电弹性体微制动器的制备方法,包括如下步骤:
①将PTMEG在真空下120℃搅拌2h,除水后冷却至70℃;
②将HDI加入烧瓶中搅拌1h,后加入DBTDL升温80℃搅拌3h;
③降温至70℃后,加入UPy-NCO并加入DMF作为溶剂在80℃反应2h;
④将Au纳米颗粒和TiC按照质量比1:1混合在DMF溶剂中,并超声分散;
⑤将表面改性的Au/TiC复合填料按0.02wt%重量比例与PU-UPy混合,并搅拌30min;
⑥将产物倒入模具,放入烘箱干燥成膜;
⑦将薄膜上下两侧均匀涂膜导电碳脂,并通过铜箔导线连接高压电源进行制动测试。
测试结果详见表1。
实施案例2:
如图1所示为本发明的介电弹性体微制动器基础结构,其为电容式结构,由中间的介电层和上下两侧的柔性电极组成,电极材料为导电碳脂,两极分别通过导电铜箔连接高压电源的正负极;介电层为填入Au/TiC复合填料的自愈合聚氨酯(PU-UPy),其中Au/TiC重量含量为0.04wt混合构成,厚度为100μm。一种高介电性能自愈合性能的介电弹性体微制动器的制备方法,包括如下步骤:
①将PTMEG在真空下120℃搅拌2h,除水后冷却至70℃;
②将HDI加入烧瓶中搅拌1h,后加入DBTDL(催化剂)升温80℃搅拌3h;
③降温至70℃后,加入UPy-NCO并加入DMF作为溶剂在80℃反应2h;
④将Au纳米颗粒和TiC按照质量比1:1混合在DMF溶剂中,并超声分散;
⑤将表面改性的Au/TiC复合填料按0.04wt%比例与PU-UPy混合,并搅拌30min;
⑥将产物倒入模具,放入烘箱干燥成膜;
⑦将薄膜上下两侧均匀涂膜导电碳脂,并通过铜箔导线连接高压电源进行制动测试。
测试结果详见表1。
实施案例3:
如图1所示为本发明的介电弹性体微制动器基础结构,其为电容式结构,由中间的介电层和上下两侧的柔性电极组成,电极材料为导电碳脂,两极分别通过导电铜箔连接高压电源的正负极;介电层为填入Au/TiC复合填料的自愈合聚氨酯(PU-UPy),其中Au/TiC重量含量为0.06wt%的混合构成,厚度为100μm。一种高介电性能自愈合性能的介电弹性体微制动器的制备方法,包括如下步骤:
①将PTMEG在真空下120℃搅拌2h,除水后冷却至70℃;
②将HDI加入烧瓶中搅拌1h,后加入DBTDL升温80℃搅拌3h;
③降温至70℃后,加入UPy-NCO并加入DMF作为溶剂在80℃反应2h;
④将Au纳米颗粒和TiC按照质量比1:1混合在DMF溶剂中,并超声分散;
⑤将表面改性的Au/TiC复合填料按0.06wt%比例与PU-UPy混合,并搅拌30min;
⑥将产物倒入模具,放入烘箱干燥成膜;
⑦将薄膜上下两侧均匀涂膜导电碳脂,并通过铜箔导线连接高压电源进行制动测试。
测试结果详见表1。
实施案例4:
如图1所示为本发明的介电弹性体微制动器基础结构,其为电容式结构,由中间的介电层和上下两侧的柔性电极组成,电极材料为导电碳脂,两极分别通过导电铜箔连接高压电源的正负极;介电层为填入Au/TiC复合填料的自愈合聚氨酯(PU-UPy),其中Au/TiC重量含量为0.08wt%的混合构成,厚度为100μm。一种高介电性能自愈合性能的介电弹性体微制动器的制备方法,包括如下步骤:
①将PTMEG在真空下120℃搅拌2h,除水后冷却至70℃;
②将HDI加入烧瓶中搅拌1h,后加入DBTDL升温80℃搅拌3h;
③降温至70℃后,加入UPy-NCO并加入DMF作为溶剂在80℃反应2h;
④将Au纳米颗粒和TiC按照质量比1:1混合在DMF溶剂中,并超声分散;
⑤将表面改性的Au/TiC复合填料按0.08wt%比例与PU-UPy混合,并搅拌30min;
⑥将产物倒入模具,放入烘箱干燥成膜;
⑦将薄膜上下两侧均匀涂膜导电碳脂,并通过铜箔导线连接高压电源进行制动测试。
测试结果详见表1。
实施案例5:
如图1所示为本发明的介电弹性体微制动器基础结构,其为电容式结构,由中间的介电层和上下两侧的柔性电极组成,电极材料为导电碳脂,两极分别通过导电铜箔连接高压电源的正负极;介电层为填入Au/TiC复合填料的自愈合聚氨酯(PU-UPy),其中Au/TiC重量含量为0.1wt%的混合构成,厚度为100μm。一种高介电性能自愈合性能的介电弹性体微制动器的制备方法,包括如下步骤:
①将PTMEG在真空下120℃搅拌2h,除水后冷却至70℃;
②将HDI加入烧瓶中搅拌1h,后加入DBTDL升温80℃搅拌3h;
③降温至70℃后,加入UPy-NCO并加入DMF作为溶剂在80℃反应2h;
④将Au纳米颗粒和TiC按照质量比1:1混合在DMF溶剂中,并超声分散;
⑤将表面改性的Au/TiC复合填料按0.1wt%比例与PU-UPy混合,并搅拌30min;
⑥将产物倒入模具,放入烘箱干燥成膜;
⑦将薄膜上下两侧均匀涂膜导电碳脂,并通过铜箔导线连接高压电源进行制动测试。
测试结果详见表1。
表1实施例1-5的制动性能测试
Au/TiC占比(wt%) | 样品厚度(μm) | 施加电压(MV/m) | 最大制动应变(%) | |
实施例1 | 0.02 | 105 | 36.5 | 29.2 |
实施例2 | 0.04 | 101 | 38 | 31.6 |
实施例3 | 0.06 | 98 | 39.6 | 33.5 |
实施例4 | 0.08 | 96 | 41 | 37.2 |
实施例5 | 0.1 | 102 | 37.5 | 39.9 |
由表1可知,Au/TiC填料的少量的填入(0.02-0.1%),一方面提高了弹性体薄膜的介电性能;另一方面开辟了提高弹性体制动器制动性能的新方法。
以上所述实施例仅表达了本申请的具体实施方式,其描述较为具体和详细,但并不能因此而理解为对本申请保护范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本申请技术方案构思的前提下,还可以做出若干变形和改进,这些都属于本申请的保护范围。
Claims (9)
1.一种自愈合介电弹性体微制动器,其特征在于,其结构为电容式结构,由柔性电极和夹在柔性电极中间的介电层组成,所述介电层由高介电性能自愈合聚氨酯复合材料制备而成;所述高介电性能自愈合聚氨酯复合材料是由M/TiC复合填料与自愈合介电弹性体材料组成的混合材料,所述M/TiC复合填料重量含量为0.02-0.1%,M/TiC复合填料为纳米颗粒材料,M为Au、Al、Ti、Zr、Fe、Co、Ni、Cu、Ag和Zn中的任意一种。
2.根据权利要求1所述的一种自愈合介电弹性体微制动器,其特征在于,所述自愈合介电弹性体材料为PU-UPy。
3.根据权利要求1所述的一种自愈合介电弹性体微制动器,其特征在于,所述高介电性能自愈合聚氨酯复合材料是由Au/TiC复合填料与自愈合介电弹性体材料PU-UPy组成的混合材料,所述Au/TiC复合填料重量含量为0.02wt%-0.1wt%,Au/TiC为纳米颗粒材料。
4.根据权利要求1-3任一项所述的一种自愈合介电弹性体微制动器,其特征在于,高介电性能自愈合聚氨酯复合材料的制备方法,包括如下步骤:
步骤1:将PTMEG在真空下110-130℃搅拌1.5-3h,除水后冷却至65-75℃;
步骤2:将HDI加入搅拌0.5-1.5h,后加入DBTDL升温75-85℃搅拌2.5-3.5h;
步骤3:降温至65-75℃后,加入UPy-NCO并加入DMF作为溶剂在75-85℃反应2.5-3.5h;
步骤4:将M和TiC按照质量比1:(0.8-1.2)混合在DMF溶剂中,并超声分散;
步骤5:将M/TiC复合填料按重量比0.02-0.1%与PU-UPy混合,并搅拌30min;
步骤6:将产物放入烘箱干燥,即得到高介电性能自愈合聚氨酯复合材料。
5.根据权利要求4所述的一种自愈合介电弹性体微制动器,其特征在于,所述PTMEG、HDI、UPy-NCO的用量摩尔比为1:1.5:0.5。
6.根据权利要求1所述的一种自愈合介电弹性体微制动器,其特征在于,所述介电层的厚度为90-110μm。
7.根据权利要求1所述的一种自愈合介电弹性体微制动器,其特征在于,所述柔性电极为导电碳脂、碳润滑脂、石墨、银纳米线、碳纳米管中的任意一种。
8.根据权利要求1所述的一种自愈合介电弹性体微制动器,其特征在于,所述自愈合介电弹性体微制动器的制备方法为:将高介电性能自愈合聚氨酯复合材料倒入模具中,放入烘箱干燥成介电薄膜,即得到介电层;再将所述介电层上下两侧均匀涂覆柔性电极,即得到自愈合介电弹性体微制动器。
9.根据权利要求8所述的一种自愈合介电弹性体微制动器,其特征在于,所述介电薄膜通过旋涂、刮涂、滴膜、印刷中的任意一种方法制备而成。
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