CN114131825A - 一种双面有序阵列发泡材料及其制备方法和应用 - Google Patents
一种双面有序阵列发泡材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及功能性材料技术领域,具体涉及一种双面有序阵列发泡材料及其制备方法和应用,本发明发泡材料将热塑性聚合物薄片与不具有发泡性能的硬质网格紧密结合为层状结构,硬质网格能够实现热塑性聚合物内部受限,在发泡过程中硬质网格从内部限制了气体的水平逸出,产生竖直方向的气体定向逃逸,竖直方向上硬质网格周围的气体逸出较弱,越远离硬质网格气体的定向逸出越强,从而使气体呈现出在网格两侧反向逸出的趋势,进而形成双向有序阵列结构的发泡材料。阵列结构与泡孔结构可通过压强、温度、网格尺寸等参数予以调控。该类发泡材料在自支撑纳米发电、柔性传感等领域具有高应用价值。本发明制备方法工艺简单,易调控,成本低,易于规模化且节能环保。
Description
技术领域
本发明涉及功能性材料技术领域,具体涉及一种双面有序阵列发泡材料及其制备方法和应用。
背景技术
在绿色制造与低碳目标的背景下,超临界发泡技术受到越来越多的关注,逐渐成为聚合物泡沫材料生产的一项主要技术。超临界CO2(scCO2)发泡技术由于其高效、环保、安全、成本低、适用性广等优势,广泛应用于日常生产、生活以及军工、航空领域,在人类生产生活中发挥着不可替代的作用。
热塑性聚氨酯(TPU)等聚合物弹性体,是常用的发泡聚合物材料之一。TPU发泡材料具有良好缓冲吸能功能,可作为鞋底、沙发家具、枕头、坐垫、玩具、服装和隔音内衬;良好的隔热性能使其可应用于建筑物外墙保温,屋面防水保温一体化、冷库保温隔热、管道保温材料、建筑发泡材料、冷藏车及冷库隔热材等。
聚合物材料表面形成规则阵列泡沫能够增加宏观尺度的复杂性,提升其比表面积,赋予其功能化特性,拓展其应用场景和应用领域。目前制备聚合物材料阵列结构的方法主要有三种,一种是刻蚀法,主要是通过化学刻蚀或者物理激光刻蚀等减材制造的技术得到有序的阵列;另一种是3D打印技术,与刻蚀法的减材制造模式完全相反,3D打印技术通过增材制造的加工方式同样可以得到高分子有序阵列结构;第三种为转印法,此方法建立在前两者的基础上,先通过上述工艺得到相应的模板,然后通过复刻模板得到有序阵列。这三种方式存在诸如能耗大,操作复杂,环境污染等问题,极大程度上限制了它们的工业推广和使用范围,导致这些方式很难走出实验室实现工业生产的大规模连续化生产。此外,目前尚未有文献报道过具有阵列结构的聚合物泡沫材料的研制。
因此,研究开发一种操作简便、省时环保、能耗小、适于工业化生产的双面有序阵列结构的发泡材料,能够拓展该类材料在新兴功能化领域的应用潜力,同时有望提升发泡材料的吸能、缓冲、阻隔、隔热、电磁屏蔽等综合性能。
发明内容
本发明的目的之一在于提供一种双面有序阵列发泡材料,利用硬质网格对热塑性聚合物进行受限,诱导气体的定向逃逸,并利用硬质网格的自身强度对整体结构产生支撑作用,继而在发泡过程中产生相邻网格的热塑性聚合物产生反向的气体逃逸,一步发泡直接产生双面有序阵列结构,可用作自供能传感的组装,同时还有望应用于吸能、缓冲、阻隔、隔热、电磁屏蔽、等诸多领域。
本发明的目的之二在于提供一种双面有序阵列发泡材料的制备方法,通过在热塑性聚合物发泡材料之间设置硬质网格材料夹层,再结合发泡技术一步发泡直接获得有序双面阵列结构的高分子发泡材料。该方法省时环保,操作简单,易于调控和规模化,提供了一种全新的双面有序阵列发泡材料的制备方法。
本发明的目的之三在于提供采用本发明提供的双面有序阵列发泡材料,可制备自支撑摩擦电纳米发电机,应用于绿色能源收集,以及作为自供能传感器来监测人体活动。
为了实现上述目的,本发明采用的技术方案如下:
一种双面有序阵列发泡材料的制备方法,包括以下操作步骤:
1)将两层热塑性聚合物薄片与置于两层热塑性聚合物薄片之间的无发泡性能的硬质网格紧密结合,形成复合材料预制件;
2)将复合材料预制件进行气体发泡处理,制得所述双面有序阵列发泡材料。
可选的,步骤1)所述复合材料预制件的厚度为0.4~0.7mm。
为了提高所制备发泡材料阵列结构的有序性,作为优选的,步骤1)中无发泡性能的硬质网格的目数为14目、16目或18目。
任意的不具有发泡性能、能够对上下层的热塑性聚合物薄片的发泡性能产生限制作用,形成受限发泡的网格薄片均可应用与本发明,作为举例说明,步骤1)中无发泡性能的硬质网格为不锈钢网。考虑到具体应用场景,比如应用于制作摩擦纳米发电机,步骤1)无发泡性能的硬质网格为具有导电性能的金属网。
任意的具有发泡性能的热塑性聚合物薄片均可应用于本发明制作双面有序阵列发泡材料,作为举例说明,步骤1)中热塑性聚合物薄片为热塑性聚氨酯(TPU)薄片。
可选的,步骤1)中通过热压的方式形成复合材料预制件;当热塑性聚合物为聚氨酯时,热压温度为180~200℃,热压时间为10~20min。
可选的,步骤2)中所述的气体发泡处理为将复合材料预制件在发泡温度下与超临界CO2形成饱和稳定的共混体系后,保持一定时间,快速卸压,将样品取出自然冷却至室温。
在本发明的一些具体实施例中,发泡温度为100~120℃;饱和稳定共混体系的压强为13~16MPa;保持时间为1.5~2小时。
由上述制备方法制备而成的双面有序阵列发泡材料,能够应用于制作摩擦电纳米发电机。具体的,以双面有序阵列发泡材料作为正极材料,并提供支撑,硅橡胶(Ecoflex)设置在双面有序阵列发泡材料的上下表面作为负极,双面有序阵列发泡材料中间的金属网(不锈钢网)作为电极导出电子。在需要刚性工作模式的应用场景下,采用了亚克力板固定负极材料(硅橡胶);在需要柔性工作模式的应用场景下,采用了聚酰亚胺膜封装负极材料(硅橡胶)。
摩擦电纳米发电机装置,在外力作用下被压缩,在压缩过程中硅橡胶层受压发生变形进入双面阵列结构发泡材料的凹陷内部,由于正负电材料的接触产生电荷,从而在外电路形成电流,输出电流信号,实现机械能向电能的转换。该柔性摩擦电纳米发电机装置由于其体积小、无能耗的优势,可应用于柔性传感器领域,用于检测人体活动,例如:人走路习惯、频率的监测,落座时间、频率的监测,拳击力度和频率的监测等。
本发明双面有序阵列发泡材料的制备基于聚合物发泡材料的受限发泡和气体定向逃逸原理,利用不具有发泡性能的硬质网格对热塑性聚合物进行内部受限发泡。将热塑性聚合物薄片与不具有发泡性能的硬质网格紧密结合为层状结构,硬质网格能够实现热塑性聚合物内部受限,在发泡过程中硬质网格从内部限制了气体的水平逸出,产生竖直方向的气体定向逃逸,竖直方向上硬质网格周围的气体逸出较弱,越远离硬质网格的气体定向逸出越强,从而使气体呈现出在网格两侧反向逸出的趋势,进而形成双向有序阵列结构的发泡材料。阵列结构与泡孔结构可通过压强、温度、网格尺寸等参数予以调控,与传统有序阵列的制备工艺相比,比如3D打印、刻蚀法、转印法,本发明制备方法,工艺简单,成本低,易于规模化,且节能环保。该类发泡材料在自支撑纳米发电、柔性传感等领域具有高应用价值。
附图说明
图1为实施例1提供的双面有序阵列TPU发泡材料制备工艺流程示意;
图2为实施例1提供的双面有序阵列TPU发泡材料制备工艺的方法原理示意图;
图3为不同目数不锈钢网发泡制备的双面有序阵列TPU发泡材料正面与反面的照片;
图4为不同目数不锈钢网发泡制备的双面有序阵列TPU发泡材料的横截面SEM照片;
图5为不同目数不锈钢网发泡制备的双面有序阵列TPU发泡材料的表面SEM照片;
图6为不同发泡压强下制备的双面有序阵列TPU发泡材料正面与反面的照片
图7为不同发泡压强下制备的双面有序阵列TPU发泡材料的横截面SEM照片
图8为不同发泡压强下制备的双面有序阵列TPU发泡材料的表面SEM照片
图9为基于双面有序阵列TPU发泡材料的刚性模式摩擦电纳米发电机装置结构示意图;
图10为基于双面有序阵列TPU发泡材料的柔性模式摩擦电纳米发电机装置结构示意图;
图11为基于双面有序阵列TPU发泡材料的柔性模式摩擦电纳米发电机不受力与压缩状态下的结构变化照片;
图12为基于双面有序阵列TPU发泡材料的柔性模式摩擦电纳米发电机装置用做自供能传感器来监测:(a-c)人走路习惯、频率,(d-f)落座时间、频率,(g-i)拳击力度和频率。
具体实施方式
下面结合具体实施例对本发明做进一步的详细说明。除特殊说明的之外,各实施例及试验例中所用的设备和试剂均可从商业途径得到。
实施例1
本实施例提供一种双面有序阵列发泡材料的制备方法,其工艺流程示意图如图1所示,具体操作步骤为:
1)使用无水乙醇对不锈钢网进行清洗,真空烘箱干燥后取出,使用草酸对不锈钢网进行表面处理,在模板模腔的底面铺满干燥的TPU颗粒,将处理后的不锈钢网放置在TPU颗粒表面,然后不锈钢网表面再铺满干燥的TPU颗粒,进行热压处理,其中热压温度为190℃,热压时间为10min,然后脱模得到中间层为不锈钢网的TPU复合压片,压片厚度约为0.5mm;
2)将步骤1)制备的TPU复合压片放入超临界发泡反应釜中,利用温控系统精准调控发泡釜内部温度达到120℃,采用超临界CO2供气系统调控压强至设定压强,保持高温高压2小时后,关闭进气阀,停止scCO2的注入,迅速完全打开出气阀,发泡釜内气压在极短的时间内,快速卸压至大气压强,打开发泡釜,取出制品,自然冷却至室温,即制备获得双面有序阵列TPU发泡材料。
本实施例提供的制备方法,基于受限发泡和气体定向逃逸原理,如图1和图2所示,通过真空热压处理将热塑性聚氨酯与不锈钢网紧密结合在一起,得到复合材料预制件。预制件进行超临界二氧化碳浸泡处理后,在发泡过程中不锈钢网从内部限制了CO2气体在发泡过程中的水平逸出,产生竖直方向的CO2气体定向逃逸,并且由于受限作用,竖直方向上不锈钢丝周围的气体逸出较弱,越远离不锈钢丝的气体定向逸出越强。但不锈钢网自身的强度保证了整体结构不会弯曲,整体结构维持力的平衡,所以不锈钢网格的气体呈现出反向逸出的趋势,形成双向有序阵列结构。
需要补充说明的是,步骤1)TPU复合压片的热压温度控制在180~200℃,热压时间控制在10~20min,压片厚度为0.4~0.7mm;步骤2)发泡温度控制在100~120℃,可制备获得同等性能的双面有序阵列TPU发泡材料。
实施例2
本实施例对比不同目数不锈钢网形成的双面有序阵列TPU发泡材料的形貌差异,具体为按照实施例1所述的制备方法,步骤2)中采用超临界CO2供气系统调控压强至16MPa,保持高温高压2小时,分别采用目数为14目,16目和18目的不锈钢网,制备双面有序阵列TPU发泡材料,如图3、图4和图5所示,不同目数的钢丝网制备的TPU发泡材料上下表面均能形成有序阵列的凸起结构,凸起的形状和尺寸,包括高度、相邻凸起之间的距离等,不同的目数之间存在一定的差异,钢丝网目数越大凸起的高度越低,相邻凸起之间的间隔越小。
实施例3
本实施例对比不同发泡压强条件下形成的双面有序阵列TPU发泡材料的形貌差异,具体为按照实施例1所述的制备方法,采用16目不锈钢网,步骤2)中采用超临界CO2供气系统调控压强分别至10MPa、13MPa、16MPa,制备双面有序阵列TPU发泡材料,如图6、图7和图8所示,在低于10MPa发泡压强作用下,不能产生阵列的凸起结构,发泡压强高于10MPa,例如13MPa和16MPa作用下能够形成有序的凸起阵列,并且随着发泡压强的增大凸起高度越高,但相邻凸起之间间隔基本保持不变。
实施例4
本实施例提供一种摩擦电纳米发电机装置,如图9所示,以实施例2采用16目不锈钢网制备的双面有序阵列发泡材料作为正极材料,并提供支撑,硅橡胶(Ecoflex)设置在双面有序阵列发泡材料的上下表面作为负极,双面有序阵列发泡材料中间的金属网(不锈钢网)作为电极导出电子,上下表面采用了亚克力板固定负极材料(硅橡胶),组装成刚性模式摩擦纳米发电机装置。
实施例5
本实施例一种摩擦电纳米发电机装置,如图10所示,以实施例2采用16目不锈钢网制备的双面有序阵列发泡材料作为正极材料,并提供支撑,硅橡胶(Ecoflex)设置在双面有序阵列发泡材料的上下表面作为负极,双面有序阵列发泡材料中间的金属网(不锈钢网)作为电极导出电子,采用聚酰亚胺膜封装负极材料(硅橡胶),组装成柔性模式摩擦纳米发电机装置。
本实施例提供的摩擦电纳米发电机装置,在外力作用下被压缩,如图11所示,在压缩过程中硅橡胶层受压发生变形进入双面阵列发泡材料的阵列结构内部,产生感应电荷,从而在外电路形成电流,输出电流信号,实现机械能向电能的转换,实现对外力作用的检测,如图12所示,以本实施例提供的柔性模式摩擦电纳米发电机装置作为自供能传感器能够成功检测到人体走、跑、起、坐、刺拳、直拳等不同力度、频率的活动情况,表明本发明提供的双面有序阵列TPU发泡材料组装成的摩擦电纳米发电机装置能够作为传感器结构用于检测人体活动情况,能够应用于制作人体运动监测穿戴设备。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种双面有序阵列发泡材料的制备方法,其特征在于,包括以下操作步骤:
1)将两层热塑性聚合物薄片与置于两层热塑性聚合物薄片之间的无发泡性能的硬质网格紧密结合,形成复合材料预制件;
2)将复合材料预制件进行气体发泡处理,制得所述双面有序阵列发泡材料。
2.如权利要求1所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤1)所述复合材料预制件的厚度为0.4~0.7mm。
3.如权利要求2所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤1)中无发泡性能的硬质网格的目数为14目、16目或18目。
4.如权利要求1~3任一项所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤1)中无发泡性能的硬质网格为不锈钢网。
5.如权利要求1~3任一项所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤1)中热塑性聚合物薄片为热塑性聚氨酯薄片。
6.如权利要求5所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤1)中通过热压的方式形成复合材料预制件;热压温度为180~200℃,热压时间为10~20min。
7.如权利要求5所述的双面有序阵列发泡材料的制备方法,其特征在于,步骤2)中所述的气体发泡处理为将复合材料预制件在发泡温度下与超临界CO2形成饱和稳定的共混体系后,保持一定时间,快速卸压,将发泡样品取出自然冷却至室温。
8.如权利要求7所述的双面有序阵列发泡材料的制备方法,其特征在于,发泡温度为100~120℃;饱和稳定共混体系的压强为13~16MPa;保持时间为1~2小时。
9.一种双面有序阵列发泡材料,其特征在于,由如权利要求1~8任一项所述的制备方法制备而成。
10.一种如权利要求9所述的双面有序阵列发泡材料在制作摩擦电纳米发电机方面的应用。
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