CN112046104A - 一种具有运动监测功能的柔性防刺复合材料及制备方法 - Google Patents

一种具有运动监测功能的柔性防刺复合材料及制备方法 Download PDF

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CN112046104A
CN112046104A CN202010813516.3A CN202010813516A CN112046104A CN 112046104 A CN112046104 A CN 112046104A CN 202010813516 A CN202010813516 A CN 202010813516A CN 112046104 A CN112046104 A CN 112046104A
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graphene
shear thickening
multiphase
composite material
resistant composite
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王秋实
冯燕
魏亮
董洁
孙润军
梁高勇
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Xian Polytechnic University
Institute of Quartermaster Engineering Technology Institute of Systems Engineering Academy of Military Sciences
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Abstract

本发明公开了一种具有运动监测功能的柔性防刺复合材料及其制备方法，包括三维织物预制件和石墨烯多相剪切增稠液基体，三维织物预制件为角连锁结构三维织物，石墨烯多相剪切增稠液基体原料包括石墨烯、纳米SiO2和PEG 200。将石墨烯、纳米SiO2和表面活性剂加入无水乙醇中混合，再加入PEG 200，球磨，脱泡，再置于无水乙醇中稀释混合，得到石墨烯多相剪切增稠液基体稀释液；将三维织物预制件浸渍在稀释液中，取出并使用织物压辊挤压，将经压辊挤压后的三维物预制件烘干，得到具有运动监测功能的柔性防刺复合材料。

Description

一种具有运动监测功能的柔性防刺复合材料及制备方法
技术领域
本发明智能纺织材料技术领域，涉及一种具有运动监测功能的材料，还涉及该运动监测功能的材料的制备方法。
背景技术
随着材料科学的快速发展，人们对于防刺装备的要求正逐步向轻量化、舒适化的方向发展。剪切增稠液(Shear Thickening Fluid)作为一种智能材料，在受到一定速率剪切作用时，其黏度急剧增长呈现出类似固体的物理状态，同时在液-固相变过程产生大量能量耗散，并且在外力撤出后材料仍能恢复至液体状态，因此该材料特别适宜作为基体制备柔性防刺复合材料。
然而常规单相剪切增稠液在与剪切增稠效果直接相关的剪切增稠率和剪切增稠触发条件等方面的局限性使材料在防刺性能提高上仍存在较大的提升空间。据文献报道，通过额外增加添加相制备多相剪切增稠液的方式可以获得更加显著的防刺效果，逐渐成为剪切增稠液基柔性复合材料的重要研究方向。此外，使用碳纳米管(CNTs)、石墨烯等低维碳纳米材料作为剪切增稠液的添加相还会赋予了材料独特的压阻特性，可以作为织物传感器根据织物的变形程度等条件对穿着者的运动姿态进行判断，使其在智能可穿戴材料应用领域具备良好的发展潜力。因此，研究开发使用低维碳纳米材料作为添加相制备的兼具防刺性能和运动监测功能的多功能柔性防刺复合材料在智能单兵作战装备、警用防护服等国防安全领域具有广阔的应用前景。
发明内容
本发明的目的是提供了一种具有运动监测功能的柔性防刺复合材料，该材料不仅具有优异的抵御动态穿刺的能力，还可以根据复合材料的压阻特性实现穿着者运动姿态的实时监测。
本发明的另一目的是提供一种具有运动监测功能的柔性防刺复合材料的制备方法，该制备方法简单，操作简便，且方便大规模生产。
本发明所采用的第一种技术方案是，一种具有运动监测功能的柔性防刺复合材料，包括三维织物预制件和石墨烯多相剪切增稠液基体，所述三维织物预制件为角连锁结构三维织物，所述石墨烯多相剪切增稠液基体原料包括石墨烯、纳米SiO2和PEG 200。
本发明特点还在于，
所述石墨烯为多层结构，厚度为4-10nm。
本发明所采用的第二种技术方案是，一种具有运动监测功能的柔性防刺复合材料的应用，用于碱洗脱硫，具体操作为：
步骤1：取石墨烯、纳米SiO2和表面活性剂放入无水乙醇中混合，得到石墨烯多相剪切增稠液分散相混合液；
步骤2：在步骤2得到的石墨烯多相剪切增稠液分散相混合液中加入PEG 200，球磨，得到石墨烯多相剪切增稠液基体；
步骤3：将步骤2得到的石墨烯多相剪切增稠液基体进行脱泡，再置于无水乙醇中稀释混合，得到石墨烯多相剪切增稠液基体稀释液；
步骤4：将三维织物预制件浸渍在步骤3得到的石墨烯多相剪切增稠液基体稀释液中，使用织物压辊挤压浸渍后的三维织物预制件；
步骤5：将步骤4经压辊挤压后的三维织物预制件烘干，得到具有运动监测功能的柔性防刺复合材料。
本发明的特点还在于，
步骤1石墨烯多相剪切增稠液分散相混合液中石墨烯、纳米SiO2和表面活性剂的质量分数分别为0.1-0.5％、27.5-27.9％和0.02-0.1％，石墨烯和纳米SiO2的质量分数之和为28％，混合方式为超声混合20-40min；表面活性剂为十二烷基硫酸钠。
步骤1石墨烯多相剪切增稠液基体中PEG 200的质量分数为72％，球磨时间为24-36h。
步骤3石墨烯多相剪切增稠液基体与无水乙醇的质量比为1:0.5-4，混合方式为超声混合20-40min。
步骤4中三维织物预制件的结构浅交直联，织物层数为5-15层，线密度为750D，织物有n层，n层织物的经密为200×n根/10cm，纬密为180×n根/10cm；压辊挤压压力为0.1-0.5Mpa。
步骤5压辊挤压次数为1-5次，烘干条件为在真空干燥箱中50℃烘干4h。
与现有技术相比，本发明具有以下有益效果：
(1)现有剪切增稠液体系多为单分散相体系，材料的剪切增稠效果和剪切增稠触发条件受剪切增稠液体系中纳米SiO2分散相添加量的限制，含量过高会使剪切增稠液成凝胶状，失去剪切增稠特效，且难以与织物预制件复合制备复合材料。本发明通过引入石墨烯添加项的方式，一方面突破了纳米SiO2单一分散相对体系剪切增稠性能的制约，进一步提升了剪切增稠效果，调控了剪切增稠触发条件，对剪切增稠液基织物复合材料的动态防刺性能也存在明显的增强；另一方面利用石墨烯低维碳纳米材料的导电特性使剪切增稠液基复合材料具备随材料弯曲变形程度变化呈现阻抗变化的压阻性能，从而可以根据复合材料的阻抗变化特征对柔性防刺服装穿着者的运动姿态进行判断，实现智能可穿戴的目标；
(2)本发明添加表面活性剂十二烷基硫酸钠其主要功能是辅助石墨烯和纳米SiO2的分散，从而使多相剪切增稠液的剪切增稠特征更加稳定；
(3)本发明制备的柔性防刺复合材料不仅可以在标准刀具以一定动能条件下冲击试样时，有效阻碍刀刃的刺入，并且充分耗散冲击动能，起到动态防刺功能，还可以在不同弯曲程度的变形过程中呈现出不同幅度的阻抗变化，且阻抗变化幅度与材料弯曲程度存在正相关关系，从而对人体弯腰、屈膝、曲臂等各类运动状态起到监测功能。因此在应变传感器、智能可穿戴纺织复合材料、智能单兵装备等方面都具有广阔的应用前景。
附图说明
图1为实施例3制备的具有运动监测功能的柔性防刺复合材料的表面和横截面场发射扫描电镜照片；
图2为实施例3制备的具有运动监测功能的柔性防刺复合材料的时间-动态穿刺力曲线和时间-能量耗散曲线；
图3为实施例3制备的具有运动监测功能的柔性防刺复合材料因弯曲变形程度的不同而产生的材料阻抗变化特征图。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
现详细说明本发明的多种示例性实施方式，该详细说明不应认为是对本发明的限制，而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。
应理解本发明中所述的术语仅仅是为描述特别的实施方式，并非用于限制本发明。另外，对于本发明中的数值范围，应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明，否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料，但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。本说明书中提到的所有文献通过引用并入，用以公开和描述与所述文献相关的方法和/或材料。在与任何并入的文献冲突时，以本说明书的内容为准。
在不背离本发明的范围或精神的情况下，可对本发明说明书的具体实施方式做多种改进和变化，这对本领域技术人员而言是显而易见的。由本发明的说明书得到的其他实施方式对技术人员而言是显而易见得的。本申请说明书和实施例仅是示例性的。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等，均为开放性的用语，即意指包含但不限于。
本发明中涉及原料的具体来源：
纳米二氧化硅从阿拉丁生化科技股份有限公司购入；
十二烷基硫酸钠从阿拉丁生化科技股份有限公司购入，AR，纯度≥92.5％；
PEG 200从天津市科密欧化学试剂有限公司购入，AR，纯度≥99％；
三维织物从东莞可可纺织材料有限公司购入，其中经、纬纱均使用芳纶1414长丝纱线，纱线线密度为750D。
实施例1
将质量分数为0.1％的多层石墨烯、质量分数为27.9％的纳米SiO2以及质量分数为0.02％的十二烷基硫酸钠分别加入无水乙醇溶液中，超声混合30min；再将混合液加入行星球磨机中持续研磨30h，边研磨边加入质量分数为72％的PEG 200溶液，得到混合均匀的石墨烯多相剪切增稠液基体，脱泡，再置于真空干燥箱中50℃烘干4h；烘干后的石墨烯多相剪切增稠液基体与无水乙醇按照质量比1:4混合后超声30min，得到石墨烯多相剪切增稠液基体稀释液；将经密为2000根/10cm，纬密为1800根/10cm，幅宽≥20cm的10层芳纶织物浸渍在石墨烯多相剪切增稠液基体稀释液中5min，然后使用0.5Mpa的辊压压力挤压浸渍后的三维织物，反复浸渍挤压操作3次后将三维织物置于真空干燥箱中50℃烘干4h，得到吸附率为15％的柔性防刺复合材料。
实施例2
将质量分数为0.5％的多层石墨烯、质量分数为27.7％的纳米SiO2以及质量分数为0.06％的十二烷基硫酸钠分别加入无水乙醇溶液中，超声混合30min；再将混合液加入行星球磨机中持续研磨24h，边研磨边加入质量分数为72％的PEG 200溶液，得到混合均匀的石墨烯多相剪切增稠液基体，脱泡，再置于真空干燥箱中50℃烘干4h；烘干后的石墨烯多相剪切增稠液基体与无水乙醇按照质量比1:2混合后超声20min，得到石墨烯多相剪切增稠液基体稀释液；将经密为2000根/10cm，纬密为1800根/10cm，幅宽≥20cm的10层芳纶织物浸渍在石墨烯多相剪切增稠液基体稀释液中5min，然后使用0.1Mpa的辊压压力挤压浸渍后的三维织物，反复浸渍挤压操作3次后将三维织物置于真空干燥箱中50℃烘干4h，得到吸附率为33％的柔性防刺复合材料。
实施例3
将质量分数为0.3％的多层石墨烯、质量分数为27.5％的纳米SiO2以及质量分数为0.1％的十二烷基硫酸钠分别加入无水乙醇溶液中，超声混合30min；再将混合液加入行星球磨机中持续研磨36h，边研磨边加入质量分数为72％的PEG 200溶液，得到混合均匀的石墨烯多相剪切增稠液基体，脱泡，再置于真空干燥箱中50℃烘干4h；烘干后的石墨烯多相剪切增稠液基体与无水乙醇按照质量比1:2混合后超声40min，得到石墨烯多相剪切增稠液基体稀释液；将经密为3000根/10cm，纬密为2700根/10cm，幅宽≥20cm的15层芳纶织物浸渍在石墨烯多相剪切增稠液基体稀释液中5min，然后使用0.3Mpa的辊压压力挤压浸渍后的三维织物，反复浸渍挤压操作3次后将三维织物置于真空干燥箱中50℃烘干4h，得到吸附率为33％的柔性防刺复合材料。
对所得吸附率为33％的15层浅交直联柔性防刺复合材料进行电镜扫描，结果如图1，从图1中可以看出，三维织物的表面及横截面均被多相剪切增稠液充分渗透，织物内部的纱线和纤维间隙可见大量石墨烯多相剪切增稠液基体的存在。当织物层数相同时，吸附率与织物防刺性能在一定范围内呈正相关，当吸附率达到临界值后防刺性能无明显差异。
对所得吸附率为33％的15层浅交直联柔性防刺复合材料进行动态穿刺实验得到时间-动态穿刺力、时间-能量耗散曲线如图2所示，从图中可以看出，刀受到的阻碍作用在刀刃与柔性复合材料接触过程中持续增加，由于石墨烯多相剪切增稠液基体的剪切增稠行为的触发使材料出现明显增强现象，一方面体现为材料***使动态穿刺力在5-25ms阶段出现平台期，另一方面体现在能量耗散在动态穿刺力进入平台期后迅速增加，最终达到仪器预先设定的24J的初始动能值，从而使刀具停留在复合材料中。
对所得吸附率为33％的15层浅交直联柔性防刺复合材料进行压阻性能测试，如图3所示，当材料弯曲处于伸直状态和进行不同角度的弯曲时，可以检测到材料阻抗的明显变化，并且随弯曲程度的增加，阻抗变化率逐渐增大，说明该柔性防刺复合材料具有优异的传感性能。
对比例1
将质量分数28％的纳米SiO2和质量分数为0.06％的十二烷基硫酸钠分别加入无水乙醇溶液中，超声混合30min；再将混合液加入行星球磨机中持续研磨24-36h，边研磨边加入质量分数为72％的PEG200溶液，得到混合均匀的单相剪切增稠液基体，脱泡，再置于真空干燥箱中50℃烘干4h；烘干后的单相剪切增稠液基体与无水乙醇按照质量比1:2混合后超声30min，得到单相剪切增稠液基体稀释液；将经密为3000根/10cm，纬密为2700根/10cm，幅宽≥20cm的15层三维织物浸渍在单相剪切增稠液基体稀释液中5min，然后使用0.3Mpa的辊压压力挤压浸渍后的三维织物，反复浸渍挤压操作3次后将三维织物置于真空干燥箱中50℃烘干4h，得到吸附率为33％的柔性防刺复合材料。
对所得吸附率为33％的柔性防刺复合材料进行动态力学性能和压阻性能测试，实验结果表明材料由于没有添加石墨烯不仅穿刺力和穿刺耗能存在不同程度的降低，而且在材料弯曲变形过程中未出现随变形程度变化而呈现的阻抗特征变化，因此未添加石墨烯的单相剪切增稠液基三维织物增强复合材料不仅动态防刺性能减弱而且不具备运动监测功能。
对比例2
将质量分数为0.3％的多层石墨烯、质量分数为27.7％的纳米SiO2分别加入无水乙醇溶液中，超声混合30min；再将混合液加入行星球磨机中持续研磨24-36h，边研磨边加入质量分数为72％的PEG 200溶液，得到混合均匀的石墨烯多相剪切增稠液基体，脱泡，再置于真空干燥箱中50℃烘干4h；烘干后的石墨烯多相剪切增稠液基体与无水乙醇按照质量比1:2混合后超声30min，得到石墨烯多相剪切增稠液基体稀释液；将经密为3000根/10cm，纬密为2700根/10cm，幅宽≥20cm的15层三维织物浸渍在单相剪切增稠液基体稀释液中5min，然后使用0.3Mpa的辊压压力挤压浸渍后的三维织物，反复浸渍挤压操作3次后将三维织物置于真空干燥箱中50℃烘干4h，得到吸附率为33％的柔性防刺复合材料。
对所得吸附率为33％的柔性防刺复合材料进行动态穿刺实验和压阻性能测试，实验结果表明复合材料由于没有添加表面活性剂，石墨烯多相剪切增稠液基体中分散相分散不均匀，材料的最大穿刺力、穿刺耗能值均存在不同程度的降低，并且当材料进行不同程度的弯曲变形时，阻抗变化规律较为杂乱，不利于对材料变形状态进行定量分析。
对比例3
同实施例3，区别在于，添加相为石墨。
结果发现制备的多相剪切增稠液的剪切增稠效果和剪切增稠触发条件未出现明显变化，且制备得到的复合材料动态防刺性能也未呈现明显增强，此外虽然石墨的添加使多相剪切增稠液体系导电性能增强，但是压阻性能不显著。
对比例4
同实施例3，区别在于，所述石墨烯质量分数为0.8％，纳米SiO2质量分数为27.2％，十二烷基硫酸钠质量分数为0.06％。
结果发现制备的材料呈胶状且失去剪切增稠特性，无法与织物预制件复合制备复合材料。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (8)

1.一种具有运动监测功能的柔性防刺复合材料，其特征在于，包括三维织物预制件和石墨烯多相剪切增稠液基体，所述三维织物预制件为角连锁结构三维织物，所述石墨烯多相剪切增稠液基体原料包括石墨烯、纳米SiO2和PEG 200。
2.根据权利要求1所述的一种具有运动监测功能的柔性防刺复合材料，其特征在于，所述石墨烯为多层结构，厚度为4-10nm。
3.一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，用于碱洗脱硫，具体操作为：
步骤1：取石墨烯、纳米SiO2和表面活性剂放入无水乙醇中混合，得到石墨烯多相剪切增稠液分散相混合液；
步骤2：在步骤2得到的石墨烯多相剪切增稠液分散相混合液中加入PEG 200，球磨，得到石墨烯多相剪切增稠液基体；
步骤3：将步骤2得到的石墨烯多相剪切增稠液基体进行脱泡，再置于无水乙醇中稀释混合，得到石墨烯多相剪切增稠液基体稀释液；
步骤4：将三维织物预制件浸渍在步骤3得到的石墨烯多相剪切增稠液基体稀释液中，使用织物压辊挤压浸渍后的三维织物预制件；
步骤5：将步骤4经压辊挤压后的三维织物预制件烘干，得到具有运动监测功能的柔性防刺复合材料。
4.根据权利要求3所述的一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，步骤1所述石墨烯多相剪切增稠液分散相混合液中石墨烯、纳米SiO2和表面活性剂的质量分数分别为0.1-0.5％、27.5-27.9％和0.02-0.1％，石墨烯和纳米SiO2的质量分数之和为28％，所述混合方式为超声混合20-40min；所述表面活性剂为十二烷基硫酸钠。
5.根据权利要求3所述的一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，步骤1所述石墨烯多相剪切增稠液基体中PEG 200的质量分数为72％，球磨时间为24-36h。
6.根据权利要求3所述的一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，步骤3所述石墨烯多相剪切增稠液基体与无水乙醇的质量比为1:0.5-4，所述混合方式为超声混合20-40min。
7.根据权利要求4所述的一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，步骤4中三维织物预制件的结构浅交直联，织物层数为5-15层，线密度为750D，织物有n层，n层织物的经密为200×n根/10cm，纬密为180×n根/10cm；所述压辊挤压压力为0.1-0.5Mpa。
8.根据权利要求3所述的一种具有运动监测功能的柔性防刺复合材料的制备方法，其特征在于，步骤5所述压辊挤压次数为1-5次，所述烘干条件为在真空干燥箱中50℃烘干4h。
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CN113956847B (zh) * 2021-10-19 2023-08-08 北京理工大学重庆创新中心 一种防爆液及其制备方法
CN114250629A (zh) * 2021-12-02 2022-03-29 西安工程大学 一种智能防刺面料的制备方法及其产品和应用

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