CN114550999B - 一种多层皮芯结构的电化学红外调控纤维的连续化制备方法 - Google Patents
一种多层皮芯结构的电化学红外调控纤维的连续化制备方法 Download PDFInfo
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Abstract
本发明涉及一种多层皮芯结构的电化学红外调控纤维的连续化制备方法。该制备方法包括:利用放线器与导线器,连续传送芯电极进入电解质分散液中涂覆电解质分散液,然后刮膜,加热固化,通过导线器进入红外调控材料分散液中连续涂覆红外调控材料分散液,然后刮膜,加热固化,熔融挤出包覆聚合物保护层。该纤维器件结构简单,电解质层和红外调控层厚度可控,纤维表面涂覆层均匀,可实现连续化制备,温度调控效果优异,能够应用在热管理、红外伪装以及智能服装领域。
Description
技术领域
本发明属于红外调控技术领域,特别涉及一种多层皮芯结构的电化学红外调控纤维的连续化制备方法。
背景技术
红外调控技术可用于智能窗、光通信、军用伪装和热控制等领域,近些年受到越来越多的关注。例如,近红外材料红外调控器件可以调节透射NIR辐射的强度,这将在智能热控方面有广泛的应用价值;中红外调控材料具有在红外探测器中伪装的热调节能力,在军事红外自适应伪装具有巨大的应用潜力;此外中红外电致变色器件用于控制航天器的发射率,从而适应太空环境中的温度波动。
基于红外调控纤维在具有红外辐射可控性的基础上兼备一维结构优势,是制备智能红外管理服装的基础结构单元,在实现人体热舒适与红外伪装方向具有巨大的应用前景。目前,大多数红外调控器件的制备仍然局限于平面柔性器件,平面器件与纤维器件相比在透气性、透湿性、湿热舒适性以及耐磨性等方面都有较大的差距,并不适用于智能服装的应用。并且,随着红外调控器件研究的不断深入,越来越多的问题出现:(1)大多数电致变色材料表现出可见光和近红外的电致变色特性,目前只有少数电致变色材料具有用于热调节的中红外电致变色能力,在中红外电致变色新材料仍需开发;(2)由于红外调控器件的多层结构导致纤维化困难,到目前为止关于红外调控器件纤维化的相关报道仍然较少,并且制备连续长纤维还存在大量工艺与技术难题。
Ergoktas等人(Nano Letters.2020,20(7):5346-52.)将涂覆有石墨烯的薄膜以手工缠绕的形式制备成了石墨烯红外调控纤维。通过棉制纺织品吸附离子液体作为电解质层,制备的红外调控纤维在70℃的背景温度下可以实现14℃温度范围的调控效果。但是这种红外调控纤维器件只能手工制备,生产效率低。此外,这种纤维器件没有聚合物保护层,不能在复杂的环境条件下应用。
发明内容
本发明所要解决的技术问题是提供一种多层皮芯结构的电化学红外调控纤维的连续化制备方法,以克服现有可见光调控纤维在红外光波段无调控效果和不能连续化制备的缺陷。本发明红外调控纤维器件结构简单,调控温度宽,响应时间快。
本发明提供一种多层皮芯结构的电化学红外调控纤维,所述调控纤维为:在芯电极表面依次包覆电解质层、红外调控层、聚合物保护层,其中,所述红外调控层又作为外层导电层。
优选地,所述芯电极为金属丝、导电纱线中的一种。
优选地,所述芯电极为镍包铜金属芯电极。
优选地,所述芯电极的直径为20~2000μm。
优选地,所述电解质层电解质材料包括:锂盐或离子液体,以及聚合物。
优选地,所述电解质层厚度为10~1000μm。
优选地,所述锂盐包括双三氟甲磺酰亚胺锂LiTFSI、高氯酸锂LiClO4、四氟硼酸锂LiBF4、六氟砷酸锂LiAsF6、六氟磷酸锂LiPF6中的一种或几种。
优选地,所述离子液体包括三丁基甲基铵双三氟甲磺酰亚胺盐TBMA-TFSI、1-丁基-3-甲基咪唑四氟硼酸盐BMI-BF4、1-乙基-3-甲基咪唑三氟乙酸盐EMIm-TfA、1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐EMI-TFSI中的一种或几种。
优选地,所述聚合物包括聚偏氟乙烯PVDF、聚甲基丙烯酸甲酯PMMA、聚氨酯TPU、纤维素中的一种或几种。
优选地,所述红外调控层红外调控材料包括单壁碳纳米管、多壁碳纳米管、酸化碳纳米管、羧基碳纳米管、氨基碳纳米管、氧化钒、氧化钨中的一种或几种。
优选地,所述红外调控层厚度为0.05μm~100μm。
优选地,所述聚合物保护层聚合物为红外透明的聚合物,所述红外透明的聚合物为聚乙烯。
优选地,所述聚合物保护层厚度为50~400μm。
本发明还提供一种多层皮芯结构的电化学红外调控纤维的连续化制备方法,包括以下步骤:
(1)将电解质材料溶解于有机溶剂,搅拌,得到电解质分散液,利用放线器与导线器,连续传送芯电极进入电解质分散液中涂覆电解质分散液,然后刮膜,加热固化,得到表面涂有电解质层的纤维;
(2)将步骤(1)中表面涂有电解质层的纤维通过导线器进入红外调控材料分散液中连续涂覆红外调控材料分散液,然后刮膜,加热固化,得到涂有红外调控层的初级红外调控纤维,其中,红外调控层又作为外层导电层;
(3)通过导线器将步骤(2)中涂有红外调控层的初级红外调控纤维连续熔融挤出包覆聚合物保护层,冷却,得到多层皮芯结构的电化学红外调控纤维。
优选地,所述步骤(1)中有机溶剂为碳酸丙烯酯PC。
优选地,所述步骤(1)中电解质分散液中锂盐或离子液体与有机溶剂质量比为1:9~10:0,聚合物含量为10wt.%~80wt.%。
优选地,所述步骤(1)中涂覆电解质分散液速度为30~300m/h。
优选地,所述步骤(1)中刮膜采用孔径为30~3000μm的刮膜圈。
优选地,所述步骤(1)中加热温度为90~200℃。
优选地,所述步骤(2)中红外调控材料分散液是将红外调控材料与有机溶剂混合,超声分散1~6h获得。
优选地,所述步骤(2)中红外调控材料分散液浓度为0.1~5mg/ml。
优选地,所述步骤(2)中刮膜采用孔径为30~3000μm的刮膜圈。
优选地,所述步骤(2)中加热温度为60~160℃。
优选地,所述步骤(3)中熔融挤出包覆聚合物保护层是采用熔融包覆装置,所述熔融包覆装置包括螺杆挤出机、冷却槽;其中熔融温度为150~240℃,冷却槽中为循环水。
本发明还提供一种多层皮芯结构的电化学红外调控纤维制备的连续化设备包括:放线器、导线器、电解质分散液槽、加热装置A、红外调控材料分散液槽、加热装置B、刮膜圈、熔融包覆装置、冷却装置、收线器;其中通过放线器和导线器将芯电极依次通过电解质分散液槽、刮膜圈、加热装置A,然后通过导线器依次通过红外调控材料分散液槽、刮膜圈、加热装置B,再次依次通过红外调控材料分散液槽、刮膜圈、加热装置B,然后通过导线器依次进入熔融包覆装置、冷却装置、收线器。
本发明还提供一种多层皮芯结构的电化学红外调控纤维在热管理、红外伪装或智能服装中的应用。
本发明电解质层厚度与红外调控层厚度通过控制分散液浓度与刮膜圈孔径控制。
本发明电化学红外调控纤维中的红外调控层与外电极可以通过一体化制备有效的实现。
本发明制备的多层皮芯结构电化学红外调控纤维不仅拥有优异的温度调控能力,而且通过优化制备工艺条件和结合保护层的制备实现了红外调控纤维的连续化制备。
有益效果
(1)本发明中单壁碳纳米管、多壁碳纳米管、酸化碳纳米管、羧基碳纳米管、氨基碳纳米管或氧化钨纳米线等红外调控材料除了作为红外调控层外,还可作为外电极,红外调控层与外电极的一体化形式简化了纤维器件结构,通过简单的逐层涂覆法,利用连续设备实现了红外调控纤维的连续化生产。
(2)本发明利用刮膜圈孔径的设计可以控制电解质与红外调控层的厚度,克服了连续化涂覆红外调控纤维不均匀的问题。
(3)本发明通过外电极与红外调控层结构的融合,强化电子/离子在轴向与径向三维空间上的传输效率与可控性,实现红外调控纤维的长程可控与加工。
(4)本发明制备得到的红外调控纤维表面涂覆层均匀、可实现几百米的连续化制备,工艺简单,红外调控纤维温度调控效果优异,响应时间快,能够应用在热管理、红外伪装以及智能服装领域。
附图说明
图1为实施例1连续化制备的红外调控纤维的数码照片;
图2为本发明红外调控纤维连续化制备设备的结构示意图,其中1为放线器,2为导线器,3为电解质分散液槽,4为刮膜圈,5为加热装置A,6为红外调控材料分散液槽,7为加热装置B,8为熔融包覆装置,9为冷却装置,10为收线器。
图3为实施例1连续化制备的红外调控纤维的扫描电镜照片。
图4为实施例1制备的红外调控纤维的显微红外热成像照片;其中(a)为施加+3V外加电压,(b)为施加-3V外加电压。
图5为实施例1制备的红外调控纤维在正负电压测试过程中,热成像探测的纤维表面实时温度变化曲线。
图6为实施例1制备的红外调控纤维的应力-应变曲线。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
聚偏氟乙烯PVDF购于法国阿科玛公司。聚氨酯TPU购于顺捷塑料有限公司。双三氟甲磺酰亚胺锂LiTFSI、四氟硼酸锂LiBF4、购于默克sigma公司。N-甲基吡咯烷酮NMP、碳酸丙烯酯PC购于国药集团化学试剂有限公司。碳纳米管由中国科学院成都有机化学有限公司提供。镍包铜金属纤维由科炎光电有限公司提供。三丁基甲基铵双三氟甲磺酰亚胺盐TBMA-TFSI、1-丁基-3-甲基咪唑四氟硼酸盐BMI-BF4购于默尼化工(上海)有限公司提供。
使用FLIR A300型号热成像仪进行红外热成像测试,测试时基底温度条件为50℃,环境温度条件为21℃。
实施例1
称取18g碳酸丙烯酯PC和2g三丁基甲基铵双三氟甲磺酰亚胺盐TBMA-TFSI(溶剂与离子液体质量比为9:1)在室温下搅拌均匀,然后称取20g聚偏氟乙烯PVDF(50wt.%)加入混合溶液中,继续搅拌至悬浮液均匀后,得到固态电解质前驱体溶液。称取10mg单壁碳纳米管和100ml N-甲基吡咯烷酮NMP溶液,在30℃温度下超声分散1h,搅拌均匀后制备成红外调控材料悬浮液。
利用图2所示的设备进行红外调控纤维连续化制备,首先通过放线器1将直径300μm镍包铜金属芯电极以300m/h的速度转动,芯电极通过导线器2进入电解质分散液槽3(装有上述固态电解质前驱体溶液)中,然后涂有电解质的芯电极经过直径500μm刮膜圈4后利用导线器进入加热装置A 5,加热温度设置为200℃;接下来电解质固化的涂有电解质的纤维经过导线器2进入红外调控材料分散液槽6(装有上述红外调控材料悬浮液)中,再经过800μm刮膜圈4后利用导线器进入加热装置B 7,加热温度设置为160℃;接着利用导线器2将纤维再次进入红外调控材料分散液槽6中,经过1000μm刮膜圈4后利用导线器2再次进入加热装置B 7,得到涂有红外调控层的初级红外调控纤维。
利用导线器将初级红外调控纤维导入熔融包覆装置8包覆聚乙烯PE保护层,之后纤维进入冷却装置9,包覆层厚度通过控制给料速度将厚度保持为100μm;之后经过收线器10收集制备好的红外调控纤维,其中熔融包覆装置8包括螺杆挤出机、冷却槽,熔融温度为160℃,冷却槽中为循环水。
上述制备的红外调控纤维在50℃的基底温度下,未施加电压时纤维的表面温度为39.0℃左右,如图4所示,施加+3V外加电压纤维温度下降至34.4℃,施加-3V外加电压纤维温度上升至40.6℃,温度调控范围达到6.2℃;如图3所示扫描显微镜SEM照片显示纤维表面平整光滑。如图5所示,由低发射状态向高发射状态转换施加电压时间为30s;由高发射状态向低发射状态转换施加电压时间为15s。如图6所示,红外调控纤维的拉伸强度为34.8MPa。
实施例2
称取8g三丁基甲基铵双三氟甲磺酰亚胺盐TBMA-TFSI(溶剂与离子液体质量比为0:1)在室温下搅拌均匀,然后称取32g聚偏氟乙烯PVDF(80wt.%)加入混合溶液中,继续搅拌至悬浮液均匀后,得到固态电解质前驱体溶液。称取10mg酸化碳纳米管加入到100ml NMP溶液,在30℃的冰水浴中超声分散6h,搅拌均匀后制备成红外调控材料悬浮液。
利用图2所示的设备进行红外调控纤维连续化制备,首先通过放线器1将直径300μm镍包铜金属芯电极以30m/h的速度转动,芯电极通过导线器2进入电解质分散液槽3(装有上述固态电解质前驱体溶液)中,然后涂有电解质的芯电极经过直径500μm刮膜圈4后利用导线器进入加热装置A 5,加热温度设置为110℃;接下来电解质固化的涂有电解质的纤维经过导线器2进入红外调控材料分散液槽6(装有上述红外调控材料悬浮液)中,再经过600μm刮膜圈后利用导线器进入加热装置B 7,加热温度设置为160℃;接着利用导线器将纤维再次进入红外调控材料分散液槽6中,经过800μm刮膜圈4后利用导线器2再次进入加热装置B7,得到涂有红外调控层的初级红外调控纤维。
利用导线器将初级红外调控纤维导入熔融包覆装置8包覆聚乙烯PE保护层,之后纤维进入冷却装置9,包覆层厚度通过控制给料速度将厚度保持为200μm;之后经过收线器10收集制备好的红外调控纤维,其中熔融包覆装置8包括螺杆挤出机、冷却槽,熔融温度为160℃,冷却槽中为循环水。
上述制备的红外调控纤维在50℃的基底温度下,未施加电压时纤维的表面温度为39℃左右,施加+3V外加电压纤维温度下降至34.5℃,施加-3V外加电压纤维温度上升至49.8℃,由于保护层厚度增加导致温度调控范围下降到5.3℃。由于纤维在涂覆红外调控层时经过的刮膜圈变小,涂覆的红外调控层厚度下降,导致由低发射状态向高发射状态转换施加电压时间增加为50s;由高发射状态向低发射状态转换时间电压时间增加为30s。
实施例3
称取18g碳酸丙烯酯PC(10wt.%)和18g 1-丁基-3-甲基咪唑四氟硼酸盐BMI-BF4(溶剂与离子液体质量比为1:1),然后称取4g聚氨酯TPU(10wt.%)加入混合溶液中,继续搅拌至悬浮液均匀后,得到固态电解质前驱体溶液。称取10mg多壁碳纳米管和10mg氧化钨,然后加入到100ml NMP溶液,在30℃的冰水浴中超声分散6h,搅拌均匀后制备成红外调控材料悬浮液。
利用图2所示的设备进行红外调控纤维连续化制备,首先通过放线器1将直径2000μm镍包铜金属芯电极以100m/h的速度转动,首先芯电极通过导线器2进入电解质分散液槽3(装有上述固态电解质前驱体溶液)中,然后涂有电解质的芯电极经过直径2200μm刮膜圈4后利用导线器进入加热装置A5,加热温度设置为160℃;接下来电解质固化的涂有电解质的纤维经过导线器进入红外调控材料分散液槽6(装有上述红外调控材料悬浮液)中,再经过2500μm刮膜圈4后利用导线器进入加热装置B 7,加热温度设置为60℃;接着利用导线器将纤维再次进入红外调控材料分散液槽6中,经过3000μm刮膜圈4后利用导线器2再次进入加热装置B 7,得到涂有红外调控层的初级红外调控纤维。
利用导线器将初级红外调控纤维导入熔融包覆装置8包覆聚乙烯PE保护层,之后纤维进入冷却装置9,包覆层厚度通过控制给料速度将厚度保持为200μm;之后经过收线器收集制备好的红外调控纤维,其中熔融包覆装置8包括螺杆挤出机、冷却槽,熔融温度为200℃,冷却槽中为循环水。
实施例4
称取18g碳酸丙烯酯PC和18g双三氟甲磺酰亚胺锂LiTFSI(溶剂与锂盐质量比为1:1),然后称取4g聚偏氟乙烯PVDF(10wt.%)加入混合溶液中,继续搅拌至悬浮液均匀后,得到固态电解质前驱体溶液。称取10mg羧基碳纳米管,然后加入到100ml NMP溶液,在0℃的冰水浴中超声分散3h,搅拌均匀后制备成红外调控材料悬浮液。
利用图2所示的设备进行红外调控纤维连续化制备,首先通过放线器1将直径100μm镍包铜金属芯电极以300m/h的速度转动,首先芯电极通过导线器2进入电解质分散液槽3(装有上述固态电解质前驱体溶液)中,然后涂有电解质的芯电极经过直径200μm刮膜圈4后利用导线器进入加热装置A 5,加热温度设置为160℃;接下来电解质固化的涂有电解质的纤维经过导线器2进入红外调控材料分散液槽6(装有上述红外调控材料悬浮液)中,再经过300μm刮膜圈4后利用导线器进入加热装置B 7,加热温度设置为160℃;接着利用导线器2将纤维再次进入红外调控材料分散液槽6中,经过450μm刮膜圈后利用导线器再次进入加热装置B 7,得到涂有红外调控层的初级红外调控纤维。
利用导线器将初级红外调控纤维导入熔融包覆装置8包覆聚乙烯PE保护层,之后纤维进入冷却装置9,包覆层厚度通过控制给料速度将厚度保持为100μm;之后经过收线器10收集制备好的红外调控纤维,其中熔融包覆装置8包括螺杆挤出机、冷却槽,熔融温度为240℃,冷却槽中为循环水。
实施例5
称取18g碳酸丙烯酯PC和2g四氟硼酸锂LiBF4(溶剂与锂盐质量比为9:1),然后称取20g聚氨酯TPU(50wt.%)加入混合溶液中,继续搅拌至悬浮液均匀后,得到固态电解质前驱体溶液。称取10mg单壁碳纳米管和10mg氧化钒,然后加入到100ml NMP溶液,在0℃的冰水浴中超声分散3h,搅拌均匀后制备成红外调控材料悬浮液。
利用图2所示的设备进行红外调控纤维连续化制备,首先通过放线器1将直径20μm镍包铜金属芯电极以30m/h的速度转动,首先芯电极通过导线器2进入电解质分散液槽3(装有上述固态电解质前驱体溶液)中,然后涂有电解质的芯电极经过直径30μm刮膜圈4后利用导线器进入加热装置A 5,加热温度设置为140℃;接下来电解质固化的涂有电解质的纤维经过导线器2进入红外调控材料分散液槽6(装有上述红外调控材料悬浮液)中,再经过40μm刮膜圈4后利用导线器进入加热装置B 7,加热温度设置为160℃;接着利用导线器2将纤维再次进入红外调控材料分散液槽6中,经过50μm刮膜圈4后利用导线器2再次进入加热装置B7,得到涂有红外调控层的初级红外调控纤维。
利用导线器将初级红外调控纤维导入熔融包覆装置8包覆聚乙烯PE保护层,之后纤维进入冷却装置9,包覆层厚度通过控制给料速度将厚度保持为50μm;之后经过收线器10收集制备好的红外调控纤维,其中熔融包覆装置8包括螺杆挤出机、冷却槽,熔融温度为150℃,冷却槽中为循环水。
Claims (9)
1.一种多层皮芯结构的电化学红外调控纤维,其特征在于,所述调控纤维为:在芯电极表面依次包覆电解质层、红外调控层、聚合物保护层,其中,所述红外调控层又作为外层导电层;
所述电解质层电解质材料为:锂盐或离子液体,以及聚合物;所述锂盐为双三氟甲磺酰亚胺锂LiTFSI、高氯酸锂LiClO4、四氟硼酸锂LiBF4、六氟砷酸锂LiAsF6、六氟磷酸锂LiPF6中的一种或几种;离子液体为三丁基甲基铵双三氟甲磺酰亚胺盐TBMA-TFSI、1-丁基-3-甲基咪唑四氟硼酸盐BMI-BF4、1-乙基-3-甲基咪唑三氟乙酸盐EMIm-TfA、1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐EMI-TFSI中的一种或几种;聚合物为聚偏氟乙烯PVDF、聚甲基丙烯酸甲酯PMMA、聚氨酯TPU、纤维素中的一种或几种;
所述红外调控层红外调控材料为单壁碳纳米管、多壁碳纳米管、酸化碳纳米管、羧基碳纳米管、氨基碳纳米管、氧化钒、氧化钨中一种或几种;
所述聚合物保护层聚合物为红外透明的聚合物,所述红外透明的聚合物为聚乙烯。
2. 根据权利要求1所述的电化学红外调控纤维,其特征在于,所述芯电极为金属丝、导电纱线中的一种;芯电极的直径为20~2000 μm;电解质层厚度为10~1000 μm。
3. 根据权利要求1所述的电化学红外调控纤维,其特征在于,所述红外调控层厚度为0.05 μm~100 μm。
4. 根据权利要求1所述的电化学红外调控纤维,其特征在于,所述聚合物保护层厚度为50~400 μm。
5.一种如权利要求1所述的多层皮芯结构的电化学红外调控纤维的连续化制备方法,包括以下步骤:
(1)将电解质材料溶解于有机溶剂,搅拌,得到电解质分散液,利用放线器与导线器,连续传送芯电极进入电解质分散液中涂覆电解质分散液,然后刮膜,加热固化,得到表面涂有电解质层的纤维;
(2)将步骤(1)中表面涂有电解质层的纤维通过导线器进入红外调控材料分散液中连续涂覆红外调控材料分散液,然后刮膜,加热固化,得到涂有红外调控层的初级红外调控纤维,其中红外调控层又作为外层导电层;
(3)通过导线器将步骤(2)中涂有红外调控层的初级红外调控纤维连续熔融挤出包覆聚合物保护层,冷却,得到多层皮芯结构的电化学红外调控纤维。
6. 根据权利要求5所述的连续化制备方法,其特征在于,所述步骤(1)中有机溶剂为碳酸丙烯酯PC;电解质分散液中锂盐或离子液体与有机溶剂质量比为1:9~10:0,聚合物含量为10 wt.%~80 wt.%。
7. 根据权利要求5所述的连续化制备方法,其特征在于,所述步骤(1)中涂覆电解质分散液速度为30~300 m/h;刮膜采用孔径为30~3000 μm的刮膜圈;加热温度为90~200℃。
8. 根据权利要求5所述的连续化制备方法,其特征在于,所述步骤(2)中红外调控材料分散液浓度为0.1~5 mg/ml;刮膜采用孔径为30~3000 μm的刮膜圈;加热温度为60~160℃。
9.一种如权利要求1所述的多层皮芯结构的电化学红外调控纤维在热管理、红外伪装或智能服装中的应用。
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