CN107475840B - 一种可拉伸电热致变色纤维及其制备方法 - Google Patents

一种可拉伸电热致变色纤维及其制备方法 Download PDF

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CN107475840B
CN107475840B CN201710743290.2A CN201710743290A CN107475840B CN 107475840 B CN107475840 B CN 107475840B CN 201710743290 A CN201710743290 A CN 201710743290A CN 107475840 B CN107475840 B CN 107475840B
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王宏志
李强
李克睿
范宏伟
侯成义
李耀刚
张青红
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Donghua University
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Abstract

本发明涉及一种可拉伸电热致变色纤维,以包芯纱作为弹性基体,在其表面依次制备导电层、保护层以及变色层;制备方法包括包芯纱的预处理,多层氧化石墨烯修饰的包芯纱的合成,多层石墨烯修饰的包芯纱的合成,可拉伸电热致变色纤维的合成。本发明的方法简单,条件温和,成本低,适合规模化生产;本发明得到的可拉伸电热致变色纤维可以实现多种颜色的变化,具有良好的导电性和循环稳定性,同时表现出优异的可拉伸性能,为纤维功能化和智能化提供了基础,在军事伪装、智能可穿戴以及视觉传感器等方面展现出巨大的应用价值。

Description

一种可拉伸电热致变色纤维及其制备方法
技术领域
本发明属于变色纤维领域,特别涉及一种可拉伸电热致变色纤维及其制备方法。
背景技术
变色纤维是一种具有特殊组成或结构的,在受到光、电、磁、热、水分或辐射等外界条件刺激后可以改变颜色的纤维。变色纤维最早应用在1970年的越南战争的战场上,美国的Cyanamide公司为满足美军对作战服装的要求而开发的一种光致变色纤维,这类纤维可以吸收光线后改变颜色。此后不同机制的变色纤维不断发展,主要包括热致变色、电致变色、磁致变色、光致变色、湿致变色等,在智能可穿戴、军事伪装、柔性显示器等方面展现出巨大的潜力。
近年来,随着可穿戴技术的发展,可拉伸智能变色纤维已成为热门话题。电致变色通过控制电流或者电压的大小来实现纤维颜色的转变,是一种更容易、更可控的方法。电致变色纤维一般为多层结构,包含变色层,电解质层以及电极层。然而,复杂的多层结构导致电致变色纤维的拉伸在制备上比较困难,性能较差;这种复杂的结构以及对电极的使用也使纤维几乎不可拉伸,限制了其在可穿戴领域的发展。因此,迫切需要寻找一种新的方法制备出可拉伸智能变色纤维。
相对于电致变色纤维而言,电热致变色纤维具有更加简单的结构、更丰富的颜色以及更加令人满意的拉伸性能。在不拉伸状态下,通过外加电场的刺激,能实现可控、可逆的颜色转变。同时,在不同程度的拉伸下,纤维电阻也随之变化,在较小电流下即可实现颜色的改变。选择不同颜色和转变温度的热致变色材料,能实现多种颜色的转变。这类可拉伸电热致变色纤维能够与传统的针织、或者编织工艺相结合,为纤维的功能化智能化以及可穿戴领域的发展提供一种新的并且十分有效的方案。
发明内容
本发明所要解决的技术问题是提供一种可拉伸电热致变色纤维及其制备方法,该方法简单,成本低,适合规模化生产;制备得到的可拉伸电热致变色纤维具有良好的导电性、循环稳定性、可拉伸性和变色性。
本发明的一种可拉伸电热致变色纤维,以包芯纱作为弹性基体,在其表面依次制备导电层、保护层以及变色层。
所述包芯纱为双层结构,包芯纱包括芯层和表层,芯层为聚氨酯纤维,表层为螺旋状聚乙烯纤维。
本发明的一种可拉伸电热致变色纤维的制备方法,具体步骤如下:
(1)将包芯纱预处理得到处理后的包芯纱;
(2)将步骤(1)中处理后的包芯纱放到氧化石墨烯分散液中浸泡,干燥,得到单层氧化石墨烯修饰的包芯纱,其中处理后的包芯纱与氧化石墨烯的质量比为0.04:1~0.05:1;
(3)用步骤(2)中的单层氧化石墨烯修饰的包芯纱重复步骤(2)多次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱释放预拉伸后,置于氢碘酸中反应,得到多层石墨烯修饰的包芯纱,其中多层氧化石墨烯修饰的包芯纱与氢碘酸的质量比为1:315~1:330;
(4)将聚二甲基硅氧烷PDMS与固化剂以质量比为6:1~10:1混合,搅拌,静置,得到混合剂,将步骤(3)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,固化,得到固化后的多层石墨烯修饰的包芯纱,其中PDMS与多层石墨烯修饰的包芯纱的质量比为420:1~432:1,在固化后的多层石墨烯修饰的包芯纱上浸涂热致变色油墨,再固化,得到可拉伸电热致变色纤维,其中热致变色油墨与固化后的多层石墨烯修饰的包芯纱的质量比为139:1~145:1。
所述步骤(1)中包芯纱预处理的具体步骤为:将包芯纱分别置于去离子水、丙酮和乙醇中超声,烘干,等离子体处理15min后进行预拉伸。
所述超声时间为10~30min;预拉伸的比为10~50%。
所述步骤(2)中氧化石墨烯分散液的制备方法为:将氧化石墨烯溶解在水中,超声,得到氧化石墨烯分散液,氧化石墨烯分散液的浓度为5mg/mL。
所述步骤(2)中浸泡时间为5~10s。
所述步骤(3)中多次为5~40;反应时间为2~4h。
所述步骤(4)中固化温度为60~90℃,固化时间为60~120min;再固化温度为60~80℃,再固化时间为30~90min。
所述步骤(4)中热致变色油墨为45℃热致变色油墨,变色时间为15s,褪色时间为10s,多次重复此行为(>1000次),热致变色油墨性能未出现衰减现象。
所述步骤(4)中可拉伸电热致变色纤维在拉伸状态下,施加10mA电流,温度为47.9℃,其颜色变化为黑色到绿色。
本发明的一种可拉伸电热致变色纤维的制备方法,将拉伸性能好,具有双层结构的包芯纱作为弹性支架,在包芯纱表面负载导电性能和导热性能好的石墨烯作为导电层,然后涂覆PDMS作为保护层,防止石墨烯脱落和滑动,最后涂覆不同种类的热致变色油墨来实现多种变色效果。
有益效果
(1)本发明的方法简单,条件温和,成本低,适合规模化生产;
(2)本发明得到的可拉伸电热致变色纤维,可以实现多种颜色的变化,具有良好的导电性和循环稳定性,同时表现出优异的可拉伸性能,为纤维功能化和智能化提供了基础,在军事伪装、智能可穿戴以及视觉传感器等方面展现出巨大的应用价值。
附图说明
图1是实施例1中制备的可拉伸电热致变色纤维的结构示意图;
图2是实施例1中制备的可拉伸电热致变色纤维的断面扫描电镜图;
图3是实施例1中制备的可拉伸电热致变色纤维的相对电阻变化曲线;
图4是实施例1中制备的可拉伸电热致变色纤维变色的数码照片;
图5是实施例1中制备的可拉伸电热致变色纤维在不同拉伸状态下的反射光谱;
图6是实施例1中制备的可拉伸电热致变色纤维在不同拉伸程度下的温度时间曲线。
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。
实施例1
(1)将500mg氧化石墨烯粉末溶解在100mL去离子水中,用超声波细胞粉碎机超声1h,得到呈棕色的氧化石墨烯分散液。
(2)将包芯纱(0.0226g)分别置于去离子水、丙酮和乙醇中超声15min,烘干,将其等离子体处理15min后预拉伸40%,得到处理后的包芯纱。
(3)将步骤(2)中处理后的包芯纱(0.0227g)放到步骤(1)中氧化石墨烯分散液中浸泡8s,取出用吹风机吹干,得到单层氧化石墨烯修饰的包芯纱。
(4)用步骤(3)中的单层氧化石墨烯修饰的包芯纱重复步骤(3)30次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱(0.02335g)释放预拉伸后,置于氢碘酸(7.5g)中浸泡4h,得到多层石墨烯修饰的包芯纱(0.02332g)。
(5)将聚二甲基硅氧烷PDMS 10g与固化剂1g混合,搅拌30min,静置2h,得到混合剂,将步骤(4)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,待PDMS与纤维表面完全接触后,取出在70℃下固化90min,得到固化后的多层石墨烯修饰的包芯纱,将固化后的多层石墨烯修饰的包芯纱(0.03536g)通过5.0g的45℃热致变色油墨并使其浸涂均匀,在60℃下固化30min,得到可拉伸电热致变色纤维(0.04735g)。
图1表明:本实施例1制备的可拉伸电热致变色纤维具有多层结构。
图2表明:本实施例1制备的可拉伸电热致变色纤维直径在0.8mm。
图3表明:本实施例1制备的可拉伸电热致变色纤维有着优异的电学稳定性能。
图4表明:本实施例1制备得到的可拉伸电热致变色纤维在10mA电流下,在不同拉伸情况下其呈现不同颜色(黑色,灰黑色,墨绿色,绿色),在拉伸大于30%后,可拉伸电热致变色纤维颜色逐渐从黑色变为绿色。
图5表明:本实施例1制备得到的可拉伸电热致变色纤维在拉伸超过30%之后,在波长约为505nm处的反射率明显增强,表明颜色从黑色逐渐变为绿色。
图6表明:本实施例1制备得到的可拉伸电热致变色纤维在拉伸30%时,纤维表面温度已经接近转变温度。
实施例2
(1)将500mg氧化石墨烯粉末溶解在100mL去离子水中,用超声波细胞粉碎机超声1h,得到呈棕色的氧化石墨烯分散液。
(2)将包芯纱(0.0226g)分别置于去离子水、丙酮和乙醇中超声15min,烘干,将其等离子体处理15min后预拉伸10%,得到处理后的包芯纱。
(3)将步骤(2)中处理后的包芯纱(0.0227g)放到步骤(1)中氧化石墨烯分散液中浸泡8s,取出用吹风机吹干,得到单层氧化石墨烯修饰的包芯纱。
(4)用步骤(3)中的单层氧化石墨烯修饰的包芯纱重复步骤(3)30次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱(0.02326g)释放预拉伸后,置于氢碘酸(7.5g)中浸泡4h,得到多层石墨烯修饰的包芯纱(0.02321g)。
(5)将聚二甲基硅氧烷PDMS 10g与固化剂1g混合,搅拌30min,静置2h,得到混合剂,将步骤(4)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,待PDMS与纤维表面完全接触后,取出在70℃下固化90min,得到固化后的多层石墨烯修饰的包芯纱,将固化后的多层石墨烯修饰的包芯纱(0.03521g)通过5.0g的45℃热致变色油墨并使其浸涂均匀,在60℃下固化30min,得到可拉伸电热致变色纤维(0.04689g)。由于预拉伸程度较低,降低氧化石墨烯的负载量,故导电性较实施例1要差,导致变色效果减弱。
实施例3
(1)将500mg氧化石墨烯粉末溶解在100mL去离子水中,用超声波细胞粉碎机超声1h,得到呈棕色的氧化石墨烯分散液。
(2)将包芯纱(0.0226g)分别置于去离子水、丙酮和乙醇中超声15min,烘干,将其等离子体处理15min后预拉伸50%,得到处理后的包芯纱。
(3)将步骤(2)中处理后的包芯纱(0.0227g)放到步骤(1)中氧化石墨烯分散液中浸泡8s,取出用吹风机吹干,得到单层氧化石墨烯修饰的包芯纱。
(4)用步骤(3)中的单层氧化石墨烯修饰的包芯纱重复步骤(3)30次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱(0.02354g)释放预拉伸后,置于氢碘酸(7.5g)中浸泡4h,得到多层石墨烯修饰的包芯纱(0.02348g)。
(5)将聚二甲基硅氧烷PDMS 10g与固化剂1g混合,搅拌30min,静置2h,得到混合剂,将步骤(4)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,待PDMS与纤维表面完全接触后,取出在70℃下固化90min,得到固化后的多层石墨烯修饰的包芯纱,将固化后的多层石墨烯修饰的包芯纱(0.03572g)通过5.0g的45℃热致变色油墨并使其浸涂均匀,在60℃下固化30min,得到可拉伸电热致变色纤维(0.04801g)。由于预拉伸程度过高,氧化石墨烯在纤维间隙大量堆积,降低纤维力学性能,故拉伸性能较实施例1要差,导致纤维变色性能降低。
实施例4
(1)将500mg氧化石墨烯粉末溶解在100mL去离子水中,用超声波细胞粉碎机超声1h,得到呈棕色的氧化石墨烯分散液。
(2)将包芯纱(0.0226g)分别置于去离子水、丙酮和乙醇中超声15min,烘干,将其等离子体处理15min后预拉伸40%,得到处理后的包芯纱。
(3)将步骤(2)中处理后的包芯纱(0.0227g)放到步骤(1)中氧化石墨烯分散液中浸泡8s,取出用吹风机吹干,得到单层氧化石墨烯修饰的包芯纱。
(4)用步骤(3)中的单层氧化石墨烯修饰的包芯纱重复步骤(3)5次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱(0.02273g)释放预拉伸后,置于氢碘酸(7.5g)中浸泡4h,得到多层石墨烯修饰的包芯纱(0.02364g)。
(5)将聚二甲基硅氧烷PDMS 10g与固化剂1g混合,搅拌30min,静置2h,得到混合剂,将步骤(4)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,待PDMS与纤维表面完全接触后,取出在70℃下固化90min,得到固化后的多层石墨烯修饰的包芯纱,将固化后的多层石墨烯修饰的包芯纱(0.03527g)通过5.0g的45℃热致变色油墨并使其浸涂均匀,在60℃下固化30min,得到可拉伸电热致变色纤维(0.04726g)。由于氧化石墨烯浸涂次数较少,导致氧化石墨烯涂覆量较少,故导电性能较实施例1要差,导致纤维变色性能降低。
实施例5
(1)将500mg氧化石墨烯粉末溶解在100mL去离子水中,用超声波细胞粉碎机超声1h,得到呈棕色的氧化石墨烯分散液。
(2)将包芯纱(0.0226g)分别置于去离子水、丙酮和乙醇中超声15min,烘干,将其等离子体处理15min后预拉伸40%,得到处理后的包芯纱。
(3)将步骤(2)中处理后的包芯纱(0.0227g)放到步骤(1)中氧化石墨烯分散液中浸泡8s,取出用吹风机吹干,得到单层氧化石墨烯修饰的包芯纱。
(4)用步骤(3)中的单层氧化石墨烯修饰的包芯纱重复步骤(3)40次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱(0.02362g)释放预拉伸后,置于氢碘酸(7.5g)中浸泡4h,得到多层石墨烯修饰的包芯纱(0.02357g)。
(5)将聚二甲基硅氧烷PDMS 10g与固化剂1g混合,搅拌30min,静置2h,得到混合剂,将步骤(4)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,待PDMS与纤维表面完全接触后,取出在70℃下固化90min,得到固化后的多层石墨烯修饰的包芯纱,将固化后的多层石墨烯修饰的包芯纱(0.03567g)通过5.0g的45℃热致变色油墨并使其浸涂均匀,在60℃下固化30min,得到可拉伸电热致变色纤维(0.04752g)。由于氧化石墨烯浸涂次数较多,导致氧化石墨烯涂覆量与实施例1相比无太大差别,故变色性能基本不变,但是其操作较繁琐。

Claims (9)

1.一种可拉伸电热致变色纤维,其特征在于,以包芯纱作为弹性基体,在其表面依次制备导电层、保护层以及变色层,所述包芯纱为双层结构,包芯纱包括芯层和表层,芯层为聚氨酯纤维,表层为螺旋状聚乙烯纤维,所述导电层为石墨烯,所述保护层为聚二甲基硅氧烷PDMS,所述变色层为热致变色油墨。
2.一种可拉伸电热致变色纤维的制备方法,具体步骤如下:
(1)将包芯纱预处理得到处理后的包芯纱;
(2)将步骤(1)中处理后的包芯纱放到氧化石墨烯分散液中浸泡,干燥,得到单层氧化石墨烯修饰的包芯纱,其中处理后的包芯纱与氧化石墨烯的质量比为0.04:1~0.05:1;
(3)用步骤(2)中的单层氧化石墨烯修饰的包芯纱重复步骤(2)多次,得到多层氧化石墨烯修饰的包芯纱,将多层氧化石墨烯修饰的包芯纱释放预拉伸后,置于氢碘酸中反应,得到多层石墨烯修饰的包芯纱,其中多层氧化石墨烯修饰的包芯纱与氢碘酸的质量比为1:315~1:330;
(4)将聚二甲基硅氧烷PDMS与固化剂以质量比为6:1~10:1混合,搅拌,静置,得到混合剂,将步骤(3)中的多层石墨烯修饰的包芯纱浸渍在该混合剂中,固化,得到固化后的多层石墨烯修饰的包芯纱,其中PDMS与多层石墨烯修饰的包芯纱的质量比为420:1~432:1,在固化后的多层石墨烯修饰的包芯纱上浸涂热致变色油墨,再固化,得到可拉伸电热致变色纤维,其中热致变色油墨与固化后的多层石墨烯修饰的包芯纱的质量比为139:1~145:1。
3.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(1)中包芯纱预处理的具体步骤为:将包芯纱分别置于去离子水、丙酮和乙醇中超声,烘干,等离子体处理15min后进行预拉伸。
4.按照权利要求3所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述超声时间为10~30min;预拉伸的比为10~50%。
5.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(2)中氧化石墨烯分散液的制备方法为:将氧化石墨烯溶解在水中,超声,得到氧化石墨烯分散液,氧化石墨烯分散液的浓度为5mg/mL。
6.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(2)中浸泡时间为5~10s。
7.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(3)中多次为5~40;反应时间为2~4h。
8.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(4)中固化温度为60~90℃,固化时间为60~120min;再固化温度为60~80℃,再固化时间为30~90min。
9.按照权利要求2所述的一种可拉伸电热致变色纤维的制备方法,其特征在于,所述步骤(4)中热致变色油墨为45℃热致变色油墨,变色时间为15s,褪色时间为10s。
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