CN113445309A - 一种导电pbo纤维及其制备方法 - Google Patents
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Abstract
本发明属于高性能纤维及其复合材料技术领域,尤其为一种导电PBO纤维及其制备方法,所述导电PBO纤维主要由基材纤维和外层金属两部分组成,所述基材纤维为聚对苯撑苯并二噁唑纤维(PBO),所述外层金属通过真空镀、冷喷涂或化学镀方式,在所述基材纤维表面沉积一层金属层;本发明创造性地提出了导电PBO纤维制备技术,填补了国内相关技术领域的空白,本发明所制备的导电PBO纤维性能优异,具有重量轻(米重≤0.16g/m)、强度高(比强度≥27cN/dtex)、导电性能优(长度表面电阻≤2.5Ω/m)、耐高温、柔韧性好、金属层结合牢固等诸多优点,本发明中提出的导电PBO纤维的制备工艺简单、耗时较短、成本较低,且节能、安全、环保,易于实现工业化生产。
Description
技术领域
本发明属于高性能纤维及其复合材料技术领域,具体涉及一种导电PBO纤维及其制备方法。
背景技术
PBO纤维,即聚对苯撑苯并二噁唑纤维,是一种综合性能优异的有机纤维,它不仅具有非常优异的力学性能,而且具有良好的耐热性能和超高的极限氧指数,基于PBO纤维的上述优良特性,如果将其表面金属化,制成的导电PBO纤维,不仅继承了基材纤维优异的力学性能、耐热性能和阻燃特性,而且具有良好的导电功能,可应用于航空航天、军工、高频通讯、电磁屏蔽和兵工消防等诸多领域。
然而,由于PBO分子规则有序的取向结构使纤维表面非常光滑,且分子链上的极性杂原子绝大部分包裹在纤维内部,纤维表面极性很小,使得纤维表现出极强的化学惰性,很难与导电物质结合。目前,全球范围内可实现导电PBO纤维商业化生产的只有美国的SYSCOM公司,处于垄断地位,产品在国内的售价很高,并对我国实行技术封锁,可以预见随着全球贸易局势升温,相关产品对我国的钳制作用将愈加显著。因此,自主开发导电PBO纤维,推进高性能导电纤维产品国产化进程迫在眉睫。目前,国内仅有少数个别单位在开展相关产品的研究与开发工作,但由于技术和工艺限制,仍然停留在实验室阶段,尚未形成工业化生产能力。
发明CN103789754A公开了一种在PBO纤维表面制备Ni/P/纳米SiO2三元复合镀层的方法,作者首先制备了纳米SiO2溶胶,然后对PBO纤维依次进行粗化→敏化→活化→还原→复合镀镍,最后得到覆有Ni/P/纳米SiO2三元复合镀层的PBO纤维,该技术解决的主要问题是PBO纤维在受到紫外线辐照而发生光氧化老化,引起材料耐久性降低的问题。该发明并未提及成品的导电性和强度等技术指标,且该发明中纳米SiO2溶胶制备时间长达3-7h,粗化时间长达1-4h,耗时太长且工艺复杂,难以实现工业化生产。
因此,本技术领域人员提出了一种导电PBO纤维及其制备方法,以解决上述背景中提出的问题。
发明内容
为解决上述背景技术中提出的问题。本发明提供了一种导电PBO纤维及其制备方法,具有重量轻、强度高、导电性能优、耐高温、柔韧性好、金属层结合牢固的特点。
为实现上述目的,本发明提供如下技术方案:一种导电PBO纤维,主要由基材纤维和外层金属两部分组成,所述基材纤维为聚对苯撑苯并二噁唑纤维(PBO),所述外层金属通过真空镀、冷喷涂或化学镀方式,在所述基材纤维表面沉积一层金属层。
优选的,所述基材纤维为PBO纤维长丝或短切纤维。
优选的,所述PBO纤维长丝由100-2000根PBO单丝组成,所述基材纤维中PBO单丝直径为10-20μm。
优选的,所述外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
优选的,所述外层金属总厚度为0.5-5μm,所述外层金属均匀、连续地覆盖每根纤维单丝表面。
一种导电PBO纤维及其制备方法,包括如下步骤:
S6.1、除油除胶:将所述基材纤维进行除油除胶处理,处理完毕用去离子水洗至中性,然后吹干;
S6.2、表面改性:将经过步骤S6.1处理后的PBO纤维进行表面改性处理,处理完毕用去离子水洗至中性,然后吹干;
S6.3、金属化:对经过步骤S6.2处理后的PBO纤维表面进行金属化处理,处理完毕用去离子水洗至中性,最后吹干得到导电PBO纤维成品。
优选的,所述除油除胶方法可以是有机溶剂法、高温化学法、高温碱液法和电化学法中的一种或几种,除油除胶处理时间为1-10min,所述表面改性方法可以是化学法、电化学法、偶联剂法、紫外线照射、等离子刻蚀和γ射线辐照中的一种或几种方法的组合,表面改性处理时间为0.1-30min,所述金属化处理可以为真空镀、冷喷涂或化学镀方式中的任意一种。
优选的,所述真空镀中镀金属可以是铝、镍、铜、银、锌和金中的一种或几种的组合,真空镀温度为150-750℃,真空度为1-10-2Pa。
优选的,所述冷喷涂中喷涂金属可以是铝、镍、铜、锡和锌中的一种或几种的组合,采用低压冷喷涂工艺,工作压力为5-8bar。
优选的,所述化学镀通过以下步骤完成:
S10.1、预浸:将经过步骤S6.2处理后的PBO纤维进行预浸处理,处理时间为1-10min,所述预浸过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.2、活化:将经过步骤S10.1处理后的PBO纤维进行活化处理,处理时间为1-10min,所述活化过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.3、解胶:将经过步骤S10.2处理后的PBO纤维进行解胶处理,处理时间为1-10min,所述解胶过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.4、化学镀:将经过步骤S10.3处理后的纤维放入化学镀液中,所述化学镀液可以是化学镀镍、化学镀铜、化学镀银、化学镀锡和化学镀金中的一种或几种的组合,所述化学镀过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以使PBO纤维在溶液中保持良好的分散状态,确保纤维束中的每一根单丝都均匀、连续地沉积上金属,最终得到导电PBO纤维成品,化学镀温度为20-100℃,反应时间为1-60min;
S10.5、将经过步骤S10.4处理后的纤维水洗至中性,并吹干得到导电PBO纤维成品。
与现有技术相比,本发明的有益效果是:
1、本发明创造性地提出了导电PBO纤维制备技术,填补了国内相关技术领域的空白;
2、本发明所制备的导电PBO纤维性能优异,具有重量轻(米重≤0.16g/m)、强度高(比强度≥27cN/dtex)、导电性能优(长度表面电阻≤2.5Ω/m)、耐高温、柔韧性好、金属层结合牢固等诸多优点;
3、本发明中提出的导电PBO纤维的制备工艺简单、耗时较短、成本较低,且节能、安全、环保,易于实现工业化生产。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:
图1为本发明实施例1所制备的导电PBO纤维截面金相照片;
图2为本发明实施例2所制备的导电PBO纤维截面金相照片;
图3为本发明实施例3所制备的导电PBO纤维截面金相照片;
图4是本发明实施例4所制备的导电PBO纤维截面金相照片。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,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。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
请参阅图1-4,本发明提供以下技术方案:一种导电PBO纤维,主要由基材纤维和外层金属两部分组成,基材纤维为聚对苯撑苯并二噁唑纤维(PBO),外层金属通过真空镀、冷喷涂或化学镀方式,在基材纤维表面沉积一层金属层。
具体的,基材纤维为PBO纤维长丝或短切纤维。
具体的,PBO纤维长丝由100-2000根PBO单丝组成,基材纤维中PBO单丝直径为10-20μm。
具体的,外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
具体的,外层金属总厚度为0.5-5μm,外层金属均匀、连续地覆盖每根纤维单丝表面。
一种导电PBO纤维及其制备方法,包括如下步骤:
S1、除油除胶:将基材纤维置于质量分数30%的丙酮溶液中,辅助以超声波震荡,除油除胶处理时间为10min,处理完毕用去离子水洗至中性,然后吹干;
S2、表面改性:将经过步骤S1处理后的PBO纤维进行化学改性处理,所用改性液为重铬酸钾和浓硫酸的混合溶液,其中重铬酸钾质量浓度为2-10g/L,浓硫酸质量分数为5-20%,改性温度为30-60℃,改性时间为5-30min,处理完毕用去离子水洗至中性,然后吹干;
S3、金属化:对经过步骤S2处理后的PBO纤维表面进行真空镀锌处理,真空镀温度为280℃,真空度为5×10-2Pa,保温时间30min,最终得到导电PBO纤维成品。
实施例2
请参阅图1-4,本发明提供以下技术方案:一种导电PBO纤维,主要由基材纤维和外层金属两部分组成,基材纤维为聚对苯撑苯并二噁唑纤维(PBO),外层金属通过真空镀、冷喷涂或化学镀方式,在基材纤维表面沉积一层金属层。
具体的,基材纤维为PBO纤维长丝或短切纤维。
具体的,PBO纤维长丝由100-2000根PBO单丝组成,基材纤维中PBO单丝直径为10-20μm。
具体的,外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
具体的,外层金属总厚度为0.5-5μm,外层金属均匀、连续地覆盖每根纤维单丝表面。
一种导电PBO纤维及其制备方法,包括如下步骤:
S1、除油除胶:称取一定量的无磷除油粉,加入所需量的去离子水配制成除油液,将除油液加热到50-60℃,然后将基材纤维浸没在溶液中进行除油除胶处理,过程中辅助以超声波震荡,处理时间为5min,处理完毕用去离子水洗至中性,然后吹干;
S2、表面改性:将经过步骤S1处理后的PBO纤维表面进行等离子刻蚀处理,等离子刻蚀采用真空等离子表面处理机,处理功率为0.2-5kW,工作真空度为1-50Pa,处理时间为6-240s;
S3、金属化:对经过步骤S2处理后的PBO纤维表面进行冷喷锌处理,冷喷锌采用低压冷喷涂工艺,喷涂过程中基材表面温度为120-150℃,工作压力为5bar,最终得到导电PBO纤维成品。
实施例3
请参阅图1-4,本发明提供以下技术方案:一种导电PBO纤维,主要由基材纤维和外层金属两部分组成,基材纤维为聚对苯撑苯并二噁唑纤维(PBO),外层金属通过真空镀、冷喷涂或化学镀方式,在基材纤维表面沉积一层金属层。
具体的,基材纤维为PBO纤维长丝或短切纤维。
具体的,PBO纤维长丝由100-2000根PBO单丝组成,基材纤维中PBO单丝直径为10-20μm。
具体的,外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
具体的,外层金属总厚度为0.5-5μm,外层金属均匀、连续地覆盖每根纤维单丝表面。
一种导电PBO纤维及其制备方法,包括如下步骤:
S1、除油除胶:称取一定量的纯碱和固体氢氧化钠,加入所需量的去离子水配制成混合碱溶液,将混合碱溶液加热到50-70℃,然后将基材纤维浸没在热碱溶液中进行除油除胶处理,过程中辅助以机械搅拌或空气搅拌,处理时间为2min,处理完毕用去离子水洗至中性,然后吹干;
S2、表面改性:将经过上述步骤处理后的PBO纤维采用硅烷偶联剂进行交联接枝改性,所述硅烷偶联剂可以是KH550、KH560或KH570的醇水溶液,改性时间为10-30min,改性温度为50-70℃,改性完毕用去离子水洗至中性,然后烘干;
S3、预浸:将经过上述步骤处理后的PBO纤维浸没在预浸液中,预浸时间为1-10min,预浸温度为20-40℃,过程中辅助以机械搅拌或空气搅拌,以确保PBO纤维中每一根单丝都处理到位。
S4、活化:将经过上述步骤处理后的PBO纤维浸没在活化液中,活化时间为1-10min,活化温度为20-40℃,过程中辅助以机械搅拌或空气搅拌,以确保PBO纤维中每一根单丝都处理到位。
S5、解胶:将经过上述步骤处理后的PBO纤维浸没在解胶液中,解胶时间为1-10min,解胶温度为20-40℃,过程中辅助以机械搅拌或空气搅拌,以确保PBO纤维中每一根单丝都处理到位。
S6、化学镀:将经过上述步骤处理后的PBO纤维放入化学镀锡液中,进行化学镀锡,反应温度为70-100℃,反应时间为1-10min,化学镀锡过程中辅助以机械搅拌或空气搅拌,以使PBO纤维在溶液中保持良好的分散状态,确保纤维束中的每一根单丝都均匀、连续地沉积上金属锡,最终得到导电PBO纤维成品。
实施例4
请参阅图1-4,本发明提供以下技术方案:一种导电PBO纤维,主要由基材纤维和外层金属两部分组成,基材纤维为聚对苯撑苯并二噁唑纤维(PBO),外层金属通过真空镀、冷喷涂或化学镀方式,在基材纤维表面沉积一层金属层。
具体的,基材纤维为PBO纤维长丝或短切纤维。
具体的,PBO纤维长丝由100-2000根PBO单丝组成,基材纤维中PBO单丝直径为10-20μm。
具体的,外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
具体的,外层金属总厚度为0.5-5μm,外层金属均匀、连续地覆盖每根纤维单丝表面。
一种导电PBO纤维及其制备方法,包括如下步骤:
S1、除油除胶:将基材纤维置于质量分数30%的丙酮溶液中,过程中辅助以超声震荡或机械震动,除油除胶处理时间为5min,处理完毕用去离子水洗至中性,然后吹干。
S2、表面改性:将经过上述步骤处理后的PBO纤维表面进行γ射线辐照处理,γ射线辐照剂量为1-10KGy,以5-20KGy/h的剂量率辐照处理相应的时间。
S3、预浸:将经过上述步骤处理后的PBO纤维浸没在预浸液中,预浸时间为1-10min,预浸温度为20-40℃,过程中辅助以超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位。
S4、活化:将经过上述步骤处理后的PBO纤维浸没在活化液中,活化时间为1-10min,活化温度为20-40℃,过程中辅助以超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位。
S5、解胶:将经过上述步骤处理后的PBO纤维浸没在解胶液中,解胶时间为1-10min,解胶温度为20-40℃,过程中辅助以超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位。
S6、化学镀:将经过上述步骤处理后的PBO纤维放入化学镀银液中,进行化学镀银,反应温度为50-80℃,反应时间为1-8min,化学镀银过程中辅助以超声震荡或机械震动,以使PBO纤维在溶液中保持良好的分散状态,确保纤维束中的每一根单丝都均匀、连续地沉积上金属银,最终得到导电PBO纤维成品。
本发明中的试验结果:取上述实施例1、实施例2、实施例3和实施例4所制备的导电PBO纤维进行导电性能和断裂强度测试,测得样品的长度表面电阻分别为2.42Ω/m、2.06Ω/m、2.43Ω/m和1.88Ω/m,断裂强度平均高达27cN/dtex。因此,本发明制得的导电PBO纤维是一种高强度、高导电、耐高温、阻燃性能优异的导电纤维。
本发明中的工作原理及使用流程:首先,对基材PBO纤维表面进行除油除胶处理,以获得清洁的表面;然后,对PBO纤维进行改性处理,获得具有一定缺陷和粗糙度的表面,以利于导电物质附着;最后,对上述改性后的PBO纤维进行金属化加工,制得导电PBO纤维。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下。由语句“包括一个限定的要素,并不排除在包括要素的过程、方法、物品或者设备中还存在另外的相同要素”。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种导电PBO纤维,其特征在于:主要由基材纤维和外层金属两部分组成,所述基材纤维为聚对苯撑苯并二噁唑纤维(PBO),所述外层金属通过真空镀、冷喷涂或化学镀方式,在所述基材纤维表面沉积一层金属层。
2.根据权利要求1所述的一种导电PBO纤维,其特征在于:所述基材纤维为PBO纤维长丝或短切纤维。
3.根据权利要求2所述的一种导电PBO纤维,其特征在于:所述PBO纤维长丝由100-2000根PBO单丝组成,所述基材纤维中PBO单丝直径为10-20μm。
4.根据权利要求3所述的一种导电PBO纤维,其特征在于:所述外层金属为铝、镍、铜、银、锡、锌和金中的一种或几种的组合。
5.根据权利要求4所述的一种导电PBO纤维,其特征在于:所述外层金属总厚度为0.5-5μm,所述外层金属均匀、连续地覆盖每根纤维单丝表面。
6.根据权利要求5所述的一种导电PBO纤维及其制备方法,其特征在于:包括如下步骤:
S6.1、除油除胶:将所述基材纤维进行除油除胶处理,处理完毕用去离子水洗至中性,然后吹干;
S6.2、表面改性:将经过步骤S6.1处理后的PBO纤维进行表面改性处理,处理完毕用去离子水洗至中性,然后吹干;
S6.3、金属化:对经过步骤S6.2处理后的PBO纤维表面进行金属化处理,处理完毕用去离子水洗至中性,最后吹干得到导电PBO纤维成品。
7.根据权利要求6所述的一种导电PBO纤维及其制备方法,其特征在于:所述除油除胶方法可以是有机溶剂法、高温化学法、高温碱液法和电化学法中的一种或几种,除油除胶处理时间为1-10min,所述表面改性方法可以是化学法、电化学法、偶联剂法、紫外线照射、等离子刻蚀和γ射线辐照中的一种或几种方法的组合,表面改性处理时间为0.1-30min,所述金属化处理可以为真空镀、冷喷涂或化学镀方式中的任意一种。
8.根据权利要求7所述的一种导电PBO纤维及其制备方法,其特征在于:所述真空镀中镀金属可以是铝、镍、铜、银、锌和金中的一种或几种的组合,真空镀温度为150-750℃,真空度为1-10-2Pa。
9.根据权利要求7所述的一种导电PBO纤维及其制备方法,其特征在于:所述冷喷涂中喷涂金属可以是铝、镍、铜、锡和锌中的一种或几种的组合,采用低压冷喷涂工艺,工作压力为5-8bar。
10.根据权利要求7所述的一种导电PBO纤维及其制备方法,其特征在于:所述化学镀通过以下步骤完成:
S10.1、预浸:将经过步骤S6.2处理后的PBO纤维进行预浸处理,处理时间为1-10min,所述预浸过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.2、活化:将经过步骤S10.1处理后的PBO纤维进行活化处理,处理时间为1-10min,所述活化过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.3、解胶:将经过步骤S10.2处理后的PBO纤维进行解胶处理,处理时间为1-10min,所述解胶过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以确保PBO纤维中每一根单丝都处理到位;
S10.4、化学镀:将经过步骤S10.3处理后的纤维放入化学镀液中,所述化学镀液可以是化学镀镍、化学镀铜、化学镀银、化学镀锡和化学镀金中的一种或几种的组合,所述化学镀过程中辅助以机械搅拌、空气搅拌、超声震荡或机械震动,以使PBO纤维在溶液中保持良好的分散状态,确保纤维束中的每一根单丝都均匀、连续地沉积上金属,最终得到导电PBO纤维成品,化学镀温度为20-100℃,反应时间为1-60min;
S10.5、将经过步骤S10.4处理后的纤维水洗至中性,并吹干得到导电PBO纤维成品。
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