CN105926012A - 一种铁-镍-铜氧体长纤维管的制备方法 - Google Patents

一种铁-镍-铜氧体长纤维管的制备方法 Download PDF

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CN105926012A
CN105926012A CN201610372575.5A CN201610372575A CN105926012A CN 105926012 A CN105926012 A CN 105926012A CN 201610372575 A CN201610372575 A CN 201610372575A CN 105926012 A CN105926012 A CN 105926012A
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nickel
copper
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苑晨洲
罗奕兵
吴明哲
余小峰
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Changsha University of Science and Technology
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Abstract

一种铁‑镍‑铜氧体长纤维管的制备方法，技术方案的步骤：聚丙烯纤维的表面处理；聚丙烯纤维的化学镀铜；纤维镀镍；纤维镀铁；聚丙烯纤维的去除；长纤维金属复合管的焙烧氧化制成铁‑镍‑铜氧体长纤维管。本发明可制备不同规铬和断面形状的铁‑镍‑铜氧体长纤维管，长纤维管管内残炭的反射和吸收作用将增强电磁波的衰减效果，与传统制备方法相比，可制备超长的铁‑镍‑铜氧体纤维管。

Description

一种铁-镍-铜氧体长纤维管的制备方法
技术领域
本发明涉及功能化金属纤维管制备技术领域，尤其是涉及一种铁-镍-铜氧体长纤维管的制备方法。
背景技术
随着微波和微电子工程技术的迅速发展，先进吸波材料在抗电磁干扰以及隐身技术等领域的重要性日益突出。磁性纤维管吸收剂由于其形状各向异性和磁各向异性，在长轴方向可以获得很高的磁导率，能够摆脱各向同性粉末材料对有效磁导率的限制，因此可以在占空比较小的情况下获得较高的磁导率，从而有利于减轻涂层重量并加宽对电磁波吸收的频带。于是在继磁性纳米粉体吸收剂之后，磁性微纤维吸收剂的研制和开发逐渐成为该领域的一个热点。铁氧体微纳米纤维不仅拥有传统铁氧体的低介电性、高电阻率和易于匹配等优点，而且还具有比磁性金属及合金纤维更高的抗氧化性和耐腐蚀性等特征，同时纤维的形状各向异性还有利于克服铁氧体本身的自然共振频率过低和较低的Snoek 极限等问题，从而能大大提高其在微波频段的磁导率和磁损耗以及使用频率范围，有望发展成为一种能够满足现代隐身技术发展需求的新型高性能微波吸收剂。
铁氧体纤维的制备方法多种多样，大致可划分为物理模板辅助生长和无模板化学合成两个方面。模板辅助生长技术往往利用模板( 如多孔阳极氧化铝膜、多孔聚碳酸酯膜、介孔分子筛、碳纳米管等) 的空间限域效应结合电化学沉积、化学沉积或外延生长等具体方法使磁体在模板的孔道中生长，从而获得具有一维结构特征的磁性材料。相对于模板法，无模板化学合成法制备一维磁性纳米材料则显得更为方便和灵活。一是其设备简单，投资少，且产量较大，易于转化为工业化生产；二是可通过多种途径来控制一维纳米结构的形貌参数和晶面取向，获得具有不同显微结构的一维纳米结构磁性材料。无模板化学合成法主要包括液相及磁场辅助液相法、磁场诱导有机金属热分解法和静电纺丝法等。以上方法制备铁氧体纤维的长度受限。
发明内容
本发明要解决的技术问题是提供一种铁-镍-铜氧体长纤维管的制备方法：对聚丙烯纤维表面处理（粗化、活化、敏化）、化电镀铜、电镀镍、电镀铁制成复合纤维、复合纤维经分解、裂解、燃烧，焙烧氧化形成铁-镍-铜氧体长纤维管。
本发明解决其技术问题所采用的技术方案，包括以下步骤：
（1）聚丙烯纤维的表面处理：采用10~20%wt的氢氧化钠溶液进行化学除油，采用铬酐和硫酸溶液进行纤维表面的粗化，采用酸性的锡盐溶液进行纤维的敏化，敏化后纤维的清洗，采用硝酸银和氨水溶液进行纤维表面的活化，活化后的纤维经甲醛溶液还原；
（2）纤维的化学镀铜，其溶液成分为：酒石酸钾钠10～20g/L ，氢氧化钠2～5g/L，硫酸铜2～4g/L ，氯化镍,0.2~1g/L， 甲醛1～3g/L，化学镀时间为2-8min；
（3）纤维镀镍，电镀液组成为，硫酸镍150-250g/L，硼酸30-45g/L，氯化钠5-15g/L，络合剂微量，pH=2~3；
（4）纤维镀铁，电镀液组成为硫酸亚铁70-150g/L，氯化亚铁150-250g/L，硼酸30-50g/L，络合剂微量，稳定剂微量，pH=1~2；
（5）聚丙烯纤维的去除，复合纤维在400～500℃氧化性气氛下氧化1-3h；
（6）金属复合长纤维管的焙烧氧化，在氧化性气氛下，700~950℃保温2-10h，金属原子扩散与氧化制成铁-镍-铜氧体长纤维管。
本发明的优点是：
（1）选择不同直径或异形截面的聚丙烯纤维，可制备不同规铬和断面形状的磁性金属连续纤维管；
（2）可通过调整电镀工艺的时间，可获得具有不同比例构成的铁-镍-铜氧体长纤维管；
（3）与传统制备方法相比，可制备超长的铁-镍-铜氧体纤维管，纤维管长度不受本工艺条件的限制，仅取决于原聚丙烯纤维的长度；
（4）采用中空结构，本发明制备的铁氧体纤维管可有利于减轻涂层重量，并由于纤维管内壁和外壁的反射和散射，对电磁波吸收更具有更高效率，提升隐身性能。
具体实施方式：
以下结合实施例对本发明作进一步说明：
实施例1：φ 0.012 mm铁-镍-铜氧体长纤维管的成形工艺
（1）聚丙烯连续性纤维直径为φ0.006 mm，先采用10%wt氢氧化钠溶液进行化学除油5min；粗化的水溶液配比为80g/L 铬酐、300ml/L 硫酸，粗化处理温度为60℃，粗化处理时间20min；敏化液组成为氯化锡8g/L，盐酸40ml/L ，敏化处理时间3min；采用硝酸银和氨水溶液进行纤维表面的活化，活化后的纤维经甲醛溶液还原；
（2）纤维的化学镀铜，其溶液成分为：酒石酸钾钠10 g/L ，氢氧化钠2.5g/L，硫酸铜2g/L ，氯化镍0.2g/L， 甲醛1.2 g/L，化学镀时间为5min；
（3）纤维镀镍，电镀液组成为，硫酸镍220g/L，硼酸38g/L，氯化钠10g/L，络合剂微量，pH=2~3，电镀时间为20min；
（4）纤维镀铁，电镀液组成为硫酸亚铁100g/L，氯化亚铁200g/L，硼酸45g/L，络合剂微量，稳定剂微量，pH=1~2，电镀时间为10min；
（5）聚丙烯纤维的去除，复合纤维在450 ℃空气气氛下氧化1.5 h；
（6）长纤维金属复合管的焙烧氧化，在氧气气氛下，800℃保温5h，自然冷却至室温，获得φ 0.012 mm铁-镍-铜氧体长纤维管，内径尺寸为φ0.006 mm。

Claims (1)

1.一种铁-镍-铜氧体长纤维管的制备方法，其特征在于，技术方案的步骤为：（1）聚丙烯连续性纤维的表面处理：采用10~20%wt的氢氧化钠溶液进行化学除油，采用铬酐和硫酸溶液进行纤维表面的粗化，采用酸性的锡盐溶液进行纤维的敏化，敏化后纤维的清洗，采用硝酸银和氨水溶液进行纤维表面的活化，活化后的纤维经甲醛溶液还原；（2）纤维的化学镀铜，其溶液成分为：酒石酸钾钠10～20g/L ，氢氧化钠2～5g/L，硫酸铜2～4g/L ，氯化镍,0.2~1g/L， 甲醛1～3g/L，化学镀时间为2-8min；（3）纤维镀镍，电镀液组成为，硫酸镍150-250g/L，硼酸30-45g/L，氯化钠5-15g/L，络合剂微量，pH=2~3；（4）纤维镀铁，电镀液组成为硫酸亚铁70-150g/L，氯化亚铁150-250g/L，硼酸30-50g/L，络合剂微量，稳定剂微量，pH=1~2；（5）聚丙烯纤维的去除，复合纤维在400～500℃氧化性气氛下氧化1-3h；（6）长纤维金属复合管的焙烧氧化，在氧化性气氛下，700~950℃保温2-10h，金属原子扩散与氧化制成铁-镍-铜氧体长纤维管。
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CN107805830A (zh) * 2017-10-11 2018-03-16 武汉钢铁有限公司 闪镀铁镀液及闪镀方法
CN108265243A (zh) * 2017-01-02 2018-07-10 罗奕兵 一种铁-镍-磷非晶合金复合纤维及其制备方法
CN108265512A (zh) * 2017-01-02 2018-07-10 罗奕兵 一种镍-磷非晶合金复合纤维及其制备方法
CN109136895A (zh) * 2017-06-18 2019-01-04 刘志红 一种钴-镍-磷磁性复合纤维及制备方法
CN109126866A (zh) * 2017-06-27 2019-01-04 罗奕兵 一种钴-锌-磷催化反应器及制备方法
CN109137488A (zh) * 2017-06-27 2019-01-04 刘志红 一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法
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CN109136888A (zh) * 2017-06-28 2019-01-04 罗奕兵 一种Fe-Ni-P非晶合金催化反应器及生产方法
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CN108265512A (zh) * 2017-01-02 2018-07-10 罗奕兵 一种镍-磷非晶合金复合纤维及其制备方法
CN108265243A (zh) * 2017-01-02 2018-07-10 罗奕兵 一种铁-镍-磷非晶合金复合纤维及其制备方法
CN109136891A (zh) * 2017-06-18 2019-01-04 罗奕兵 一种镍-磷非晶合金复合纤维及制备方法
CN109136895A (zh) * 2017-06-18 2019-01-04 刘志红 一种钴-镍-磷磁性复合纤维及制备方法
CN109137486A (zh) * 2017-06-18 2019-01-04 刘志红 一种钴-锌-磷磁性复合纤维及制备方法
CN109137487A (zh) * 2017-06-18 2019-01-04 罗奕兵 一种镍-铁-磷非晶合金复合纤维及制备方法
CN109126866A (zh) * 2017-06-27 2019-01-04 罗奕兵 一种钴-锌-磷催化反应器及制备方法
CN109137488A (zh) * 2017-06-27 2019-01-04 刘志红 一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法
CN109126656A (zh) * 2017-06-27 2019-01-04 罗奕兵 一种镍-铁-磷非晶合金催化反应器生产方法
CN109136889A (zh) * 2017-06-27 2019-01-04 罗奕兵 一种钴-镍-磷催化反应器及生产方法
CN109136890A (zh) * 2017-06-28 2019-01-04 罗奕兵 一种Fe-P非晶合金催化反应器及生产方法
CN109136888A (zh) * 2017-06-28 2019-01-04 罗奕兵 一种Fe-Ni-P非晶合金催化反应器及生产方法
CN109137489A (zh) * 2017-06-28 2019-01-04 罗奕兵 一种Fe-P/聚合物复合纤维及制备方法
CN107805830A (zh) * 2017-10-11 2018-03-16 武汉钢铁有限公司 闪镀铁镀液及闪镀方法
CN111472030A (zh) * 2020-06-05 2020-07-31 麦德美科技（苏州）有限公司 锰锌铁氧体化学粗化电镀工艺

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