CN114059051B - 一种玄武岩纤维材料表面金属化的方法 - Google Patents

一种玄武岩纤维材料表面金属化的方法 Download PDF

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CN114059051B
CN114059051B CN202111236308.2A CN202111236308A CN114059051B CN 114059051 B CN114059051 B CN 114059051B CN 202111236308 A CN202111236308 A CN 202111236308A CN 114059051 B CN114059051 B CN 114059051B
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张津
翟亚领
陈耀
沈鑫
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Chongqing Zhidu New Material Technology Co ltd
University of Science and Technology Beijing USTB
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Abstract

本发明涉及一种玄武岩纤维材料表面金属化的方法，属于非金属材料表面处理领域。首先对玄武岩纤维进行亲水处理，硅烷偶联剂和贵金属离子分别对其进行偶联改性和活化处理，然后利用能将活化液中的贵金属离子还原的还原剂对纤维进行还原处理，最后将纤维置于化学镀液中通过化学镀法使玄武岩纤维表面金属化，实现玄武岩纤维—金属核壳结构。该方法中偶联改性处理工艺替代了传统化学镀方法中的敏化处理，增强了玄武岩纤维在活化过程中对贵金属离子的吸附能力，在纤维表面形成了均匀的活化层。该方法简单易行、安全可靠、经济环保，得到的金属镀层综合性能好，便于工业化应用生产。

Description

一种玄武岩纤维材料表面金属化的方法
技术领域
本发明属于非金属材料表面处理领域，具体涉及一种玄武岩纤维材料表面金属化的方法。
背景技术
玄武岩纤维是以天然玄武岩矿石为原料，高温熔融后通过铂铑合金拉丝漏板拉制而成的连续无机非金属纤维，其主要成分由SiO2、Al2O3、MgO、FeOx、CaO、TiO2等氧化物组成。玄武岩纤维具有优异的力学性能、化学稳定性、耐酸碱性能、耐温性能、介电性能以及吸波透磁和隔音隔热性能，以连续玄武岩纤维为增强体制成的性能优异的复合材料，广泛应用于航空航天、建筑、化工、农业等军工和民用领域。
但是玄武岩矿石属于绝缘材料，相应的纤维电阻率大于1012Ω·m，这一性质限制了玄武岩纤维在导体、半导体等领域的应用。而开发表面金属化玄武岩纤维有望在防静电、电磁屏蔽、吸波等领域中代替碳纤维，可以进一步提升玄武岩纤维材料的应用附加值。目前国内外有关增强非金属材料的导电性，常用的方法有化学气相沉积法、磁控溅射法、物理气相沉积法、化学镀法以及复合镀法等，如专利CN108218216A报道通过化学气相沉积将碳系纳米材料在玄武岩纤维表面均匀沉积碳纳米材料涂层，得到的纤维电导率在101到104S/cm可调。此方法虽可增强玄武岩纤维材料的导电性，但该方法所用设备昂贵、过程繁琐难以实现工业化应用。而化学镀工艺以其镀层均匀、致密、孔隙率低以及与基体结合力好等优点，在非金属材料表面金属化领域中得到了广泛应用，化学镀不需要外加电源，利用溶液中的还原剂将金属离子还原为金属并沉积在非金属基体表面上形成镀层。如专利CN101302080A、CN101311309A中报道通过超声波清洗、分散处理、粗化处理、偶联处理、敏化、活化处理、解胶处理以及烘干的化学镀前处理工艺，进行施镀制备导电导磁的玻璃纤维，其镀层的综合性能好，但该化学镀工艺前处理中敏化工艺使用的氯化亚锡溶液和解胶处理用的盐酸溶液对环境有一定的危害性，且整体前处理步骤较为冗余，制备时间较长。
鉴于此，本发明旨在提供适合制备表面金属化玄武岩纤维材料，且满足镀层性能优异、易工业化应用的一种化学镀方法。
发明内容
本发明旨在解决导电玄武岩纤维材料的制备，提供一种新的制备表面金属化玄武岩纤维材料的化学镀方法，该方法工艺简单易行、安全可靠、经济环保，便于规模化生产，得到的导电玄武岩纤维镀镍层厚度均匀，镍层厚度在0.5～0.8微米之间，纤维表面形貌优良，其方块电阻在0.3～5Ω/□之间可控。
为解决上述技术问题，本发明通过以下技术方案实现：
一种玄武岩纤维材料表面金属化的方法，包括下述步骤：
(1)纤维表面亲水处理：在碱性溶液中对玄武岩纤维进行亲水处理并清洗；
(2)偶联：将经步骤(1)亲水处理后的玄武岩纤维置于氨基类的硅烷偶联剂溶液中进行纤维表面偶联改性处理并进行固化处理；
(3)活化：将经步骤(2)偶联处理后的玄武岩纤维置于活化液中进行活化处理并清洗；
(4)还原：将经步骤(3)活化处理后的玄武岩纤维置于还原剂溶液中，随后清洗并干燥；
(5)施镀。
优选的，碱性溶液为40～60g/L的氢氧化钠溶液或56～70g/L的氢氧化钾溶液，亲水处理温度为30～50℃，时间为5～30min。
氢氧化钠溶液与氢氧化钾溶液如果浓度过高，会对纤维造成损伤，浓度过低，则出现亲水效果不理想，不利于生产，因此本发明氢氧化钠溶液优选的浓度范围是40～60g/L，氢氧化钾溶液优选的浓度范围是56～70g/L。
优选的，氨基类的硅烷偶联剂溶液包括1～5wt％的氨基类硅烷，氨基类硅烷偶联剂为KH550、KH792、KH602其中的至少一种。
氨基类硅烷偶联剂如果浓度过高，则增加成本，浓度过低则会增加偶联处理时间，不利于生产，因此本发明氨基类硅烷优选的浓度范围是1～5wt％。
优选的，偶联处理温度25～50℃，时间为10～30min，固化温度80～120℃固化时间为10～30min。
优选的，氯化钯浓度为0.1～0.3g/L，盐酸浓度为0.1～0.3mol/L。
优选的，活化处理温度为30～50℃，时间为10～30min。
优选的，还原剂溶液为2～10g/L次磷酸钠溶液或2～10g/L次磷酸钾溶液或3～8g/L的硼氢化钠溶液，还原处理的温度为25～50℃，还原处理的时间为10～50min，干燥的温度为70～80℃，干燥的时间为10～20min。
优选的，施镀是指在纤维表面镀镍、铜、金、银、铁等金属及其合金。
氨基类的硅烷偶联剂尾端悬挂着氨基，氨基可以与活化液中的钯离子进行共价键配位，通过此类硅烷偶联剂能够更好地满足纤维化学吸附钯离子的效果。
优选的，玄武岩纤维可以为无捻粗纱、加捻丝束、平纹织物、缎纹织物、毡的纤维制品。
本发明摒弃了非金属材料传统化学镀中的敏化、解胶前处理，在粗化与活化处理之间采用偶联改性处理，偶联改性处理中硅烷偶联剂硅烷头基与粗化后纤维表面的羟基反应，通过Si-O-Si键发生化学吸附，形成具有活性端基(即氨基)的分子自组装膜，在活化处理中可以使纤维对钯离子具有更好地吸附效果。而活化处理后的还原处理是将纤维表面吸附钯离子还原成金属钯，并在纤维表面原位沉积。金属钯微粒具有很强的催化活性，从而使玄武岩纤维表面具有高催化活性，诱发镀液中还原剂发生氧化，释放出初生态原子氢并吸附在玄武岩纤维表面使之活化，进而还原镀液中的主盐金属离子，析出的金属以金属钯微粒形成的催化表面为形核中心发生沉积，从而使这种氧化还原反应继续进行，最后得到以玄武岩纤维为核心、金属层为壳的导电玄武岩纤维材料。
本发明所述的一种玄武岩纤维材料表面金属化的方法，该发明具有以下有益效果：
1、本发明采用偶联剂表面改性技术，通过硅烷偶联剂对粗化后的纤维进行改性处理后，可直接吸附活化液中的金属离子，避免了现有技术敏化处理使用的氯化亚锡对环境造成的污染，减少了操作步骤，且将解胶处理替换为还原处理，在一定程度上也避免了解胶液中浓盐酸的危害，适合工业化生产需要。
2、针对常规方法仅靠物理吸附作用制备的镀镍层不牢固、易剥落的问题，本发明技术方案通过氨基类硅烷偶联剂在纤维表面的化学吸附，形成分子自组装膜，该分子自组装膜通过价键理论可以与钯离子形成σ配位键，发生快速化学吸附，获得了表面金属化玄武岩纤维镀层连续致密，镀层与纤维结合性好等有益效果。
附图说明
图1为经KH550偶联处理的玄武岩纤维无捻粗纱施镀30min后的表面SEM图。
图2为经KH550偶联处理的玄武岩纤维无捻粗纱施镀30min后的截面SEM图。
图3为经KH792偶联处理的玄武岩纤维缎纹织物施镀30min后的表面SEM图。
图4为经KH792偶联处理的玄武岩纤维缎纹织物施镀30min后的截面SEM图。
图2和图4中：1、玄武岩纤维，2、金属镍壳层。
具体实施方式
下面通过实施实例对本发明进行具体描述，有必要指出的是以下实施例只用于本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域技术熟练人员可以根据上述发明的内容对本发明做出一些非本质的改进和调整仍属于本发明的保护范围。
实施例1：
一种玄武岩纤维材料表面金属化的方法，包括下述步骤：
(1)将玄武岩纤维无捻粗纱放置在pH＝13的微电水中，浸泡清洗5min，超纯水清洗；
(2)将步骤(1)处理后的纤维置于40g/LNaOH溶液中，50℃下粗化20min后取出，清洗备用；
(3)将步骤(2)处理后的纤维置于3wt％KH550溶液中，50℃下偶联30min后取出，清洗后固化备用；
(4)将步骤(3)处理后的纤维置于0.2g/LPdCl2和0.2mol/L盐酸组成的活化液中，35℃下活化15min后取出，清洗备用；
(5)将步骤(4)处理后的纤维置于3g/L NaH2PO2溶液中，50℃下还原15min后取出，清洗后烘干；
(6)将步骤(5)处理后的纤维置于镀镍液中75℃下反应30min，其中镀镍液组成为24g/L NiSO4·6H2O、30g/L NaH2PO2·H2O、30g/LNa3C6H5O7·2H2O和40g/L(NH4)2SO4，然后用水冲洗，烘干即得表面镀镍玄武岩纤维，其表面形貌与截面形貌如图1和图2所示。
实施例2：
一种玄武岩纤维材料表面金属化的方法，包括下述步骤：
(1)将玄武岩纤维平纹织物放置在pH＝13的微电水中，浸泡清洗10min，超纯水冲洗；
(2)将步骤(1)处理后的纤维置于40g/LNaOH溶液中，50℃下粗化20min后取出，清洗备用；
(3)将步骤(2)处理后的纤维置于3wt％KH792溶液中，50℃下偶联30min后取出，清洗后固化备用；
(4)将步骤(3)处理后的纤维置于0.2g/LPdCl2和0.2mol/L盐酸组成的活化液中，35℃下活化15min后取出，清洗备用；
(5)将步骤(4)处理后的纤维置于3g/L NaH2PO2溶液中，50℃下还原15min后取出，清洗后烘干；
(6)将步骤(5)处理后的纤维置于镀镍液中75℃下施镀30min，其中镀镍液组成为24g/L NiSO4·6H2O、30g/L NaH2PO2·H2O、30g/LNa3C6H5O7·2H2O和40g/L(NH4)2SO4，然后用水冲洗，烘干即得表面镀镍导电玄武岩纤维，其表面形貌与截面形貌如图3和图4所示。
分析图1～图4纤维表面形貌与截面形貌图，可以看出制备的表面金属化玄武岩纤维镀镍层连续且致密，形成了玄武岩纤维—镍核壳结构。

Claims (7)

1.一种玄武岩纤维材料表面金属化的方法，其特征在于：包括下述步骤，
（1）纤维表面亲水处理：在碱性溶液中对玄武岩纤维进行亲水处理并清洗；
（2）偶联：将经步骤（1）亲水处理后的玄武岩纤维置于氨基类的硅烷偶联剂溶液中进行纤维表面偶联改性处理并进行固化处理；
（3）活化：将经步骤（2）偶联处理后的玄武岩纤维置于活化液中进行活化处理并清洗；所述活化液包括氯化钯、盐酸和去离子水，其中氯化钯的浓度为0.1~0.3g/L，盐酸的浓度为0.1~0.3mol/L；所述活化处理温度为30~50℃，时间为10~30min；
（4）还原：将经步骤（3）活化处理后的玄武岩纤维置于还原剂溶液中进行还原处理，随后清洗并干燥；
（5）施镀。
2.根据权利要求1所述的玄武岩纤维材料表面金属化的方法，其特征在于：在纤维表面亲水处理前，采用pH≥11的微电水对纤维表面进行清洗除油。
3.根据权利要求1所述玄武岩纤维材料表面金属化的方法，其特征在于：所述碱性溶液为40~60g/L的氢氧化钠溶液或56~70g/L的氢氧化钾溶液，亲水处理温度为30~50℃，时间为5~30min。
4.根据权利要求1所述的玄武岩纤维材料表面金属化的方法，其特征在于：在步骤（2）中，所述氨基类的硅烷偶联剂溶液包括1~5wt%的氨基类硅烷，氨基类硅烷偶联剂为KH550、KH792、KH602中的至少一种。
5.根据权利要求1所述的一种玄武岩纤维材料表面金属化的方法，其特征在于：所述偶联改性处理的温度为25~60℃，时间为10~30min，固化处理温度为80~120℃，固化时间为10~30min。
6.根据权利要求1所述的玄武岩纤维材料表面金属化的方法，其特征在于：在步骤（4）中，所述还原剂溶液为2~10g/L次磷酸钠溶液或2~10g/L次磷酸钾溶液或3~8g/L的硼氢化钠溶液，还原处理温度25~50℃，处理时间为10~50min，干燥的温度为70~80℃，干燥的时间为10~20min。
7.根据权利要求1所述的玄武岩纤维材料表面金属化的方法，其特征在于：在步骤（5）中，所述施镀是指在纤维表面镀镍、铜、金、银、铁金属及其合金。
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