CN102345144A - 一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法 - Google Patents
一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法 Download PDFInfo
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Abstract
本发明涉及可加工层状钛硅铝碳陶瓷领域,特别提供了一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法,避免镍基体与钛硅铝碳之间发生相互扩散或反应等问题。在含有硫酸镍、氯化镍和硼酸的镀镍液中,添加钛硅铝碳粉末使之在镀液中充分悬浮,在镍离子阴极还原的同时,将固体颗粒吸附或包覆与金属共沉积制备复合涂层。镀液中硫酸镍的浓度为240-300g/L,氯化镍的浓度为45-75g/L,硼酸的浓度为37-53g/L,钛硅铝碳的固相含量为2-60g/L,pH值范围为3.5-5.0,温度为49-61℃,电沉积时镀液处于搅拌状态,搅拌速率为200-600rpm,电流密度为20-80mA/cm2,沉积时间为15-60min。本发明可以在较低温度(<100℃)及较短时间内电化学共沉积制备得到固体颗粒分散均匀、致密度好的镍基钛硅铝碳复合涂层。
Description
技术领域
本发明涉及可加工层状钛硅铝碳陶瓷领域,特别提供了一种利用电化学共沉积制备镍/钛硅铝碳(Ti3SiAlC2)复合涂层的方法。
背景技术
镍是一种非常重要的在高温下应用的工程材料,然而刚性低、抗氧化性和耐磨性差限制了它在诸如内燃机及铸造模具方面的应用。
文献1-5(Thin Solid Films 95(1982)133;Surf.Coat.Technol.148(2001)171;J.Electrochem.Soc.110(1963)557;Mater.Chem.Phys.78(2003)574;Surf.Coat.Technol.192(2005)331)中报道了将镍与SiC、Al2O3、SiO2、ZrO2及TiO2等硬质相颗粒复合会使镍的力学性能如耐磨性、弯曲强度和硬度有明显的提高。
此外,文献6-9(Surf.Coat.Technol.157(2002)282;Mater.Lett.53(2002)238;Met.Finish.65(1967)52;Mater.Des.28(2007)1374)中报道了用软质相颗粒如聚四氟乙烯(PTFE)、聚乙烯(PE)、MoS2或石墨等增强的镍基复合涂层具有优异的自润滑性,可用于精密机器部件和滑动轴承方面。
钛硅碳(Ti3SiC2)及其固溶体(Ti3SiAlC2)是新型的三元层状陶瓷,具有低密度、高刚性,良好的可加工性、抗热震性、高温抗氧化性及相对低的硬度和剪切强度。因此,将钛硅碳(TiSiC2)与镍复合有望提高金属镍的耐磨性、自润滑性、高温抗氧化及耐腐蚀性。此外,钛硅碳(Ti3SiC2)的热膨胀系数与镍很匹配会使得镍基复合物的内应力小,从而可以更加拓展其在高温方面的应用。
发明内容:
本发明提出的目的在于提供一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法,避免镍基体与钛硅铝碳之间发生相互扩散或反应等问题。
本发明的技术方案是:
一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法,该方法在含有硫酸镍(NiSO4·6H2O)、氯化镍(NiCl2·6H2O)和硼酸(H3BO3)的镀镍液中,添加钛硅铝碳(Ti3SiAlC2)粉末使之在镀液中充分悬浮,在较低温度(50-60℃)及较短时间内电化学共沉积制备得到固体颗粒分散均匀、致密度好的镍基钛硅铝碳(Ti3SiAlC2)复合涂层,具体如下:
1)原料组成及成分范围:
以硫酸镍(NiSO4·6H2O)、氯化镍(NiCl2·6H2O)和硼酸(H3BO3)配置镀镍液;其中,硫酸镍(NiSO4·6H2O)的浓度为240-300g/L,氯化镍(NiCl2·6H2O)的浓度为45-75g/L,硼酸(H3BO3)的浓度为37-53g/L,其余为水;添加钛硅铝碳(Ti3SiAlC2)粉末使之在镀液中充分悬浮,悬浮液中钛硅铝碳(Ti3SiAlC2)的固相含量为2-60g/L。
2)制备工艺:
用氢氧化钠调节镀液pH值范围为3.5-5.0,电沉积时镀液温度为49-61℃,电流密度为20-80mA/cm2,沉积时间为15-60min,搅拌速率为200-600rpm,在镍离子阴极还原的同时,将固体颗粒吸附或包覆与金属共沉积制备复合涂层,获得钛硅铝碳颗粒分散均匀、致密的镍/钛硅铝碳复合涂层厚度为2-10μm。
本发明中,钛硅铝碳(Ti3SiAlC2)粉末的平均粒度为4-5μm。
本发明的优点是:
1、工艺简单、成本低、环境友好。电化学共沉积在较低温度(<100℃)下即可进行,复合涂层中钛硅铝碳(Ti3SiAlC2)的百分含量可以根据镀液中钛硅铝碳(Ti3SiAlC2)的浓度、电流密度、沉积时间等进行控制;
2、复合涂层的性能优异。采用电化学共沉积制备的镍基钛硅铝碳(Ti3SiAlC2)复合涂层与基体结合强度高、致密度高、增强相颗粒的分散性好。
附图说明
图1电化学共沉积制备镍/钛硅铝碳复合涂层的装置示意图。
图2电化学共沉积制备镍/钛硅铝碳复合涂层的表面形貌。
图3电化学沉积制备的纯镍涂层与镍/钛硅铝碳复合涂层的X射线衍射谱。
图4电化学沉积制备的纯镍涂层与镀液中含有不同浓度的钛硅铝碳镍/钛硅铝碳复合涂层的X射线衍射谱。
图5电化学共沉积制备镍/钛硅铝碳复合涂层的表面形貌。其中,(a)图为由含有5g/L钛硅铝碳粉末的镀液电化学沉积制备得到的镍/钛硅铝碳复合涂层表面形貌;(b)图为由含有25g/L钛硅铝碳粉末的镀液电化学沉积制备得到的镍/钛硅铝碳复合涂层表面形貌。
图6电化学共沉积制备的镍/钛硅铝碳复合涂层中钛硅铝碳(Ti3SiAlC2)的百分含量随镀液中钛硅铝碳(Ti3SiAlC2)浓度变化的关系曲线。
图7电化学共沉积制备镍/钛硅铝碳复合涂层的表面形貌。
具体实施方式
实施例1
如图1所示,电化学沉积装置的结构如下:将工作电极1(不锈钢)和对电极2(纯镍)浸入含有钛硅铝碳粉末的镀镍溶液3中,通过电源4施加电流。用温度计5监控镀液的温度,用磁力搅拌器控制对镀液的搅拌速度,盛放镀镍溶液3的容器设置于水浴锅6中。
以硫酸镍(NiSO4·6H2O)、氯化镍(NiCl2·6H2O)和硼酸(H3BO3)配置镀镍液;其中,硫酸镍(NiSO4·6H2O)的浓度为250g/L,氯化镍(NiCl2·6H2O)的浓度为45g/L,硼酸(H3BO3)的浓度为40g/L,其余为水;将平均粒度为4.4μm的钛硅铝碳(Ti3SiAlC2)均匀分散在镀液中充分悬浮,悬浮液中钛硅铝碳(Ti3SiAlC2)的浓度为50g/L,用氢氧化钠调节镀液pH为3.8,电化学沉积的装置如图1所示。
镀液在温度为60±1℃及不断搅拌状态下,以搅拌速率为200rpm、电流密度为50mA/cm2进行恒电流电化学沉积,沉积时间为30min,由扫描电镜照片可以观察到此条件下制备得到的镍/钛硅铝碳复合涂层中钛硅铝碳颗粒分散均匀、致密,镍/钛硅铝碳复合涂层厚度为2-10μm,如图2所示。
如图3所示,经X射线衍射分析复合涂层中存在钛硅铝碳(Ti3SiAlC2)的衍射峰,且钛硅铝碳(Ti3SiAlC2)的存在影响了镍的择优取向。
实施例2
以硫酸镍(NiSO4·6H2O)、氯化镍(NiCl2·6H2O)和硼酸(H3BO3)配置镀镍液;其中硫酸镍(NiSO4·6H2O)的浓度为260g/L,氯化镍(NiCl2·6H2O)的浓度为60g/L,硼酸(H3BO3)的浓度为50g/L,其余为水;将平均粒度为4μm的钛硅铝碳(Ti3SiAlC2)均匀分散在镀液中充分悬浮,悬浮液中钛硅铝碳(Ti3SiAlC2)的浓度为5、15、25、50g/L,用氢氧化钠调节镀液pH为4.0,电化学沉积的装置如图1所示,镀液在温度为55土1℃及不断搅拌状态下,以搅拌速率为400rpm、电流密度为20mA/cm2进行恒电流电化学沉积,沉积时间为30min,得到钛硅铝碳颗粒分散均匀、致密的镍/钛硅铝碳复合涂层,镍/钛硅铝碳复合涂层厚度为2-10μm。
如图4所示,a、b、c、d和e分别表示纯镍涂层、钛硅铝碳(Ti3SiAlC2)的浓度为5、15、25、50g/L下制备的镍/钛硅铝碳复合涂层,经X射线衍射分析复合涂层中存在钛硅铝碳(Ti3SiAlC2)的衍射峰,且随着镀液中钛硅铝碳(Ti3SiAlC2)浓度的增加复合涂层中钛硅铝碳(Ti3SiAlC2)的衍射峰逐渐增强;
如图5所示,镀液中钛硅铝碳(Ti3SiAlC2)的浓度分别为5g/L和25g/L制备得到的镍/钛硅铝碳复合涂层表面形貌,随着镀液中钛硅铝碳(Ti3SiAlC2)浓度的增加,复合涂层中钛硅铝碳的含量也随着增加。即可以通过控制镀液中钛硅铝碳(Ti3SiAlC2)浓度的方法来控制复合涂层中钛硅铝碳的含量。
如图6所示,复合涂层中钛硅铝碳(Ti3SiAlC2)的百分含量随镀液中钛硅铝碳(Ti3SiAlC2)浓度变化的关系曲线,随着镀液中钛硅铝碳(Ti3SiAlC2)浓度的增加,复合涂层中钛硅铝碳的含量也随着增加至达到一个饱和的趋势。
实施例3
以硫酸镍(NiSO4·6H2O)、氯化镍(NiCl2·6H2O)和硼酸(H3BO3)配置镀镍液;其中,硫酸镍(NiSO4·6H2O)的浓度为250g/L,氯化镍(NiCl2·6H2O)的浓度为45g/L,硼酸(H3BO3)的浓度为40g/L,其余为水;将平均粒度为4μm的钛硅铝碳(Ti3SiAlC2)均匀分散在镀液中充分悬浮,悬浮液中钛硅铝碳(Ti3SiAlC2)的浓度为50g/L,用氢氧化钠调节镀液pH为4.5,电化学沉积的装置如图1所示。
镀液在温度为50土1℃及不断搅拌状态下,以搅拌速率为500rpm、电流密度为55mA/cm2进行恒电流电化学沉积,沉积时间为15min,得到钛硅铝碳颗粒分散均匀、致密的镍/钛硅铝碳复合涂层,镍/钛硅铝碳复合涂层厚度为2-10μm,如图7所示。
关于制备镍基复合材料的方法有很多,与高温热冶或粉末冶金相比,电化学共沉积具有沉积速率快、操作温度低(<100℃)、固体颗粒在复合涂层中分散均匀等优点。本发明可以在较低温度(<100℃)及较短时间内电化学共沉积制备得到固体颗粒分散均匀、致密度好的镍基钛硅铝碳(Ti3SiAlC2)复合涂层。采用这种方法制备镍/钛硅铝碳(Ti3SiAlC2)复合涂层可以避免镍基体与钛硅铝碳之间发生相互扩散或反应。
Claims (1)
1.一种利用电化学共沉积制备镍/钛硅铝碳复合涂层的方法,该方法的特征在于:
1)原料组成及成分范围:
以硫酸镍、氯化镍和硼酸配置镀镍液;其中,硫酸镍的浓度为240-300g/L,氯化镍的浓度为45-75g/L,硼酸的浓度为37-53g/L,其余为水;添加钛硅铝碳粉末使之在镀液中充分悬浮,悬浮液中钛硅铝碳的固相含量为2-60g/L;
2)制备工艺:
pH值范围为3.5-5.0,温度为49-61℃,电沉积时电流密度为20-80mA/cm2,沉积时间为15-60min,搅拌速率为200-600rpm。
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CN103276419A (zh) * | 2013-06-08 | 2013-09-04 | 沈阳化工大学 | 一种复合脉冲高温防护涂层的制备方法 |
CN109402680A (zh) * | 2018-11-02 | 2019-03-01 | 徐州晶迪电子有限公司 | 一种mos晶体管用掩模板材料的制备方法 |
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CN103276419A (zh) * | 2013-06-08 | 2013-09-04 | 沈阳化工大学 | 一种复合脉冲高温防护涂层的制备方法 |
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CN109402680B (zh) * | 2018-11-02 | 2021-11-16 | 徐州晶迪电子有限公司 | 一种mos晶体管用掩模板材料的制备方法 |
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