CN106757008B - 一种wc/非晶复合涂层及其制备方法 - Google Patents
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Abstract
本发明提供一种WC/非晶复合涂层及其制备方法。将Fe基非晶合金粉末预铺在合金钢表面，以WC‑Co陶瓷硬质合金为电极，采用电火花沉积技术制得所述涂层。其中，以质量百分比计，Fe基非晶粉末的成分为Mo：28.5～30.0％；Co：8.0～9.0％；Cr:13.0～13.8％；Si:1.5～2.0％；Y：2.0～3.0％；其余为Fe。电火花沉积工艺参数为：电压50～150V，电容10～300μF，放电脉冲频率60～2000Hz，沉积枪转速为500rpm，Ar气流量3～9L/min。本发明制备的涂层具有高的硬度及耐磨性，可应用于金属零部件表面改性，修复及再制造，可显著改善材料的表面性能。
Description
技术领域
本发明涉及一种WC/非晶复合涂层以及制备该涂层的方法，属于表面涂层和表面改性领域。
背景技术
非晶态合金长程无序短程有序的独特原子结构，使其具有高强度、高硬度、高弹性极限、高耐磨耐蚀及理想的磁学、电学特性能等一系列优异的物理化学和力学性能，受到了广泛关注，具有广阔的应用前景。目前，已开发出Zr基、Cu基、Fe基、Ni基、Ti基、稀土基等一系列具有较大玻璃形成能力的多元合金体系。但较小的尺寸和非晶材料固有的脆性仍然是制约其作为结构材料应用的关键。非晶复合涂层可有效解决非晶的脆性和尺寸问题，突破其应用瓶颈。如学者利用喷涂技术、激光熔覆等技术在金属基体表面成功制备了非晶复合涂层，获得优异的耐磨耐蚀等性能。但喷涂非晶涂层的膜基结合力较差，很难用于工况复杂的苛刻环境。激光熔覆制备的非晶涂层可以与基材形成冶金结合，但激光器昂贵，制备成本较高。
电火花沉积技术(Electro-spark Deposition，简称ESD)是利用高能量密度电能将电极材料熔化，并以等离子态沉积到工件表面的一种脉冲微弧焊工艺。该工艺是将电极材料作为工作阳极，被沉积金属工件作为阴极，在保护介质中电极材料与工件接触，产生火花放电，在10-5～10-6s的时间内接触部位可达到8,000～25,000K的高温，使得材料瞬间熔化，在微电场的作用下离子态的电极材料高速转移到工件表面，形成与基材呈冶金结合的沉积层。由于电火花沉积技术采用脉冲加热，其放电频率高、放电区域小、能量集中，加热和冷却速度极快(可达105-106K/s)，沉积层极易形成非晶纳米晶组织。如Liu等以Fe-Cr-Mo-Gd-C-B非晶棒为电极在304不锈钢制备沉积层。研究发现，沉积层厚度约为30μm，其中含有非晶相，与基材呈冶金结合，硬度可达1542kg/mm2。
现有的电火花沉积非晶涂层专利(CN104032252A)，利用高纯Al、Ni、La进行真空中频感应熔炼，获得母合金，然后通过铜模喷铸法获得电极，利用电火花沉积技术在铝合金表面获得非晶层。该技术需要专门制作非晶合金作为电极，电极的成分与组织结构直接影响沉积层的组织与性能；一种基于电火花沉积的非晶纳米晶涂层制备方法的专利(CN104513947A)，以FeB粉、Mo粉、Fe粉、Mn粉、Cr粉、Ni粉和V粉按照比例混合，加成型剂，经球磨，成型及真空烧结后获得电极，然后利用电火花沉积技术获得非晶纳米晶沉积层。
发明内容
本发明提供一种在合金钢基材表面可快速制备的WC/非晶复合涂层及制备方法。将Fe基非晶合金粉末预先铺在合金钢基材表面，以WC-Co为电极，采用电火花沉积技术在合金钢基材表面制备WC/非晶复合涂层。
本发明所采用的Fe基非晶合金粉末的成分为：以质量百分比计，Mo：28.5～30.0％；Co：8.0～9.0％；Cr:13.0～13.8％；Si:1.5～2.0％；Y:2.0～3.0％；其余为Fe。铁基非晶合金粉末用气体雾化方法制备，制备粉末为完全非晶态结构，粉末粒度范围在：30-100μm。
上述成分中，各个元素的主要作用是：
Mo：细化组织，提高沉积层韧性和耐磨性，降低裂纹敏感性；
Co：提高沉积层的热强性、硬度和耐磨性；
Cr：提高电极电位，防止电化学腐蚀，提高沉积层耐蚀性；
Si：提高沉积层的抗氧化能力，提高沉积层的成型质量；
Y：改善沉积层成型质量，提高沉积层的非晶形成能力。
发明人经过长期试验得出本发明采用以下配比时，达到的效果最好。以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：29％；Co：8.5％；Cr：13.5％；Si:1.8％；Y:2.5％；其余为Fe。
本发明选用WC-Co陶瓷硬质合金作为电极，其成分为，WC：85～92％，Co：8～15％。电极直径为3mm。发明人经过长期试验发现，采用WC-10Co电极的沉积层与基体间结合较好，且具有较高的硬度和耐磨性。优选WC-10Co电极，其成分为：WC：90％，Co：10％。
本发明所述的一种WC/非晶复合涂层的制备方法，采用预涂覆技术，先在合金钢基材上涂覆一层Fe基非晶粉末，以WC-Co为电极，利用Spark Depo MODEL 300型电火花沉积设备进行沉积，具体工艺参数为：电压50～150V，电容10～300μF，放电脉冲频率60～2000Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量3～9L/min。沉积层厚度、表面粗糙度等沉积层质量与工艺参数密切相关。发明者经过大量试验发现，电压、电容和频率对沉积层厚度的影响是通过改变电极间放电能量实现的，沉积电容、电压越大，电极间的放电能量越大；放电频率越高，单位时间内的放电次数增加，电极材料转移量增大，厚度增大。电容、电压和放电频率三者中，电压对沉积层厚度的影响最大。电容、电压与沉积层粗糙度成正比，频率与沉积层粗糙度成反比。电容、电压越大，沉积层粗糙度越大；放电频率越大，沉积层粗糙度越小。另外，沉积工艺也会影响沉积层缺陷。电压、电容对沉积层缺陷的影响是通过改变电极间放电能量实现的，能量过小会在基体与沉积层的过渡区中产生未融合裂纹；能量过大，会由于较大的热应力和形变应力产生气孔和微裂纹等缺陷。为兼顾沉积层厚度，沉积层质量以及沉积效率，较佳的工艺为两遍沉积，具体参数为，第一遍：电压100V，电容30μF，放电脉冲频率300Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。第二遍，电压50V，电容10μF，放电脉冲频率2000Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。
本发明所制备的涂层主要由W3C和非晶组成，为WC/非晶复合涂层，涂层硬度值高达2100HV，摩擦系数在0.1～0.2之间。WC具有高硬度、高强度、高弹性模量及化学稳定性等特性。WC/非晶复合涂层在摩擦载荷作用下，可通过弹性变形调节其与摩擦副之间的载荷作用与分布，从而减少或避免对摩擦副的划伤，从而起到降低摩擦系数的作用。因此，本发明的WC/非晶复合涂层，与合金钢基体呈冶金结合，表面粗糙度较低，具有低的摩擦系数、高的硬度及耐磨性。本发明的涂层及制备技术，可用于零部件表面改性、修复与再制造，有巨大的应用前景。
附图说明
图1为预涂粉末和沉积层的XRD图谱；
可见预涂粉末的XRD图谱，只有一个漫散包，为完全非晶态。沉积层的XRD图谱在2θ＝35～50度之间也出现了明显的漫散包，说明有非晶组织存在。同时，也发现在漫散包上还叠加着明锐的衍射峰，经标定，这些衍射峰主要是W3C相。
图2为沉积层的表面形貌；
可见，涂层主要由熔滴沉积点和放电凹坑逐层覆盖形成，呈“火山坑”和“溅射状”花样形貌。这主要是由于电火花放电瞬间在电极与基体间产生的高温、高压使电极瞬间熔化，甚至汽化，在微电场的作用下，熔化的电极材料高速溅落在基材表面并快速凝固而形成“溅射状”花样。同时放电高温高压，可能使某些区域瞬间汽化，在放电弧的冲击压力下，形成“火山坑”形貌。
图3为沉积层的截面SEM图及界面处成分分布；
图4为为沉积层的截面SEM图及界面处成分分布(省略色彩)；
可见，沉积层与基体结合牢固，且在结合区Fe，Si元素明显发生了扩散。说明电火花沉积并非简单的电极材料转移涂镀过程，而是电极和基体材料各元素原子沉积时发生剧烈的扩散和重新合金化，使沉积层与基材实现了冶金结合。
图5为沉积层纵截面的硬度变化曲线；
可见，沉积层分为涂层区，过渡区和基体3个区域。从涂层到基体硬度值呈逐渐下降趋势。基体硬度在200HV左右，而WC/非晶涂层最高硬度值达到了2100HV，10倍于基体材料的硬度值。沉积层具有较高的显微硬度主要是由于沉积过程中完全熔融的基体与电极材料形成冶金结合，在基体材料表面形成了弥散分布的硬质相碳化物；另外，由于电火花沉积是一个先经快速加热快速冷却的过程，沉积过程中形成了大量的非晶组织，从而使沉积层具有较高的硬度。
图6为合金钢基体与沉积层摩擦系数随时间的变化曲线；
可见，基体和沉积涂层的摩擦曲线都分为跑合磨损和稳定磨损两个阶段。在运行初期，摩擦副试样表面粗糙不平，两者之间的实际接触面积较小，磨损率较大，摩擦系数逐渐升高。但随磨损进行，试样表面粗糙度降低，摩擦进入稳定磨损阶段，摩擦系数趋于稳定。稳定后，基体的平均摩擦系数约为0.4，WC/非晶沉积层的平均摩擦系数约为0.12。所制备的涂层主要由W3C和非晶组成。WC具有高硬度、高强度、高弹性模量及化学稳定性等特性。WC/非晶复合涂层在摩擦载荷作用下，可通过弹性变形调节其与摩擦副之间的载荷作用与分布，从而减少或避免对摩擦副的划伤，降低摩擦系数。平均摩擦系数越小，材料的减磨性越好。说明沉积层具有良好的减摩特性。
具体实施方式
实施例1
一种在合金钢基材表面可快速制备的WC/非晶复合涂层及制备方法。将Fe基非晶合金粉末预先铺在合金钢基材表面，以WC-Co为电极，采用电火花沉积技术在合金钢基材表面制备WC/非晶复合涂层。其中，以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：28.5％；Co：9.0％；Cr：13.0％；Si：2.0％；Y：2.0％，其余为Fe。
1)制备非晶合金粉末：
首先将上述所需成分用真空熔炼的方法获得母合金，然后将母合金放入雾化炉中，由气体雾化技术制备非晶合金粉末。雾化后筛选粒度范围在30-100μm粉末作为预涂覆粉末。粉末的x射线衍射图如图1所示，由图可见，粉末为完全非晶态。
2)选用45Mn2钢为基体材料，将基体材料表面除锈，磨平，再依次从100号水砂纸打磨至600号，打磨后在丙酮溶液中超声清洗10min去除油垢和污渍。
3)使用电极材料为WC-8Co，直径为3mm，成分为：WC：92％，Co：8％。
4)利用Spark Depo MODEL 300型电火花沉积设备进行沉积。具体工艺参数为：电压50V，电容10μF，放电脉冲频率60Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量3L/min。
实施例2
一种在合金钢基材表面可快速制备的WC/非晶复合涂层及制备方法。将Fe基非晶合金粉末预先铺在合金钢基材表面，以WC-Co为电极，采用电火花沉积技术在合金钢基材表面制备WC/非晶复合涂层。其中，以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：29％；Co：8.5％；Cr：13.5％；Si:1.8％；Y:2.5％；其余为Fe。
步骤(1)和(2)均与实施例1相同。步骤(3)中所采用电极材料为WC-10Co，直径为3mm，成分为：WC：90％，Co：10％。调整步骤(4)中的工艺参数如下：电压100V，电容300μF，放电脉冲频率300Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。
实施例3
一种在合金钢基材表面可快速制备的WC/非晶复合涂层及制备方法。将Fe基非晶合金粉末预先铺在合金钢基材表面，以WC-Co为电极，采用电火花沉积技术在合金钢基材表面制备WC/非晶复合涂层。其中，以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：30％；Co：8.0％；Cr：13.8％；Si：1.5％；Y：3.0％；其余为Fe。
步骤(1)和(2)均与实施例1、2相同。步骤(3)中所采用电极材料为WC-15Co，直径为3mm，成分为：WC：85％，Co：15％。，调整步骤(4)中的工艺参数如下：电压150V，电容100μF，放电脉冲频率500Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量9L/min。
实施例4
一种在合金钢基材表面可快速制备的WC/非晶复合涂层及制备方法。将Fe基非晶合金粉末预先铺在合金钢基材表面，以WC-Co为电极，采用电火花沉积技术在合金钢基材表面制备WC/非晶复合涂层。其中，以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：29％；Co：8.5％；Cr：13.5％；Si:1.8％；Y:2.5％；其余为Fe。
步骤(1)和(2)均与实施例1、2、3相同。步骤(3)中所采用电极材料为WC-10Co，直径为3mm，成分为：WC：90％，Co：10％。，调整步骤(4)中的工艺参数如下：采用两遍沉积工艺，第一遍的沉积参数为：电压100V，电容30μF，放电脉冲频率300Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。第二遍的沉积参数为：电压50V，电容10μF，放电脉冲频率2000Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。实验例：
将实施例4所述的非晶粉末预涂覆在45Mn2钢表面，以WC-10Co为电极，采用SparkDepo MODEL 300型电火花沉积设备按照实施例4中的工艺参数进行沉积实验，沉积层的组织结构与性能结果如下：
(1)沉积层的物相。对实施例4沉积的涂层进行物相分析，涂层的X射线衍射图如图1所示。由图分析可知，涂层主要由涂层主要由非晶和W3C相组成，为WC/非晶复合涂层。
(2)沉积层的表面形貌。对实施例4沉积的涂层进行表面形貌分析，如图2所示。由图可知，涂层主要由熔滴沉积点和放电凹坑逐层覆盖形成，呈“火山坑”和“溅射状”花样形貌。
(3)沉积层的厚度与结合状况。对实施例4沉积的涂层纵截面进行SEM和线扫描能谱分析，如图3、4所示。由图可知，涂层厚度约为20μm，沉积层与基体结合牢固，且在结合区Fe，Si元素明显发生了扩散实现了冶金结合。
(4)沉积层的硬度。对实施例4沉积层的硬度进行分析测试。采用HV-100A型显微硬度计，载荷25g，保载时间10s。由沉积层表面至基体每隔0.1mm的距离测一个数据，每个点测试三次，取平均值，测试结果如图5所示。由图可知，从涂层到基体硬度值呈逐渐下降趋势。基体硬度在200HV左右，而WC/非晶涂层最高硬度值达到了2100HV，约是基体硬度的10倍。
(5)沉积层的摩擦磨损性能。对实施例4沉积层的摩擦磨损性能进行分析测试。采用M-2000A型多功能摩擦磨损试验机，采用环块磨擦磨损形式，对磨件为轴承钢(GCr15)，表面硬度为HRC63。施加载荷30N，摩擦时间40min，试样转速为360r/min。沉积层摩擦系数随时间变化的曲线如图6所示。由图可知，基体的平均摩擦系数约为0.4，WC/非晶沉积层的平均摩擦系数约为0.12。采用称重法计算基体和沉积层的磨损率分别为：0.37％和0.043％。沉积层的耐磨性约是基体的8.6倍。
Claims (3)
1.一种WC/非晶复合涂层，其特征在于：在合金钢基体表面预铺一层铁基非晶合金粉末，以WC-Co为电极，采用电火花沉积技术制得，其中，以质量百分比计，所述铁基非晶合金粉末的成分为：Mo：28.5～30.0％；Co：8.0～9.0％；Cr:13.0～13.8％；Si:1.5～2.0％；Y:2.0～3.0％；其余为Fe；
以质量百分比计，所述的WC-Co电极的成分为WC：85～92％，Co：8～15％；
其制备方法为：采用预涂覆技术，先在合金钢基材上涂覆一层Fe基非晶粉末，以WC-Co为电极，利用Spark Depo MODEL 300型电火花沉积设备进行沉积，具体工艺参数为：电压50～150V，电容10～300μF，放电脉冲频率60～2000Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量3～9L/min；
所述铁基非晶合金粉末用气体雾化方法制备，粉末粒度范围在：30-100μm，为完全非晶态；
采用预涂覆技术，先在合金钢基材上涂覆一层Fe基非晶粉末，以WC-Co为电极，利用Spark Depo MODEL 300型电火花沉积设备进行两遍沉积，具体工艺参数为：第一遍：电压100V，电容30μF，放电脉冲频率300Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min；第二遍，电压50V，电容10μF，放电脉冲频率2000Hz，沉积枪转速为500rpm，沉积过程采用Ar气保护，Ar气流量5L/min。
2.根据权利要求1所述的一种WC/非晶复合涂层，其特征在于：所述的涂层主要由W3C和非晶组成，与合金钢基体之间呈冶金结合。
3.根据权利要求1所述的一种WC/非晶复合涂层，其特征在于：所述的涂层硬度值高达2100HV，摩擦系数在0.1～0.2之间。
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