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CN112030161B - 一种用于激光熔覆的高熵合金粉末及其使用方法 - Google Patents

一种用于激光熔覆的高熵合金粉末及其使用方法 Download PDF

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CN112030161B
CN112030161B CN202011052429.7A CN202011052429A CN112030161B CN 112030161 B CN112030161 B CN 112030161B CN 202011052429 A CN202011052429 A CN 202011052429A CN 112030161 B CN112030161 B CN 112030161B
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entropy alloy
alloy powder
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CN112030161A (zh
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刘洪喜
刘径舟
郝轩弘
邸英南
蔺健全
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Kunming University of Science and Technology
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Abstract

本发明公开一种用于激光熔覆的高熵合金粉末及其使用方法，属于激光熔覆领域。所述合金粉末为CoCrFeMnNiCx，x取值0.1～0.15。具体方法为：对45钢基材进行表面预处理，将称量好的CoCrFeMnNi高熵合金粉末与不同含量纳米C粉末混合均匀后预置在预处理基体表面形成预制层，然后置于80～90℃下恒温处理8～12h。在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆。本发明所述方法制备出性能优于CoCrFeMnNi高熵合金涂层的CoCrFeMnNiCx高熵合金涂层，涂层与基体可以达到良好的冶金结合，涂层具有良好的宏观形貌与较高的硬度，可用于高温、耐磨、耐腐蚀等复杂工作情况。

Description

一种用于激光熔覆的高熵合金粉末及其使用方法
技术领域
本发明涉及一种用于激光熔覆的高熵合金粉末及其使用方法，属于激光表面改性领域。
背景技术
45钢是广泛应用于机械制造中各种重要的结构零件，特别是在交变负荷下工作的连杆、螺栓、齿轮及轴类等常用零件，经调制处理后具有良好的综合力学性能。但随着现代化生产工艺对一些主要零件性能的要求日益提高，45钢表面的硬度、耐磨性以及抗腐蚀能力已远远不能满足其需求。
高熵合金即含有多种主要元素的合金，合金元素数目n≥5。与传统合金以一种或两种元素为主要组元不同，高熵合金则是将多种元素以等摩尔或者近等摩尔混合在一起得到的新型合金，其中每种元素的含量远大于5％且不高于35％；由于高熵效应，高熵合金具备一系列优异的性能，如：高硬度、高耐磨性、高耐腐蚀性、高电阻率等。具有单一面心立方(fcc)相结构的等原子CoCrFeMnNi高熵合金的良好性能包括应变硬化，即使在低温条件下也会导致非常高的拉伸伸长和异常的断裂韧性，但CoCrFeMnNi高熵合金材料在硬度强度等方面仍存在一定的局限性，不能满足日趋复杂严苛的工作环境。
激光束功率密度高，熔池冷却速度快，可获得非平衡凝固组织；热输入小，基材热影响区小；自动化程度高，可实现三维自化加工和复杂曲面加工；界面冶金结合，结合强度高；熔池温度高，可加工高熔点材料；熔覆层的厚度范围大。单次涂覆厚度可在0.2～2.0mm灵活调整；能进行选区熔敷，材料消耗少，具有卓越的性能价格比。所以本发明采用激光熔覆方法，在45钢表面熔覆CoCrFeMnNiCx高熵合金材料涂层。
发明内容
本发明的目的在于提供一种用于激光熔覆的高熵合金粉末，所述合金粉末为CoCrFeMnNiCx，x取值0.1～0.15。
本发明的另一目的在于提供所述高熵合金粉末用于制备激光熔覆涂层的方法，具体包括以下步骤：
(1)对45钢基材进行表面预处理：打磨，清洗，干燥后备用；
(2)按比例称量等原子比的CoCrFeMnNi高熵合金粉末与纳米C粉末，称量完毕后进行机械混合；
(3)将混合好的粉末与无水乙醇混合调制成糊状，使用模具将其粘接在钢基体预定位置得到预制涂层，然后进行干燥，在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆。
优选的，本发明步骤(2)中CoCrFeMnNi高熵合金粉末的平均粒度小于25μm，粉末纯度不小于99.9％；纳米C粉的平均粒度为30nm～50nm，纯度不小于99.99％。
优选的，本发明步骤(3)中干燥条件为：预制涂层厚度为0.2mm～2mm，于80～90℃下恒温处理8～12h。
优选的，本发明步骤(3)激光熔覆是通过CO2激光器进行的，具体条件为：激光功率为3.7～4.2kW，扫描速度为200～450mm/min，光斑直径为3.0～4.0mm，保护气体为氮气、氩气或二者混合气体，气体流量为15～35L/min，保护气氛的气压为0.80MPa～1.20MPa。
本发明的原理：具有单一面心立方(fcc)相结构的等原子CoCrFeMnNi高熵合金的良好性能包括应变硬化，即使在低温条件下也会导致非常高的拉伸伸长和异常的断裂韧性，但CoCrFeMnNi高熵合金材料在硬度强度等方面仍存在一定的局限性，不能满足日趋复杂严苛的工作环境。本发明添加纳米C粉，降低了CoCrFeMnNi高熵合金的层错能，增加了层间摩擦应力，导致了室温下的平面滑动；进一步提高了涂层材料的强度。
本发明的有益效果：
(1)激光熔覆法具有光束的能量密度高，加热、冷却速度快的优点；因此激光熔覆组织是一种快速凝固组织，有利于获得较好的性能；另外，激光熔覆涂层与基体材料之间呈冶金结合，使涂层与基体之间的结合较为紧密。
(2)本发明所用熔覆材料为CoCrFeMnNi高熵合金粉末，相较于其他单质、化合物材料熔覆后元素的扩散较少，保证涂层材料中不会大量含有其他非CoCrFeMnNi相。同时向CoCrFeMnNi高熵合金粉末中添加纳米C粉末，提高了涂层材料的强度。
(3)本发明通过激光熔覆技术制备的涂层宏观形貌良好，无明显气孔和裂纹等缺陷，稀释率低且界面冶金结合紧密；本发明制备的CoCrFeMnNi高熵合金的涂层具有较高硬度，耐磨及耐腐蚀性。
附图说明
图1为本发明实施例1激光熔覆涂层横截面的金相组织；
图2为本发明实施例1激光熔覆涂层结合区的金相组织；
图3为本发明实施例1激光熔覆涂层的XRD谱图；
图4为本发明实施例1熔覆涂层与基体的显微硬度。
具体实施方式
下面结合实施例对本发明作进一步说明，但本发明保护范围不局限于所述内容。
本发明的实施例1～3中基体材料45钢的化学成分如表1所示：
表145钢的化学成分
元素 C Si Mn Cr Ni Cu Fe
质量分数％ 0.42～0.50 0.17～0.37 0.50～0.80 ≤0.25 ≤0.30 ≤0.25 余量
实施例1
一种高熵合金粉末用于制备激光熔覆层的方法，具体包括以下步骤：
(1)对45钢基材进行表面预处理：先用200～800目砂纸打磨金属基材表面去除氧化膜，并用水冲洗干净，然后在无水乙醇中进行超声波清洗，去除表面残存的油污及杂质；清洗完毕后，在60℃真空环境下干燥0.5h后备用；打磨要求完全去除金属基体表面氧化膜且无粗大划痕亮，磨痕的方向一致且表面光亮。
(2)按CoCrFeMnNiC0.1的原子比称量CoCrFeMnNi高熵合金粉末与纳米C粉末，称量完毕后进行机械混合，其中纳米C粉的平均粒度为50nm，纯度不小于99.99％。
(3)将称量好的混合粉末与纯度不低于99.7％的无水乙醇混合调制成糊状，使用模具将其粘接在45钢基体预定位置得到1mm厚的预制涂层，然后置于90℃下恒温处理10h；在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆，得到由呈点阵分布的熔覆点构成的熔覆涂层；所述激光熔覆是通过CO2激光器进行的，激光功率为4.2kW，扫描速度为450mm/min，光斑直径为3mm，保护气体为Ar与N2的混合气体，气体流量为25L/min，保护气氛的气压为1.20MPa。
利用D/max-3BX型X射线衍射仪对此实施例中的CoCrFeMnNiC0.1高熵合金涂层进行物像表征；结果显示物像主要由FCC相构成。
通过使用HVS-1000A型显微硬度计测量熔覆层的显微硬度，压力为0.2kg，保压作用15s后测量涂层和金属基体的硬度；经过计算，45钢基材的平均显微硬度为163.4HV0.2，CoCrFeMnNi高熵合金涂层的平均硬度在211.2HV0.2，硬度是金属基体的1.29倍。
对涂层用王水进行腐蚀，借助Leica DFC280立式金相显微镜获得熔覆层的金相照片，如图1和图2所示，由图可以看出熔覆层结合情况良好，无明显裂纹、气孔且组织致密。利用D/max-3BX型X射线衍射仪对CoCrFeMnNiC0.1高熵合金材料涂层进行物像表征；结果如图3所示，主要由FCC相构成。
实施例2
本实施例所述高熵合金粉末用于制备激光熔覆层的方法，具体包括以下步骤：
(1)对基材进行预处理：先用200～800目砂纸打磨金属基材表面并用水冲洗干净，然后在无水乙醇中进行超声波清洗，在80℃真空环境下干燥0.5h后备用。打磨要求完全去除金属基体表面氧化膜且无粗大划痕亮，磨痕的方向一致且表面光亮。
(2)按CoCrFeMnNiC0.15的原子比称量CoCrFeMnNi高熵合金粉末与纳米C粉末，称量完毕后进行机械混合，其中纳米C粉的平均粒度为30nm，纯度不小于99.99％。
(3)将混合好的粉末与纯度不低于99.7％的无水乙醇混合调制成糊状，使用模具将其粘接在45钢基体预定位置得到1mm厚的预制涂层，然后置于85℃下恒温处理8h；在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆，得到由呈点阵分布的熔覆点构成的熔覆涂层；所述激光熔覆是通过CO2激光器进行的，激光功率为3.7kW，扫描速度为200mm/min，光斑直径为4mm，保护气体为N2，气体流量为20L/min，，保护气氛的气压为1.10MPa。
利用D/max-3BX型X射线衍射仪对CoCrFeMnNiC0.15高熵合金涂层进行物像表征；结果显示物像主要由FCC相构成。
通过使用HVS-1000A型显微硬度计测量熔覆层的显微硬度，压力为0.2kg，保压作用15s后测量涂层和金属基体的硬度；经过计算，45钢基材的平均显微硬度为160.8HV0.2，CoCrFeMnNiC0.15高熵合金涂层的平均硬度在203.3HV0.2，硬度是金属基体的1.26倍。
对比实施例1
一种高熵合金粉末用于制备激光熔覆涂层的方法，具体包括以下步骤：
(1)对45钢基材进行表面预处理：先用200～800目砂纸打磨金属基材表面去除氧化膜，并用水冲洗干净，然后在无水乙醇中进行超声波清洗，去除表面残存的油污及杂质；清洗完毕后，在70℃真空环境下干燥1h后备用；打磨要求完全去除金属基体表面氧化膜且无粗大划痕亮，磨痕的方向一致且表面光亮。
(2)称量CoCrFeMnNi高熵合金粉末，将称量好的CoCrFeMnNi高熵合金粉末与纯度不低于99.7％的无水乙醇混合调制成糊状，使用模具将其粘接在45钢基体预定位置得到1mm厚的预制涂层，然后置于80℃下恒温处理8h；在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆，得到由呈点阵分布的熔覆点构成的熔覆涂层；所述激光熔覆是通过CO2激光器进行，激光功率为3.7kW，扫描速度为200mm/min，光斑直径为3mm，保护气体为Ar，气体流量为15L/min，保护气氛的气压为1.00MPa。
通过使用HVS-1000A型显微硬度计测量熔覆层的显微硬度，压力为0.2kg，保压作用15s后测量涂层和金属基体的硬度，结果如图4所示；经过计算，45钢基材的平均显微硬度为158.4HV0.2，CoCrFeMnNi高熵合金涂层的平均硬度在188.1HV0.2，硬度是金属基体的1.19倍。
综上所述，利用D/max-3BX型X射线衍射仪对CoCrFeMnNiCx高熵合金涂层进行物像表征；结果显示实施例1、实施例2和对比实施例1中熔覆涂层物像皆主要由FCC相构成。通过使用HVS-1000A型显微硬度计测量熔覆层的显微硬度，压力为0.2kg，保压作用15s后测量涂层和金属基体的硬度，实施例1、实施例2和对比实施例1中的熔覆涂层的硬度相较于基体都有明显提升。但涂层硬度：实施例1＞实施例2＞对比实施例1。由此可见，随着C原子的增加，合金强度先增加后减少。但相比于对比实施例1中的CoCrFeMnNi高熵合金涂层，实施例1中的CoCrFeMnNiC0.1高熵合金涂层和实施例2中的CoCrFeMnNiC0.15高熵合金涂层强度都有明显的提高。

Claims (4)

1.一种用于激光熔覆的高熵合金粉末，其特征在于，所述合金粉末为CoCrFeMnNiCx，x取值0.1~0.15；
所述高熵合金粉末用于制备激光熔覆涂层的方法，具体包括以下步骤：
（1）对45钢基材进行表面预处理：打磨，清洗，干燥后备用；
（2）按比例称量等原子比的CoCrFeMnNi高熵合金粉末与纳米C粉末，称量完毕后进行机械混合；
（3）将混合好的粉末与无水乙醇混合调制成糊状，使用模具将其粘接在钢基体预定位置得到预制涂层，然后进行干燥，在保护气氛下，将熔覆粉末在45钢表面进行激光熔覆。
2.根据权利要求1所述用于激光熔覆的高熵合金粉末，其特征在于：步骤（2）中CoCrFeMnNi高熵合金粉末的平均粒度小于25μm，粉末纯度不小于99.9%；纳米C粉的平均粒度为30nm~50nm，纯度不小于99.99%。
3.根据权利要求1所述用于激光熔覆的高熵合金粉末，其特征在于：步骤（3）中干燥条件为：预制涂层厚度为0.2mm~2mm，于80~90℃下恒温处理8~12h。
4.根据权利要求1所述用于激光熔覆的高熵合金粉末，其特征在于：步骤（3）激光熔覆是通过CO2激光器进行的，具体条件为：激光功率为3.7～4.2kW，扫描速度为200～450mm/min，光斑直径为3.0~4.0mm，保护气体为氮气、氩气或二者混合气体，气体流量为15～35L/min，保护气氛的气压为0.80MPa～1.20MPa。
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