CN115094295B - 一种高熵合金粉末及其涂层和涂层的制备方法 - Google Patents
一种高熵合金粉末及其涂层和涂层的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高熵合金粉末及其涂层和涂层的制备方法，高熵合金粉末按原子百分比组成如下：Ti：20％～21.56％、Zr：20％～21.56％、Cu：20％～21.56％、Ni：20％～21.56％、Al：10％～10.76％、Co:3％～10％。先采用气雾化设备制备TiZrCuNiAl0.5高熵合金粉末，再与Co粉末混合均匀，得到粒径范围在50～180μm的高熵合金粉末。对钛合金基板打磨喷砂，并进行预热，再采用激光熔覆工艺将得到的高熵合金粉末熔融后涂敷在钛合金基板表面得到高熵非晶‑纳米晶涂层。所得的高熵非晶‑纳米晶涂层具有硬度高，组织细小，耐磨性能好等特点，具有良好的应用前景。
Description
技术领域
本发明涉及一种高熵合金粉末及其涂层和涂层的制备方法，具体涉及在钛合金基板上采用激光熔覆制备TiZrCuNiAlCo高熵合金粉末及其涂层和涂层的制备方法，属于高熵合金、非晶合金、耐磨涂层新材料领域。
背景技术
钛合金具有密度低、比强度高、耐蚀、耐高温等特点，是航空航天、船舶海工行业的关键材料。然而钛合金也存在硬度低、摩擦系数高、耐磨性差等缺点，影响了其优异力学性能的发挥，限制了应用。在钛合金表面制备一层硬度高、摩擦系数低、具有优异抗磨损性能、与基板牢固结合、厚度及性能可控的高性能涂层是提高钛合金表面硬度，改善耐磨性能的有效方法。
高熵非晶合金是高熵合金和非晶合金的交叉领域，结合了高熵合金的成分特点和非晶合金的性能特点，如高强度，高硬度，高耐磨，高耐蚀等，在某些特定的领域具有良好的应用前景。
CN109439995B公开了一种在45号钢基体表面激光熔覆高熵非晶合金涂层的方法，涂层的成分为：镍28～32％、钴28～32％、硅2～6％、硼2～6％、余量为铁。涂层显微维氏硬度在400HV0.1以上，最高可达729.5HV0.1，平均可达582.9HV0.1。然而，该体系的基板是钢，不是钛合金；同时涂层的硬度仍然不够高。
CN113416910B公开了一种在Q235钢基体表面等离子喷涂高熵非晶合金涂层的方法，涂层的成分为：Co 25％，Ni 25％，Cr 15～20％，Mo 5～10％，Nb 2～4％，B 14％和Si6％；涂层硬度在700HV以上，厚度约50～300μm。然而，该体系的基板是Q235钢，不是钛合金；同时涂层的厚度不够厚。
目前尚没有见到关于在钛合金基板上制备高熵非晶合金涂层的报道。基于此，需要开发出一种在钛合金基板制备高熵非晶合金-纳米晶涂层的方法，使得涂层硬度高，耐磨性好，能够拓展钛合金材料的应用范围。
发明内容
发明目的：本发明的第一目的是提供一种高熵合金粉末，本发明的第二目的是提供一种硬度高、耐磨性好的高熵非晶-纳米晶涂层；本发明的第三目的是提供一种该高熵非晶-纳米晶涂层的制备方法。
技术方案：本发明所述一种高熵合金粉末，所述高熵合金粉末按原子百分比包括Ti：20％～21.56％、Zr：20％～21.56％、Cu：20％～21.56％、Ni：20％～21.56％、Al：10％～10.76％、Co:3％～10％。
其中，所述高熵合金粉末的粒径为50～180μm。
本发明还包括所述的高熵合金粉末制备的高熵非晶-纳米晶涂层。
其中，所述高熵非晶-纳米晶涂层的维氏硬度＞750HV，所述高熵非晶-纳米晶涂层的厚度为100～500μm。
一种本发明所述高熵非晶-纳米晶涂层的制备方法，以钛合金为基板，通过激光熔覆工艺将本发明所述的高熵合金粉末涂覆在基板表面制得。
本发明所述的高熵非晶-纳米晶涂层的制备方法，包括以下步骤：
(1)采用气雾化制粉工艺制TiZrCuNiAl0.5高熵合金粉末；
(2)合成高熵合金粉末：将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀，用筛网进行筛分，得到混合粉末，对混合粉末进行烘干备用；
(3)钛合金基板打磨喷砂：利用喷砂去除钛合金基板表面的氧化层和杂质，利用酒精擦拭去除钛合金基板表面的油污和水渍，将钛合金基板预热；
(4)激光熔覆获得涂层：将高熵合金粉末熔融，在惰性气体保护下，利用激光熔覆工艺将其涂覆在预热的钛合金基板表面即得。
其中，步骤(1)中，所述气雾化制粉工艺是在惰性气体氩气的保护下，用高压惰性氩气气流将金属液流粉碎成小液滴并快速冷凝成粉末。
其中，步骤(1)中，气雾化制粉时，Ti、Zr、Cu、Ni、Al均为质量分数>99.99％的纯金属单质，Ti：Zr：Cu：Ni：Al＝2：2：2：2：1。
其中，步骤(1)中，气雾化制粉时精炼的温度为1500～1600℃，精炼的时间为5～15min，中间保温的温度为1300～1400℃，保温的时间为20～40min，雾化压力3～5MPa。
其中，步骤(2)中，球磨混合时球磨罐和研磨球均为刚玉(Al2O3)材质，研磨球和混合粉末的质量比为1:1，速率为200～300r/min，球磨时间为2h。
其中，步骤(4)中，激光熔覆时激光光斑直径约2.4mm，激光功率800～1200W，扫描速度为360～720mm/min，惰性气体为氩气。
因钛合金容易氧化，涂层应力大，易开裂，本申请采用Ti：Zr：Cu：Ni：Al、Co六种元素制备的高熵合金粉末熔融后激光熔覆在钛合金基板表面，可以克服上述问题，得到的涂层硬度高，组织细小，耐磨性能好。
有益效果：与现有技术相比，本发明具有如下显著优点：
(1)本发明所采用的材料价格便宜，不含贵金属及昂贵的Sc等元素；制备工艺简单，易于实现。
(2)本发明制备的高熵合金粉末可以用于在钛合金表面制备高熵非晶-纳米晶涂层。
(3)本发明所制备的高熵非晶-纳米晶涂层硬度高，组织细小，耐磨性能好。
附图说明
图1为实施例1得到高熵非晶合金-纳米晶涂层XRD图；
图2为实施例1得到高熵非晶合金-纳米晶涂层的SEM图。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
实施例1
1、制备TiZrCuNiAl0.5高熵合金粉末：
采用气雾化方法制备TiZrCuNiAl0.5高熵合金粉末，按原子百分比进行配料，所采用Ti、Zr、Cu、Ni、Al均为质量分数>99.99％的纯金属单质，Ti：Zr：Cu：Ni：Al＝2：2：2：2：1，精炼温度1500℃，精炼时间15min，中间保温温度1300℃，保温时长20min，雾化压力3MPa，通过高速气流将液态金属流粉碎为小滴并快速冷凝成TiZrCuNiAl0.5高熵合金粉末。
2、合成高熵合金粉末：
将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀得到混合粉末，其中Ti：20％、Zr：20％、Cu：20％、Ni：20％、Al：10％、Co:10％，总原子百分比为100％。球磨的具体参数为：球磨罐和研磨球均为刚玉(Al2O3)材质。将研磨球和混合粉末以质量比1:1的比例放置入球磨罐中，顺时针以200r/min的速率球磨2h，用孔径为180μm的筛网进行筛分，去掉研磨球，混合好的粉末加热至100℃，真空烘干4h，自然冷却用于后续熔覆实验。
3、钛合金基板打磨喷砂：
选用TC4钛合金基板，利用喷砂去除TC4钛合金基板表面的氧化层和杂质，利用酒精擦拭去除TC4钛合金基板表面的油污和水渍备用，将TC4钛合金基板预热至250℃，以提高基板和涂层间的结合力。
4、激光熔覆获得涂层：
将步骤2合成的高熵合金粉末熔融，利用激光熔覆工艺将熔融的高熵合金粉末涂覆在步骤3处理过的钛合金基板表面，得到涂层；激光熔覆工艺参数为：激光光斑直径约2.4mm，激光功率800W，扫描速度为720mm/min，采用氩气作为惰性气体保护，获得高熵非晶合金-纳米晶涂层。
对本实施例得到的高熵非晶合金-纳米晶涂层进行厚度测试，得到高熵非晶合金-纳米晶涂层厚度为100μm，维氏硬度为937HV，磨损量为TC4基体的45％，耐磨性能优异。
将本实施例得到高熵非晶合金-纳米晶涂层进行XRD分析，结果如图1所示。图1为实施例1得到涂层的XRD图，由图1可以看出，其显微组织为非晶基体上析出了其它晶态相。
将本实施例得到高熵非晶合金-纳米晶涂层进行电子显微镜扫描分析，结果如图2所示。图2为实施例1得到高熵非晶合金-纳米晶涂层的SEM图，由图2可以看出，在非晶合金基体上析出纳米晶，且与图1的结果互相印证。
实施例2
1、制备TiZrCuNiAl0.5高熵合金粉末：
采用气雾化方法制备TiZrCuNiAl0.5高熵合金粉末。按原子百分比进行配料，所采用Ti、Zr、Cu、Ni、Al均为质量分数>99.99％的纯金属单质，Ti：Zr：Cu：Ni：Al＝2：2：2：2：1，精炼温度1600℃，精炼时间5min，中间包保温温度1400℃，保温时长40min，雾化压力5MPa，通过高速气流将液态金属流粉碎为小滴并快速冷凝成TiZrCuNiAl0.5高熵合金粉末。
2、合成高熵合金粉末：
将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀得到混合粉末，其中Ti：21.56％、Zr：21.56％、Cu：21.56％、Ni：21.56％、Al：10.76％、Co:3％，总原子百分比为100％。球磨的具体参数为：球磨罐和研磨球均为刚玉(Al2O3)材质。将研磨球和混合粉末以1:1的比例放置入球磨罐中，顺时针以250r/min的速率球磨2h，用筛网进行筛分，去掉杂质和研磨球，将混合好的粉末加热至90℃，真空烘干4h，自然冷却用于后续熔覆实验。
3、钛合金基板打磨喷砂：
选用TC4钛合金基板，利用喷砂去除TC4钛合金基板表面的氧化层和杂质，利用酒精擦拭去除TC4钛合金基板表面的油污和水渍备用，将TC4钛合金基板预热至300℃，以提高基板和涂层间的结合力。
4、激光熔覆获得涂层：
将步骤2合成的高熵合金粉末熔融，利用激光熔覆工艺将熔融的高熵合金粉末涂覆在步骤3处理过的钛合金基板表面，得到涂层；激光熔覆工艺参数为：激光光斑直径约2.4mm，激光功率1200W，扫描速度为360mm/min，采用氩气作为惰性气体保护，获得高熵非晶合金-纳米晶涂层。
对本实施例得到的高熵非晶合金-纳米晶涂层进行厚度测试，得到高熵非晶合金-纳米晶涂层厚度为500μm，维氏硬度为795HV，磨损量为TC4基体的70％，耐磨性能优异。
实施例3
1、制备TiZrCuNiAl0.5高熵合金粉末：
采用气雾化方法制备TiZrCuNiAl0.5高熵合金粉末。按原子百分比进行配料，所采用Ti、Zr、Cu、Ni、Al均为质量分数>99.99％的纯金属单质，Ti：Zr：Cu：Ni：Al＝2：2：2：2：1，精炼温度1550℃，精炼时间10min，中间保温温度1360℃，保温时长30min，雾化压力4MPa，通过高速气流将液态金属流粉碎为小滴并快速冷凝成TiZrCuNiAl0.5高熵合金粉末。
2、合成高熵合金粉末：
将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀得到混合粉末，其中Ti：20.89％、Zr：20.89％、Cu：20.89％、Ni：20.89％、Al：10.44％、Co:6％，总原子百分比为100％。球磨的具体参数为：球磨罐和研磨球均为刚玉(Al2O3)材质。将研磨球和混合粉末以1:1的比例放置入球磨罐中，顺时针以300r/min的速率球磨2h，用筛网进行筛分，去掉杂质和研磨球，将混合好的粉末加热至80℃，真空烘干4h，自然冷却用于后续熔覆实验。
3、钛合金基板打磨喷砂：
选用TC4钛合金基板，利用喷砂去除TC4钛合金基板表面的氧化层和杂质，利用酒精擦拭去除TC4钛合金基板表面的油污和水渍备用，将TC4钛合金基板预热至350℃，以提高基板和涂层间的结合力。
4、激光熔覆获得涂层：
将步骤2合成的高熵合金粉末熔融，利用激光熔覆工艺将熔融的高熵合金粉末涂覆在步骤3处理过的钛合金基板表面，得到涂层；激光熔覆工艺参数为：激光光斑直径约2.4mm，激光功率1000W，扫描速度为480mm/min，采用氮气作为惰性气体保护，获得高熵非晶合金-纳米晶涂层。
对本实施例得到的高熵非晶合金-纳米晶涂层进行厚度测试，得到高熵非晶合金-纳米晶涂层厚度为260μm，维氏硬度为890HV，磨损量为TC4基体的50％，耐磨性能优异。
Claims (5)
1.一种高熵合金粉末，其特征在于，所述高熵合金粉末按原子百分比包括Ti：20%～21.56%、Zr：20%～21.56%、Cu：20%～21.56%、Ni：20%～21.56%、Al：10%～10.76%、Co: 3%～10%，其中，Ti：Zr：Cu：Ni：Al=2：2：2：2：1，所述TiZrCuNiAl0.5的制备包括（1）采用气雾化制粉工艺制TiZrCuNiAl0.5高熵合金粉末，所述气雾化制粉工艺是在惰性气体氩气的保护下，用高压惰性氩气气流将金属液流粉碎成小液滴并快速冷凝成粉末，气雾化制粉时，Ti：Zr：Cu：Ni：Al均为质量分数>99.99%的纯金属单质，精炼的温度为1500～1600℃，精炼的时间为5～15 min，中间保温的温度为1300～1400 ℃，保温的时间为20～40 min，雾化压力为3～5MPa；
（2）合成高熵合金粉末：将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀，用筛网进行筛分，得到混合粉末，对混合粉末进行烘干备用，球磨混合时，球磨罐和研磨球均为刚玉材质，速率为200～300 r/min。
2.根据权利要求1所述的高熵合金粉末，其特征在于，所述高熵合金粉末的粒径为50~180μm。
3.权利要求1或2所述的高熵合金粉末制备的高熵非晶-纳米晶涂层。
4.根据权利要求3所述的高熵非晶-纳米晶涂层，其特征在于，所述高熵非晶-纳米晶涂层的维氏硬度＞750HV，所述高熵非晶-纳米晶涂层的厚度为100～500μm。
5.一种权利要求3或4所述高熵非晶-纳米晶涂层的制备方法，其特征在于，以钛合金为基板，通过激光熔覆工艺将权利要求3或权利要求4所述的高熵合金粉末涂覆在基板表面制得，包括以下步骤：
（1）采用气雾化制粉工艺制TiZrCuNiAl0.5高熵合金粉末，所述气雾化制粉工艺是在惰性气体氩气的保护下，用高压惰性氩气气流将金属液流粉碎成小液滴并快速冷凝成粉末，气雾化制粉时，Ti：Zr：Cu：Ni：Al均为质量分数>99.99%的纯金属单质，精炼的温度为1500～1600℃，精炼的时间为5～15 min，中间保温的温度为1300～1400 ℃，保温的时间为20～40min，雾化压力为3～5 MPa；
（2）合成高熵合金粉末：将TiZrCuNiAl0.5高熵合金粉末及Co粉末材料经球磨混合均匀，用筛网进行筛分，得到混合粉末，对混合粉末进行烘干备用，球磨混合时，球磨罐和研磨球均为刚玉材质，速率为200～300 r/min；
（3）钛合金基板打磨喷砂：利用喷砂去除钛合金基板表面的氧化层和杂质，利用酒精擦拭去除钛合金基板表面的油污和水渍，将钛合金基板预热；
（4）激光熔覆获得涂层：将高熵合金粉末熔融，在惰性气体保护下，利用激光熔覆工艺将其涂覆在预热的钛合金基板表面即得，激光熔覆涂层时，激光功率800～1200 W，扫描速度为360～720 mm/min，惰性气体为氩气。
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