CN111995400B - 一种具有优异摩擦学性能的高熵陶瓷材料及其制备方法 - Google Patents

一种具有优异摩擦学性能的高熵陶瓷材料及其制备方法 Download PDF

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CN111995400B
CN111995400B CN202010946401.1A CN202010946401A CN111995400B CN 111995400 B CN111995400 B CN 111995400B CN 202010946401 A CN202010946401 A CN 202010946401A CN 111995400 B CN111995400 B CN 111995400B
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杨军
孙奇春
刘维民
朱圣宇
程军
乔竹辉
谈辉
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明涉及一种具有优异摩擦学性能的高熵陶瓷材料，该材料呈块体，其组成为(Hf‑Mo‑Nb‑Ta‑Ti‑)C，由下述质量百分比的原料制得：HfO2 21.2~21.9%，MoO3 14.5~15.0%，Nb2O5 13.4~13.8%，Ta2O5 22.3~23.0%，TiO2 8.0~8.3%和石墨粉末18.0~20.6%。同时，本发明还公开了该高熵陶瓷材料的制备方法。本发明在宽温域具有良好的摩擦学性能和力学性能，并且可实现特定温度的润滑，从而实现了陶瓷材料的结构/润滑功能一体化设计。

Description

一种具有优异摩擦学性能的高熵陶瓷材料及其制备方法
技术领域
本发明涉及高熵材料技术领域，尤其涉及一种具有优异摩擦学性能的高熵陶瓷材料及其制备方法。
背景技术
结构材料的可靠性和稳定性对于高端装备机械系统的安全、稳定、高效运行起关键作用。随着高新技术的快速发展，新一代核反应堆、喷气发动机、火箭喷管、超音速飞行器等服役的工况越来越苛刻，对高性能高温材料的需求更为迫切。目前，主要是通过添加第二相（润滑相或耐磨相）来改善高温材料的高温摩擦学性能。尽管该方法可有效改善摩擦学性能，但是通常会导致其力学性能的严重恶化，造成材料综合使役性能的下降，不能胜任极端的苛刻工况。
近年来，“高熵”作为一种新型的材料设计理论引起了人们的极大关注。其中高熵碳化物陶瓷因其优异的综合性能和潜在的应用前景而备受关注。目前关于高熵碳化物陶瓷主要是对其制备、力学性能和热物理性能的研究，而与其相关的摩擦学性能的研究非常少。
发明内容
本发明所要解决的技术问题是提供一种在宽温域具有优异摩擦学性能的高熵陶瓷材料。
本发明所要解决的另一个技术问题是提供该高熵陶瓷材料的制备方法。
为解决上述问题，本发明所述的一种具有优异摩擦学性能的高熵陶瓷材料，其特征在于：该材料呈块体，其组成为(Hf-Mo-Nb-Ta-Ti-)C，由下述质量百分比的原料制得：HfO2 21.2~21.9%，MoO3 14.5~15.0%，Nb2O5 13.4~13.8%，Ta2O5 22.3~23.0%，TiO2 8.0~8.3%和石墨粉末18.0~20.6%。
如上所述的一种具有优异摩擦学性能的高熵陶瓷材料的制备方法，其特征在于：首先按配比称取各原料，并将各原料置于球磨机中，然后在混合原料中加入其质量0.25~0.35倍的无水乙醇，混合均匀后，经烘干、过筛，得到粒径为5~20 μm的混合粉末；所述混合粉末装入石墨模具中，经放电等离子烧结，烧结结束后，再经高能球磨粉碎，即得粒径为0.1~1.5 μm的高熵陶瓷粉末；最后，所述高熵陶瓷粉末经放电等离子烧结，即得高熵陶瓷块体材料。
所述混合粉末的烧结条件是指真空度低于0.8 Pa，平均升温速度为50~150 ℃/min，烧结温度为1750~1850 ℃，压力为5~15 MPa，保温时间20~30 min。
所述高能球磨粉碎的条件是指球料比1.5：1~4：1，转速为250~300 r/min，球磨时间为4~6 h，磨罐和磨球均为碳化物硬质合金，球磨开始前充入氩气。
所述高熵陶瓷粉末的烧结条件是指真空度低于0.8 Pa，平均升温速度为100~150℃/min，烧结温度为1950~2050 ℃，压力为30~40 MPa，保温时间8~15 min。
本发明与现有技术相比具有以下优点：
1、本发明采用“高熵”材料设计理念，明显不同于传统摩擦材料的设计思路（利用第二相来改善摩擦学性能），有效地避免了第二相对材料综合性能的影响。
2、对本发明烧结后高熵陶瓷的物相组成以及粒径大小采用X射线衍射仪及扫描电子显微镜进行分析，发现：本发明制备的高熵陶瓷粉末具有较小的粒径，平均粒径为480nm，如图1所示。该尺寸有利于陶瓷材料的烧结，更加易于致密化。同时， 从图2可知，本发明制备的高熵陶瓷由单相组成，其组成为(Hf-Mo-Nb-Ta-Ti)C。
3、本发明高熵陶瓷块体材料经试验测试，在宽温域具有优异的摩擦学性能和力学性能。硬度最高可达19.2 GPa，磨损率低至10-7mm3/Nm量级，并且可实现特定温度的润滑，摩擦系数低至0.1左右，从而实现了陶瓷材料的结构/润滑功能一体化设计。
【致密性及力学性能】
采用阿基米德原理测量材料的密度。测试结果表明所制备块体材料的相对密度为97.3~98.6 %。
采用维式显微硬度计测试材料的硬度，测试条件为：载荷5 kg，加载持续时间10s。测试结果表明所制备块体材料的硬度在室温~900 ℃时为12~19.2 GPa，如表1所示。
表1：本发明高熵陶瓷块体材料在25~900 ℃的硬度
Figure DEST_PATH_IMAGE001
【大气摩擦学性能】
摩擦磨损实验采用HT-1000试验机进行评价，对偶球为Al2O3陶瓷，载荷为5 N，滑动线速度为0.10 m/s，摩擦半径为4 mm，行程为200 m，测试温度为25 ℃， 300 ℃和600 ℃，摩擦系数和磨损率为3次试验平均值。实验结果表明所制备的高熵陶瓷块体材料在宽温域具有优异的耐磨性能，磨损率为10-7~10-5mm3/Nm量级，如表2所示。
表2：本发明高熵陶瓷块体材料与Al2O3陶瓷球配副的摩擦系数和磨损率
Figure DEST_PATH_IMAGE003
【真空摩擦学性能】
真空摩擦磨损实验采用GHT-1000E试验机进行评价，对偶球为Al2O3陶瓷，载荷为5N，滑动线速度为0.10 m/s，摩擦半径为4 mm，行程为200 m，测试温度为25 ℃、 200 ℃ 、300 ℃、400 ℃、500 ℃、600 ℃和900 ℃。摩擦系数和磨损率为3次试验平均值。实验结果表明所制备的高熵陶瓷块体材料在真空宽温域具有优异的摩擦学性能，如表3所示。在200~400 ℃，摩擦系数低至0.1左右；在500~900 ℃时，平均摩擦系数在0.8~1.25范围内。而磨损率在25~400 ℃时为10-7mm3/Nm量级，在500~900 ℃时为10-6~10-5mm3/Nm量级。在400 ℃时的摩擦系数如图3所示，经过跑合之后摩擦系数稳定于0.1左右。
表3：本发明高熵陶瓷块体材料与Al2O3陶瓷球配副的摩擦系数和磨损率
Figure DEST_PATH_IMAGE005
4、本发明制备工艺简单，通过调整配方和工艺参数，可以调控材料性能，所得高熵材料可在高温/真空等极端苛刻工况下应用。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明。
图1为本发明制备的高熵陶瓷粉末的扫描电镜形貌。
图2为本发明制备的高熵陶瓷粉末和块体的X射线衍射图。
图3为本发明制备的高熵陶瓷块体在真空下400℃时的摩擦系数。
具体实施方式
实施例1 一种具有优异摩擦学性能的高熵陶瓷材料，该材料呈块体，其组成为(Hf-Mo-Nb-Ta-Ti-)C，由下述质量百分比的原料制得：HfO2 21.2%，MoO3 14.5%，Nb2O5 13.4%，Ta2O5 22.3%，TiO2 8.0%和石墨粉末20.6%。
该高熵陶瓷材料的制备方法：首先按配比称取各原料，并将各原料置于球磨机中，然后在混合原料中加入其质量0.25倍的无水乙醇，混合均匀后，经烘干、过筛，得到粒径为5~20 μm的混合粉末；混合粉末装入石墨模具中，置于放电等离子烧结炉中经放电等离子烧结，烧结条件是指真空度低于0.5 Pa，平均升温速度为50 ℃/min，烧结温度为1750 ℃，压力为15 MPa，保温时间30 min。烧结结束后，烧结产物置于高能球磨中粉碎即得粒径为0.1~1.5 μm的高熵陶瓷粉末，其形貌和物相组成如图1和图2所示。其中：球磨参数为球料比1.5：1，转速为300 r/min，球磨时间为6 h，磨罐和磨球均为碳化物硬质合金，球磨开始前充入氩气。最后，高熵陶瓷粉末在真空度低于0.5 Pa、升温速度为100 ℃/min、烧结温度为1950℃、压力为40 MPa、保温时间15 min的条件下经放电等离子烧结，即得高熵陶瓷块体材料。
实施例2 一种具有优异摩擦学性能的高熵陶瓷材料，该材料呈块体，其组成为(Hf-Mo-Nb-Ta-Ti-)C，由下述质量百分比的原料制得：HfO2 21.9%，MoO3 15.0%，Nb2O5 13.8%，Ta2O5 23.0%，TiO2 8.3%和石墨粉末18.0%。
该高熵陶瓷材料的制备方法：首先按配比称取各原料，并将各原料置于球磨机中，然后在混合原料中加入其质量0.35倍的无水乙醇，混合均匀后，经烘干、过筛，得到粒径为5~20 μm的混合粉末；混合粉末装入石墨模具中，置于放电等离子烧结炉中经放电等离子烧结，烧结条件是指真空度低于0.08 Pa，平均升温速率150℃/min，烧结温度1850℃，压力5MPa，保温时间20 min。烧结结束后，烧结产物置于高能球磨中粉碎即得粒径为0.1~1.5 μm的高熵陶瓷粉末。其中：球磨参数为球料比4：1，转速为250 r/min，球磨时间为4 h，磨罐和磨球均为碳化物硬质合金，球磨开始前充入氩气。最后，高熵陶瓷粉末在真空度低于0.08Pa、升温速度为150 ℃/min、烧结温度为2050 ℃、压力为30 MPa、保温时间8 min的条件下经放电等离子烧结，即得高熵陶瓷块体材料。
实施例3 一种具有优异摩擦学性能的高熵陶瓷材料，该材料呈块体，其组成为(Hf-Mo-Nb-Ta-Ti-)C，由下述质量百分比的原料制得：HfO2 21.5%，MoO3 14.7%，Nb2O5 13.6%，Ta2O5 22.7%，TiO2 8.1%和石墨粉末19.4%。
该高熵陶瓷材料的制备方法：首先按配比称取各原料，并将各原料置于球磨机中，然后在混合原料中加入其质量0.30倍的无水乙醇，混合均匀后，经烘干、过筛，得到粒径为5~20 μm的混合粉末；混合粉末装入石墨模具中，置于放电等离子烧结炉中经放电等离子烧结，烧结条件是指真空度低于0.8 Pa，平均升温速率100 ℃/min，烧结温度1800 ℃，压力10MPa，保温时间25 min。烧结结束后，烧结产物置于高能球磨中粉碎即得粒径为0.1~1.5 μm的高熵陶瓷粉末。其中：球磨参数为球料比3：1，转速为275 r/min，球磨时间为5 h，磨罐和磨球均为碳化物硬质合金，球磨开始前充入氩气。最后，高熵陶瓷粉末在真空度低于0.8Pa、升温速度为125 ℃/min、烧结温度为2000 ℃、压力为35 MPa、保温时间10 min的条件下经放电等离子烧结，即得高熵陶瓷块体材料。

Claims (4)

1.一种具有优异摩擦学性能的高熵陶瓷材料，其特征在于：该材料呈块体，其组成为(Hf-Mo-Nb-Ta-Ti-)C，由下述质量百分比的原料制得：HfO2 21.2~21.9%，MoO3 14.5~15.0%，Nb2O5 13.4~13.8%，Ta2O5 22.3~23.0%，TiO2 8.0~8.3%和石墨粉末18.0~20.6%；
其制备方法：首先按配比称取各原料，并将各原料置于球磨机中，然后在混合原料中加入其质量0.25~0.35倍的无水乙醇，混合均匀后，经烘干、过筛，得到粒径为5~20 μm的混合粉末；所述混合粉末装入石墨模具中，经放电等离子烧结，烧结结束后，再经高能球磨粉碎，即得粒径为0.1~1.5 μm的高熵陶瓷粉末；最后，所述高熵陶瓷粉末经放电等离子烧结，即得高熵陶瓷块体材料。
2.如权利要求1所述的一种具有优异摩擦学性能的高熵陶瓷材料，其特征在于：所述混合粉末的烧结条件是指真空度低于0.8 Pa，平均升温速度为50~150 ℃/min，烧结温度为1750~1850 ℃，压力为5~15 MPa，保温时间20~30 min。
3.如权利要求1所述的一种具有优异摩擦学性能的高熵陶瓷材料，其特征在于：所述高能球磨粉碎的条件是指球料比1.5：1~4：1，转速为250~300 r/min，球磨时间为4~6 h，磨罐和磨球均为碳化物硬质合金，球磨开始前充入氩气。
4.如权利要求1所述的一种具有优异摩擦学性能的高熵陶瓷材料，其特征在于：所述高熵陶瓷粉末的烧结条件是指真空度低于0.8 Pa，平均升温速度为100~150 ℃/min，烧结温度为1950~2050 ℃，压力为30~40 MPa，保温时间8~15 min。
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