CN113402279A - 一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和应用 - Google Patents

一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和应用 Download PDF

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CN113402279A
CN113402279A CN202110334256.6A CN202110334256A CN113402279A CN 113402279 A CN113402279 A CN 113402279A CN 202110334256 A CN202110334256 A CN 202110334256A CN 113402279 A CN113402279 A CN 113402279A
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carbide ceramic
sialon
rod
entropy
long
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郭伟明
周宇章
罗嗣春
林华泰
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Guangdong University of Technology
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Abstract

本发明属于高熵陶瓷材料领域，公开了一种长棒状β‑SiAlON增韧的高熵碳化物陶瓷及制备方法和应用。该高熵碳化物陶瓷是将微米级高纯度的TiC、ZrC、HfC、VC、WC、TaC、NbC中的任意五种碳化物等摩尔比混合作为高熵碳化物陶瓷基体，再加入Si3N4、Al2O3、AlN与烧结助剂Y2O3，经球磨得到混合粉体；分装入石墨模具中，在保护气氛下轴向施加压力30～40MPa，升温至1850～2200℃进行SPS烧结得到高熵碳化物陶瓷；本发明通过在高熵碳化物中加入Si3N4、Al2O3、AlN，烧结形成长棒状的β‑SiAlON实现对高熵碳化物陶瓷的增韧，提高其断裂韧性与抗弯强度，提高材料的烧结致密度。

Description

一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和 应用
技术领域
本发明属于高熵陶瓷材料技术领域，特别涉及一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和应用。
背景技术
“高熵”概念源自近十几年来对高熵合金的研究，借助反应物在制备过程中的“高熵效应”，制备出了性能优异、微观结构稳定的合金材料。随着制备工艺的发展，“高熵”理论渐渐应用到了非金属化合物的制备领域，诞生了“高熵陶瓷”材料。
五元“高熵陶瓷”化学式表示为(A0.2B0.2C0.2D0.2E0.2)Fn，其中A、B、C、D、E为过渡金属元素，它们的摩尔量相等，F为陶瓷材料的体系，目前常见的体系有碳、硼、氧、硅等；材料具有优异的力学性能与化学稳定性，在高温的应用场合下力学性能和化学性质均十分稳定。
目前，高熵陶瓷的研究中，高熵碳化物陶瓷的制备已日趋成熟，不少学者基于高硬度碳化物制备了(Hf0.2Zr0.2Ta0.2M0.2Ti0.2)C，(M＝Nb,Mo,Cr)的高熵陶瓷，研究发现高熵化处理提高了材料的抗氧化能力、弹性模量与硬度，并显著降低了导热率，在高温冶金、发动机结构件、绝热件、支撑件等领域有宽阔的应用前景。
但该种材料的烧结较为困难，常用的制备方法需要相当高的烧结温度(＞2000℃)，且直接采用商业碳化物粉体进行固溶烧结制备得到的陶瓷材料相对密度较低(约为93％～95.1％)；同时成品材料韧性较差，仅能制备形状简单的零部件，这大大制约了此类材料的进一步应用。
发明内容
为了克服现有技术中存在的缺点与不足，本发明的首要目的在于提供一种长棒状β-SiAlON增韧的高熵碳化物陶瓷的制备方法。
本发明的再一目的在于提供一种上述制备方法制备得到的长棒状β-SiAlON增韧的高熵碳化物陶瓷。该高熵碳化物陶瓷利用加入的长棒状β-SiAlON作为第二相实现对高熵碳化物陶瓷的增韧，提高其断裂韧性与抗弯强度，并抑制基体中晶粒的生长，从而提高材料的烧结致密度。
本发明的另一目的在于提供一种上述长棒状β-SiAlON增韧的高熵碳化物陶瓷的应用。
本发明的目的通过下述技术方案实现：
一种长棒状β-SiAlON增韧的高熵碳化物陶瓷的制备方法，包括以下操作步骤：将微米级高纯度的TiC、ZrC、HfC、VC、WC、TaC、NbC中的任意五种碳化物等摩尔比混合作为高熵碳化物陶瓷基体，再加入Si3N4、Al2O3、AlN与烧结助剂Y2O3，经球磨得到混合粉体，其将用于制备长棒状的β-SiAlON相作为增韧相；将混合粉体分装入石墨模具中，在保护气氛下，轴向施加压力30～40MPa，升温至1850～2200℃进行SPS烧结，得到长棒状β-SiAlON增韧的高熵碳化物陶瓷；所述增韧相的添加量为混合粉体总质量的10～40％。
所述的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为96～99％，维氏硬度为23～26GPa，断裂韧性为5～7MPa·m1/2。
所述微米级高纯度的TiC、ZrC、HfC、VC、WC、TaC、NbC的纯度均为99～100％。
所述球磨为辊式球磨，是以无水乙醇为溶剂，以碳化钨球为球磨介质；所述球磨的转速为150～500r/min，所述球磨的时间为8～24h。
所述烧结助剂Y2O3占混合粉体总质量的0.3～1.5％。
所述保护气氛为氩气。
所述升温的速率为50～200℃/min；所述烧结的时间为10～20min。
一种根据上述的制备方法制备得到的长棒状β-SiAlON增韧的高熵碳化物陶瓷。
上述的长棒状β-SiAlON增韧的高熵碳化物陶瓷在制备高温场合下的支撑零件、保护外壳或结构复杂的结构件中的应用。
本发明相对于现有技术具有如下的优点及效果：
(1)本发明引入的长棒状β-SiAlON相在制备过程抑制了碳化物晶粒的生长，通过细化晶粒提高了材料的烧结致密度和力学性能。
(2)本发明引用的长棒状β-SiAlON相增韧了高熵碳化物陶瓷的韧性与抗弯强度，使得这种材料能更广泛地应用在结构复杂的高温结构件中，且不影响材料的导热率与化学稳定性。
(3)本发明通过加入的长棒状β-SiAlON相实现对高熵碳化物陶瓷的增韧，并提高其抗弯强度，细化材料中的晶粒，提高材料的烧结致密度；所述得到长棒状β-SiAlON增韧的高熵碳化物陶瓷材料致密度为96～99％，维氏硬度为23～26GPa，断裂韧性为5～7MPa·m1 /2；制备的陶瓷可广泛应用于各种高温场合下的支撑零件、保护外壳或结构复杂的结构件。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1：
(1)以无水乙醇为溶剂，以碳化钨球为球磨介质，将TiC(纯度99.6wt.％，)、ZrC(纯度99.7wt.％)、NbC(纯度99.8wt.％)、HfC(纯度99.5wt.％)、TaC(纯度99.7wt.％)粉体按摩尔比1：1：1：1：1配料，转速为200r/min，进行球磨混合10h，得到混合粉体A；
(2)以无水乙醇为溶剂，以碳化钨球为球磨介质，将混合粉体A与Si3N4(纯度99.9wt.％)、Al2O3(纯度99.7wt.％)、AlN(纯度99.8wt.％)与Y2O3(纯度99.8wt.％)进行配料，使得混合后的粉体中将生成的长棒状β-SiAlON相(即由Si3N4、Al2O3、AlN反应得到的β-Si4Al2O2N6，其反应式为：3/4Si3N4+2/3AlN+2/3Al2O3→β-Si4Al2O2N6)的质量占混合后的粉体总质量的30％，烧结助剂Y2O3加入的质量占混合后的粉体总质量的2％，使转速为200r/min，进行球磨混合10h，得到混合粉体B；
(3)将混合粉体B装入石墨模具中，并置放于SPS烧结炉中，在氩气气氛保护下，轴向加压30MPa，以100℃/min升温至2000℃，然后进行保温15min，此后随炉自然冷却至室温，制得长棒状β-SiAlON增韧的高熵碳化物陶瓷。
本实施例所得长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为98％，维氏硬度为24GPa，断裂韧性为6MPa·m1/2。
实施例2：
与实施例1不同的在于：步骤(3)中所述轴向加压为40MPa。
本实施例所得的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为98％，维氏硬度为25GPa，断裂韧性为7MPa·m1/2。
实施例3：
与实施例1不同的在于：步骤(3)中所述升温的温度为2100℃。
本实施例所得的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为99％，维氏硬度为24GPa，断裂韧性为6MPa·m1/2。
实施例4
与实施例1不同的在于：步骤(3)中所述保温的时间为20min。
本实施例所得的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为99％，维氏硬度为24GPa，断裂韧性为5MPa·m1/2。
实施例5
与实施例1不同的在于：步骤(2)中所述混合粉体长棒状β-SiAlON相的质量占混合后的粉体总质量的20％；
本实施例所得的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为97％，维氏硬度为23GPa，断裂韧性为6MPa·m1/2。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (9)

1.一种长棒状β-SiAlON增韧的高熵碳化物陶瓷的制备方法，其特征在于包括以下操作步骤：将微米级高纯度的TiC、ZrC、HfC、VC、WC、TaC、NbC中的任意五种碳化物等摩尔比混合作为高熵碳化物陶瓷基体，再加入Si3N4、Al2O3、AlN与烧结助剂Y2O3，经球磨得到混合粉体，其将用于制备长棒状的β-SiAlON相作为增韧相；将混合粉体分装入石墨模具中，在保护气氛下，轴向施加压力30～40MPa，升温至1850～2200℃进行SPS烧结，得到长棒状β-SiAlON增韧的高熵碳化物陶瓷；所述增韧相的添加量为混合粉体总质量的10～40％。
2.根据权利要求1所述的制备方法，其特征在于：所述的长棒状β-SiAlON增韧的高熵碳化物陶瓷的致密度为96～99％，维氏硬度为23～26GPa，断裂韧性为5～7MPa·m1/2。
3.根据权利要求1所述的制备方法，其特征在于：所述微米级高纯度的TiC、ZrC、HfC、VC、WC、TaC、NbC的纯度均为99～100％。
4.根据权利要求1所述的制备方法，其特征在于：所述球磨为辊式球磨，是以无水乙醇为溶剂，以碳化钨球为球磨介质；所述球磨的转速为150～500r/min，所述球磨的时间为8～24h。
5.根据权利要求1所述的制备方法，其特征在于：所述烧结助剂Y2O3占混合粉体总质量的0.3～1.5％。
6.根据权利要求1所述的制备方法，其特征在于：所述保护气氛为氩气。
7.根据权利要求1所述的制备方法，其特征在于：所述升温的速率为50～200℃/min；所述烧结的时间为10～20min。
8.一种根据权利要求1～7任一项所述的制备方法制备得到的长棒状β-SiAlON增韧的高熵碳化物陶瓷。
9.根据权利要求8所述的长棒状β-SiAlON增韧的高熵碳化物陶瓷在制备高温场合下的支撑零件、保护外壳或结构复杂的结构件中的应用。
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