CN116283296A - 一种碳化硅增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用 - Google Patents

一种碳化硅增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用 Download PDF

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CN116283296A
CN116283296A CN202310151143.1A CN202310151143A CN116283296A CN 116283296 A CN116283296 A CN 116283296A CN 202310151143 A CN202310151143 A CN 202310151143A CN 116283296 A CN116283296 A CN 116283296A
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黄坤恒
郭伟明
刘洋
罗展鹏
林华泰
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Guangdong University of Technology
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Abstract

本发明属于非氧化物陶瓷基复合材料技术领域，公开了一种碳化硅增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用。该方法是将等摩尔比的钛粉、锆粉、铌粉、钽粉和钼粉，硅粉，碳粉通过粉体包覆机制得碳‑硅包覆金属混合粉体，然后将混合粉体放入石墨模具，采用放电等离子烧结或热压烧结工艺，制得碳化硅增硬增韧高熵碳化物的复相陶瓷，该复相陶瓷具有比高熵碳化物陶瓷更高的维氏硬度和断裂韧性，且相对密度接近100％，维氏硬度为25～27GPa，断裂韧性为5～7MPa·m1/2，可应用在制备切削难加工材料或航空航天耐磨零部件中。

Description

一种碳化硅增硬增韧高熵碳化物的复相陶瓷及其制备方法和 应用
技术领域
本发明属于非氧化物陶瓷基复合材料技术领域，更具体地，涉及一种碳化硅增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用。
技术背景
碳化硅复合高熵碳化物陶瓷材料具有高熔点、高硬度、高韧性等特点，有望被应用于高速切削和航空航天领域。目前碳化硅复合高熵碳化物陶瓷的制备工艺多采用直接将碳化硅作为第二相添加到高熵碳化物粉体中，后通过无压/有压烧结的方式，在2000℃左右的温度下实现致密化。由于碳化硅的加入带来的钉扎效应，制得的碳化硅复合高熵碳化物陶瓷通常具有较为细小的晶粒。并且由于碳化硅本身具有很高的硬度，致使碳化硅复合高熵碳化物陶瓷的硬度得到提升。另外，由于碳化硅粒子在裂纹扩展中引起的裂纹偏转、裂纹桥接等机制的存在，碳化硅复合高熵碳化物陶瓷的断裂韧性也得到了改善。
无论是纯高熵碳化物陶瓷还是碳化硅复合高熵碳化物陶瓷，由于碳化硅和高熵碳化物具有很强的共价键，其烧结致密所需的温度都比较高(约2000℃)，高的烧结温度除了导致较高的能耗以外，也诱导了高熵碳化物晶粒的长大，进而导致其力学性能提升不明显。
发明内容
为了解决上述现有技术存在的不足和缺点，本发明的目的在于提供一种碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法。该方法工艺简单，能够在低温下实现复合材料的致密，并且能够抑制高熵碳化物晶粒的长大，显著改善碳化硅复合高熵碳化物陶瓷的硬度和断裂韧性。
本发明的另一目的在于提供上述方法制得的碳化硅增硬增韧高熵碳化物的复相陶瓷。该复相陶瓷具有致密的结构，原位生成的碳化硅均匀的分布在高熵碳化物陶瓷基体中，极大地提高了复相材料的维氏硬度和断裂韧性。
本发明的再一目的在于提供上述碳化硅增硬增韧高熵碳化物的复相陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，包括以下步骤：
S1.将Ti粉、Zr粉、Nb粉、Ta粉、Mo粉、C粉和Si粉混合，以Ti、Zr、Nb、Ta、Mo的总物质的量为100％计，Ti粉占比为20mol％，Zr粉占比为20mol％，Nb粉占比为20mol％，Ta粉占比为20mol％，Mo粉占比为20mol％；C粉的摩尔量与Ti粉、Zr粉、Nb粉、Ta粉、Mo粉和C粉的总摩尔比为(1.2～2):1，Si粉和C粉的摩尔比为1:(2～6)；
S2.将Ti粉、Zr粉、Nb粉、Ta粉、Mo粉、C粉和Si粉的混合粉体经包覆机包覆后，干压成坯体，在保护气氛下，将坯体在1600～1800℃，压力为20～40MPa，进行放电等离子烧结或热压烧结，制得碳化硅增硬增韧高熵碳化物的复相陶瓷，所述复相陶瓷的分子式为(Ti,Zr,Nb,Ta,Mo)C-SiC。
优选地，步骤S1中所述的Ti粉、Zr粉、Nb粉、Ta粉、Mo粉的粒径均为1～5μm；所述的C粉和Si粉的粒径均为30～100nm。
优选地，步骤S2中所述包覆机的转速为2000～3000rad/min，所述包覆的时间为10～20min。
优选地，步骤S2中所述放电等离子烧结的具体程序为：先以100～150℃/min的速率升温至1000～1200℃，开始充氩气并且开始加压，继续升温至1600～1800℃，同时压力升至20～40MPa；升温程序执行完毕后保温保压10～20min；然后以80～100℃/min的速率降温，1000～1200℃泄压完毕，温度降至750～850℃后随炉降温。
优选地，步骤S3中所述热压烧结的程序为：先以10～14℃/min的速率升温至1000℃开始充氩气并且开始加压，继续以6～8℃/min的速率升温至1600～1800℃，同时压力升至20～40MPa；升温程序执行完毕后保温保压0.5h～1.0h；然后以10～12℃/min的速率降温，1000～1200℃泄压完毕，降温至750～850℃后随炉降温。
一种碳化硅/高熵碳化物的复相陶瓷，所述复相陶瓷是由所述的方法制备得到。
优选地，所述的碳化硅/高熵碳化物的复相陶瓷，其特征在于，所述复相陶瓷的相对密度大于99％，维氏硬度为25～27GPa，断裂韧性为5～7MPa·m1/2。
所述的碳化硅/高熵碳化物的复相陶瓷在制备切削难加工材料或航空航天耐磨零部件中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明采用了硅热碳热辅助反应烧结工艺，通过在硅和碳以及碳和金属在反应中的放热为陶瓷烧结致密提供了能量，降低了陶瓷的致密温度，节约能源，能够在低温下实现复合材料致密，并且能够抑制高熵碳化物晶粒的长大，显著改善碳化硅复合高熵碳化物陶瓷的硬度和断裂韧。
2.本发明通过在体系中引入硅，由于硅在高温下形成液相，并通过毛细管效应充满高熵碳化物晶粒间，抑制了高熵碳化物晶粒的长大。并在烧结进程中硅被碳消耗生成了碳化硅，不影响高熵碳化物陶瓷的致密度。
3.本发明制得的复相陶瓷具有高韧性、高硬度的优点，复相陶瓷的相对密度大于99％，维氏硬度为25～27GPa，断裂韧性为5～7MPa·m1/2。
附图说明
图1为实施例1的(Ti,Zr,Nb,Ta,Mo)C-SiC复相陶瓷的显微结构；
图2为实施例2的(Ti,Zr,Nb,Ta,Mo)C-SiC复相陶瓷的显微结构。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.将Ti粉(粒径为1～5μm)、Zr粉(粒径为1～5μm)、Nb粉(粒径为1～5μm)、Ta粉(粒径为1～5μm)、Mo粉(粒径为1～5μm)、C粉(粒径为30～100nm)和Si粉(粒径为30～100nm)称量混合；以Ti粉、Zr粉、Nb粉、Ta粉、Mo粉的总物质的量为100％计，Ti粉物质的量占比为20mol％，Zr粉物质的量占比为20mol％，Nb粉物质的量占比为20mol％，Ta粉物质的量占比为20mol％，Mo粉物质的量占比为20mol％。C粉物质的量和Ti、Zr、Nb、Ta、Mo、C粉总物质的量之比为1.2:1。Si粉和C粉的物质的量比为1:6；
2.将混合粉体装入粉体包覆机内，以3000rad/min运行10min。对粉体包覆后取出混合粉体，将混合粉体装入石墨模具，干压成坯体；
3.将装有坯体的石墨模具放入放电等离子烧结炉，以100℃/min的速率升温至1000℃，开始充氩气并且开始加压，然后升温至1600℃，同时压力升至20MPa，并保温保压20min，保温结束后以100℃/min的速率降温，1000℃泄压完毕，800℃后随炉降温，得到碳化硅增硬增韧高熵碳化物的复相陶瓷，即为(Ti,Zr,Nb,Ta,Mo)C-SiC。
本实施例制得的碳化硅增硬增韧高熵碳化物复相陶瓷的相对密度为100％，维氏硬度为25.0GPa，断裂韧性为6.4MPa·m1/2。图1为实施例1的(Ti,Zr,Nb,Ta,Mo)C-SiC复相陶瓷的显微结构。从图1可以看到，黑色相为SiC相，白色相为(Ti,Zr,Nb,Ta,Mo)C相。SiC相的分布及大小并不均匀，这是反应烧结的典型特征。SiC相的存在证明了通过硅热碳热反应合成(Ti,Zr,Nb,Ta,Mo)C-SiC复相陶瓷是可行的。SiC相的存在优化了陶瓷的显微结构，提升了复相陶瓷的力学性能。
实施例2
1.将Ti粉(粒径为1～5μm)、Zr粉(粒径为1～5μm)、Nb粉(粒径为1～5μm)、Ta粉(粒径为1～5μm)、Mo粉(粒径为1～5μm)、C粉(粒径为30～100nm)、Si粉(粒径为30～100nm)称量混合；以Ti粉、Zr粉、Nb粉、Ta粉、Mo粉的总物质的量为100％计，Ti粉占比为20mol％，Zr粉占比为20mol％，Nb粉物质的量占比为20mol％，Ta粉占比为20mol％，Mo粉占比为20mol％。C粉物质的量和Ti、Zr、Nb、Ta、Mo、C粉总物质的量比为2:1。Si粉和C粉的物质的量比为1:2；
2.将混合粉体装入粉体包覆机内，以3000rad/min运行10min，对粉体包覆后取出混合粉体，将混合粉体装入石墨模具，干压成坯体；
3.将装有坯体的石墨模具放入放电等离子烧结炉，以100℃/min的速率升温至1000℃，开始充氩气并且开始加压，然后升温至1600℃，同时压力升至20MPa，并保温保压20min，保温结束后以100℃/min的速率降温，1000℃泄压完毕，800℃后随炉降温，得到碳化硅增硬增韧高熵碳化物的复相陶瓷，即为(Ti,Zr,Nb,Ta,Mo)C-SiC。
本实施例制得的碳化硅增硬增韧高熵碳化物的复相陶瓷的相对密度为100％，维氏硬度为26.3GPa，断裂韧性为7.0MPa·m1/2。图2为实施例2的(Ti,Zr,Nb,Ta,Mo)C-SiC复相陶瓷的显微结构。从图2可以看到，黑色相为SiC相，白色相为(Ti,Zr,Nb,Ta,Mo)C相。SiC相的分布及大小并不均匀，这是反应烧结的典型特征。同时，在增加硅粉的添加量后，部分反应生成的SiC由颗粒状转变为棒状(与图1相比)。这些棒状结构的SiC进一步提升了复相陶瓷的力学性能。
实施例3
1.将Ti粉、Zr粉、Nb粉、Ta粉、Mo粉、C粉和Si粉称量混合；以Ti粉、Zr粉、Nb粉、Ta粉、Mo粉的总物质的量为100％计，Ti粉占比为20mol％，Zr粉占比为20mol％，Nb粉占比为20mol％，Ta粉占比为20mol％，Mo粉占比为20mol％。C粉物质的量和Ti、Zr、Nb、Ta、Mo、C粉总物质的量比为1.2:1，Si粉和碳粉的物质的量比为1:6；
2.将混合粉体装入粉体包覆机内，以2500rad/min运行20min，对粉体包覆后取出混合粉体，将混合粉体装入石墨模具，干压成坯体；
3.将装有坯体的石墨模具放入热压烧结炉，以10℃/min的速率升温至1000℃，开始充氩气并且开始加压，然后升温至1800℃，同时压力升至30MPa，并保温保压30min，保温结束后以10℃/min的速率降温，1000℃泄压完毕，800℃后随炉降温，得到碳化硅增硬增韧高熵碳化物的复相陶瓷，即为(Ti,Zr,Nb,Ta,Mo)C-SiC。
本实施例制得的碳化硅增硬增韧高熵碳化物的复相陶瓷的相对密度为100％，维氏硬度为27.0GPa，断裂韧性为5.6MPa·m1/2。
本发明的复相陶瓷具有比高熵碳化物陶瓷更高的维氏硬度和断裂韧性，且相对密度接近100％，维氏硬度为25～27GPa，断裂韧性为5～7MPa·m1/2，可应用在制备切削难加工材料或航空航天耐磨零部件中。
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、组合和简化，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 (8)

1.一种碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，其特征在于，包括以下步骤：
S1.将Ti粉、Zr粉、Nb粉、Ta粉、Mo粉、C粉和Si粉混合，以Ti、Zr、Nb、Ta、Mo的总物质的量为100％计，Ti粉占比为20mol％，Zr粉占比为20mol％，Nb粉占比为20mol％，Ta粉占比为20mol％，Mo粉占比为20mol％；C粉的摩尔量与Ti粉、Zr粉、Nb粉、Ta粉、Mo粉和C粉的总摩尔比为(1.2～2):1，Si粉和C粉的摩尔比为1:(2～6)；
S2.将Ti粉、Zr粉、Nb粉、Ta粉、Mo粉、C粉和Si粉的混合粉体经包覆机包覆后，干压成坯体，在保护气氛下，将坯体在1600～1800℃，压力为20～40MPa，进行放电等离子烧结或热压烧结，制得碳化硅增硬增韧高熵碳化物的复相陶瓷，所述复相陶瓷的分子式为(Ti,Zr,Nb,Ta,Mo)C-SiC。
2.根据权利要求1所述的碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，其特征在于，步骤S1中所述的Ti粉、Zr粉、Nb粉、Ta粉、Mo粉的粒径均为1～5μm；所述的C粉和Si粉的粒径均为30～100nm。
3.根据权利要求1所述的碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，其特征在于，步骤S2中所述包覆机的转速为2000～3000rad/min，所述包覆的时间为10～20min。
4.根据权利要求1所述的碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，其特征在于，步骤S2中所述放电等离子烧结的具体程序为：先以100～150℃/min的速率升温至1000～1200℃，开始充氩气并且开始加压，继续升温至1600～1800℃，同时压力升至20～40MPa；升温程序执行完毕后保温保压10～20min；然后以80～100℃/min的速率降温，1000～1200℃泄压完毕，温度降至750～850℃后随炉降温。
5.根据权利要求1所述的碳化硅增硬增韧高熵碳化物的复相陶瓷的制备方法，其特征在于，步骤S3中所述热压烧结的程序为：先以10～14℃/min的速率升温至1000℃开始充氩气并且开始加压，继续以6～8℃/min的速率升温至1600～1800℃，同时压力升至20～40MPa；升温程序执行完毕后保温保压0.5h～1.0h；然后以10～12℃/min的速率降温，1000～1200℃泄压完毕，降温至750～850℃后随炉降温。
6.一种碳化硅/高熵碳化物的复相陶瓷，其特征在于，所述复相陶瓷是由权利要求1～5任一项所述的方法制备得到。
7.根据权利要求6所述的碳化硅/高熵碳化物的复相陶瓷，其特征在于，所述复相陶瓷的相对密度大于99％，维氏硬度为25～27GPa，断裂韧性为5～7MPa·m1/2。
8.根据权利要求6或7所述的碳化硅/高熵碳化物的复相陶瓷在制备切削难加工材料或航空航天耐磨零部件中的应用。
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