CN116217233A - 一种SiC晶须和高熵硼化物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SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用 Download PDFInfo
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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SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷及其制备方法和应用。该复相陶瓷是将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6混合粉体放入石墨模具,采用放电等离子烧结或热压烧结,制得SiC晶须和高熵硼化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2增硬增韧高熵碳化物的复相陶瓷,该复相陶瓷具有比单一的高熵碳化物陶瓷更高的维氏硬度和断裂韧性;且相对密度大于99%,维氏硬度为23~26GPa,断裂韧性为4~6MPa·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
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SiC晶须和高熵硼化物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
高熵碳化物陶瓷材料具有高熔点、高硬度、高耐磨性和高化学稳定性等优异性能,可应用于航空航天、高速切削刀具、军事装备和核能等领域。相较于传统过渡金属一元碳化物陶瓷材料,高熵碳化物陶瓷具有多样的元素组合和简单的单一相结构,在成分设计上拥有很大的发挥空间,是传统过渡金属一元碳化物陶瓷的理想替代材料。然而,由于高熵碳化物特殊的晶体结构,导致其断裂韧性低于传统的过渡金属一元碳化物陶瓷,限制了其进一步应用。故开发提升高熵碳化物陶瓷断裂韧性的有效手段,成为了现下研究者的研究重点。
高熵硼化物陶瓷属于超高温材料,具有良好的热稳定性和化学稳定性,引起了研究者的广泛关注。其有望成为超音速飞行器、火箭发动机等极端环境下的候选材料。高熵硼化物陶瓷的维氏硬度显著高于高熵碳化物陶瓷,将高熵硼化物以第二相的形式引入高熵碳化物陶瓷有望进一步提升高熵碳化物陶瓷的维氏硬度和高温性能。同时,晶须作为传统的增韧材料已被证明对高熵碳化物陶瓷具有很好的增韧效果。
目前,多采用直接添加高熵硼化物及晶须的方法来实现对高熵碳化物的增硬增韧,这种方法成本高、工艺复杂,且易受到原材料品质的影响。然而在高熵金属非氧化物陶瓷基材料领域,尚未报道过原位生成SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷材料。
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SiC晶须和高熵硼化物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SiC晶须和高熵硼化物均匀的分布在高熵碳化物基体中,极大地提高了复相材料的维氏硬度和断裂韧性。
本发明的另一目的在于提供上述SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的制备方法。该方法采用放电等离子烧结或热压烧结,将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体通过原位反应制得SiC晶须增硬增韧的高熵碳化物复相陶瓷。
本发明的再一目的在于提供上述SiC晶须和高熵硼化物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SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,所述的复相陶瓷是将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6混合,制得(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;将上述混合粉体加入无水乙醇,超声搅拌制得浆料;经辊式球磨机球磨、干燥和过筛后装入石墨模具,干压成坯体;在保护气氛下,将坯体在压力为20~40MPa,1800~2000℃进行放电等离子烧结或者热压烧结制得。
优选地,所述的复相陶瓷的相对密度大于98%,维氏硬度为23~26GPa,断裂韧性为4~6MPa·m1/2。
优选地,所述的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体的粒径为30nm~1μm;所述的SiB6粉体的粒径为1~6μm。
优选地,以(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6粉体的总质量为100%计,(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体的质量百分比为90~99wt.%,SiB6粉体的质量百分比为1~10wt.%。
所述的SiC晶须和高熵硼化物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.将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6混合,制得(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;
S2.将(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体加入无水乙醇,超声搅拌制得浆料;然后将氮化硅介质球加入浆料经辊式球磨机球磨,经干燥和过筛后装入石墨模具,干压成坯体;
S3.在保护气氛下,将坯体在压力为20~40MPa,1800~2000℃进行放电等离子烧结或者热压烧结,制得原位生成SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,分子式为SiC-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C。
优选地,步骤S2中所述球磨的转速为100~300r/min;所述球磨的时间为18~36h;所述干燥的温度为60~80℃,所述干燥的时间为12~24h。
优选地,步骤S3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,继续将温度升至1800~2000℃,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中所述热压烧结的具体程序为:先以10~14℃/min的升温速率升温,室温~1000℃开始充氩气并且开始加压,继续以6~8℃/min的升温速率升温,将温度升至1800~2000℃,同时压力升至20~40MPa;升温程序执行完毕后保温保压1~1.5h;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。
所述的SiC晶须和高熵硼化物增硬增韧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.本发明制得的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷具有高韧性、高硬度的优点。该复相陶瓷具有比单一的高熵碳化物陶瓷更高的维氏硬度和断裂韧性;且相对密度大于99%,维氏硬度为23~26GPa,断裂韧性为4~6MPa·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。
2.本发明采用了反应烧结工艺,通过在高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C加入SiB6,在高温下与高熵碳化物反应原位生成了高熵硼化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2和SiC晶须,且(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2和SiC晶须抑制了(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C晶粒长大,提高陶瓷力学性能。
3.本发明采用了反应烧结工艺,该工艺简单,成本低,节约能源。
附图说明
图1为实施例1制备的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的微观结构照片。
图2为实施例2制备的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的微观结构照片。
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.以质量分数比为93%:7%的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体(粒径为30nm~1μm)和六硼化硅粉体(SiB6)为原料,配制混合粉体,加入无水乙醇,并超声搅拌1h制得浆料。
2.将浆料在辊式球磨机以无水乙醇为分散剂,Si3N4球为球磨介质,以200r/min转速混料24h,在烘箱80℃干燥24h,过100目筛,得到混合均匀的(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;
3.将(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体装入石墨模具,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1800℃放电等离子烧结,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,得到原位生成的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,其分子式为SiC-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C。
图1为实施例1制备的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的微观结构照片。从图1中可知,深色相为SiC相,浅色相为(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C和(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2相。从样品的显微结构中未观察到气孔存在,说明样品经过烧结后实现了致密化。(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C和(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2相晶粒呈不规则状。同时,该样品生成的SiC晶须相比实施例2的样品生成的SiC晶须具有更大的长径比,可以更为有效的提升样品的断裂韧性。本实施例制得的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的相对密度为99%,维氏硬度为26.0GPa,断裂韧性为6.1MPa·m1/2。
实施例2
1.以质量分数比为94%:6%的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和六硼化硅粉体为原料,配制混合粉体,加入无水乙醇,并超声搅拌1h制得浆料。
2.将浆料在辊式球磨机以无水乙醇为分散剂,Si3N4球为球磨介质,以200r/min转速混料24h,在烘箱80℃干燥24h,过100目筛,得到混合均匀的(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;
3.将(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体装入石墨模具,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1850℃放电等离子烧结,同时压力升至30MPa,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,得到原位生成SiC晶须和高熵硼化物增硬增韧的高熵碳化物复相陶瓷,其分子式为SiC-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C。
图2为实施例2制备的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷的微观结构照片。由图2中可知,深色相为SiC相,浅色相为(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C和(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2相。从样品的显微结构中未观察到气孔存在,说明样品经过烧结后实现了致密化。同时(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C和(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2相晶粒呈不规则状。SiC晶须可以在陶瓷断裂过程中引发裂纹偏转、晶须拔出,从而有效的提升样品的断裂韧性。而(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2高熵硼化物相具有比(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C高熵碳化物相更高的硬度,从而提升了样品的硬度。本实施例制得的原位生成SiC晶须和高熵硼化物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25.6GPa,断裂韧性为5.3MPa·m1/2。
实施例3
1.以质量分数比为90%:10%的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6粉体为原料,配制混合粉体,加入无水乙醇,并超声搅拌1h制得浆料。
2.将浆料在辊式球磨机以无水乙醇为分散剂,Si3N4球为球磨介质,以200r/min转速混料24h,在烘箱80℃干燥24h后,过100目筛,得到混合均匀的(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;
3.将(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体装入石墨模具,放入热压烧结炉,以10℃/min的速率升温至1200℃,开始充氩气并且开始加压,然后以6℃/min的速率升温至2000℃热压烧结,同时压力升至40MPa,并保温保压60min,保温结束后以10℃/min的速率降温,1000℃泄压完毕,800℃后随炉降温,得到原位生成SiC晶须和高熵硼化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2增硬增韧的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C复相陶瓷。
本实施例制得的原位生成晶须及高熵硼化物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23.4GPa,断裂韧性为4.5MPa·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 (9)
1.一种SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,其特征在于,所述的复相陶瓷是将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6混合,制得(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;将上述混合粉体加入无水乙醇,超声搅拌制得浆料;经辊式球磨机球磨、干燥和过筛后装入石墨模具,干压成坯体;在保护气氛下,将坯体在压力为20~40MPa,1800~2000℃进行放电等离子烧结或者热压烧结制得。
2.根据权利要求1所述的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,其特征在于,所述的复相陶瓷的相对密度大于98%,维氏硬度为23~26GPa,断裂韧性为4~6MPa·m1/2。
3.根据权利要求1所述的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,其特征在于,所述的高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体的粒径为30nm~1μm;所述的SiB6粉体的粒径为1~6μm。
4.根据权利要求1所述的SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,其特征在于,以(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6粉体的总质量为100%计,(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体的质量百分比为90~99wt.%,SiB6粉体的质量百分比为1~10wt.%。
5.根据权利要求1-4任一项所述的SiC晶须和高熵硼化物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.将高熵碳化物(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C粉体和SiB6混合,制得(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体;
S2.将(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C-SiB6混合粉体加入无水乙醇,超声搅拌制得浆料;然后将氮化硅介质球加入浆料经辊式球磨机球磨,经干燥和过筛后装入石墨模具,干压成坯体;
S3.在保护气氛下,将坯体在压力为20~40MPa,1800~2000℃进行放电等离子烧结或者热压烧结,制得原位生成SiC晶须和高熵硼化物增硬增韧高熵碳化物的复相陶瓷,分子式为SiC-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)B2-(Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C。
6.根据权利要求5所述的SiC晶须和高熵硼化物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中所述球磨的转速为100~300r/min;所述球磨的时间为18~36h;所述干燥的温度为60~80℃,所述干燥的时间为12~24h。
7.根据权利要求5所述的SiC晶须和高熵硼化物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,继续将温度升至1800~2000℃,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。
8.根据权利要求5所述的SiC晶须和高熵硼化物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中所述热压烧结的具体程序为:先以10~14℃/min的升温速率升温,室温~1000℃开始充氩气并且开始加压,继续以6~8℃/min的升温速率升温,将温度升至1800~2000℃,同时压力升至20~40MPa;升温程序执行完毕后保温保压1~1.5h;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。
9.权利要求1-4任一项所述的SiC晶须和高熵硼化物增硬增韧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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