CN106904977A - 一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法 - Google Patents
一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法 Download PDFInfo
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Abstract
本发明公开了一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法,其以Si3N4粉为原料,以Al2O3‑Re2O3为烧结助剂,Si3N4、Al2O3和Re2O3分别按质量分数比经混料、干燥后得到Si3N4‑Al2O3‑Re2O3混合粉体;将混合粉体通过热压烧结获得Si3N4陶瓷坯体;将所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4‑Al2O3‑Re2O3混合粉体作为陶瓷材料表层,通过热压烧结获得Si3N4陶瓷材料。利用该方法所制备的陶瓷材料的相对密度高于99%,表层硬度为15~25GPa,断裂韧性为6~10MPa·m1/2,心部硬度为10~20GPa,断裂韧性为8~14MPa·m1/2。
Description
技术领域
本发明涉及非氧化物基陶瓷材料领域,具体公开了一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法。
背景技术
Si3N4陶瓷材料因具有高强度、硬度和断裂韧性,良好的热稳定性及抗腐蚀性能而被广泛研究。通过改变配方或显微形貌获得的Si3N4梯度陶瓷材料因具有较好的综合力学性能而广泛应用于切削刀具,轴承球及发动机关键零部件等。
目前,有关Si3N4基梯度陶瓷材料已有很多研究,但大多集中在分层系统设计上,即通过调节层与层之间的配方而获得梯度结构。例如,Thompson等人通过在SiC基体表层引入Si3N4而制备了Si3N4-SiC复合梯度陶瓷材料。Belmonte等人也采用SPS烧结技术通过原位法制备Si3N4渐进式梯度陶瓷材料。
相对于传统烧结的Si3N4梯度陶瓷材料,本发明通过引入两步烧结法制备表层和心部成分相同且界面结合较好的Si3N4陶瓷材料,既不存在因成分差异引起的应力问题,同时也具有表硬心韧的力学性能。
发明内容
本发明所要解决的技术问题在于提供一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法。
为解决上述技术问题,本发明通过如下技术方案。
一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法,包括如下步骤:
(1)以Si3N4粉为基体原料,以Al2O3-Re2O3为烧结助剂,按照按Si3N4:Al2O3-Re2O3的质量分数比为98~80%:2~20%的配比经混料、干燥后,得到Si3N4-Al2O3-Re2O3混合粉体,其中Re=Sc,Y,La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu中的任一种,所述的Al2O3-Re2O3中的Al2O3:Re2O3质量分数比为1~99%:99~1%;
(2)将Si3N4-Al2O3-Re2O3混合粉体,通过热压烧结制备Si3N4陶瓷坯体;
(3)将所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4-Al2O3-Re2O3混合粉体作为陶瓷材料表层,通过热压烧结获得表硬心韧Si3N4陶瓷材料。
上述步骤(1)中,Si3N4粉纯度为95~100%,粒径为<10μm;Al2O3粉纯度为99.99%;Re2O3粉纯度为99.99%。
上述步骤(1)中,将Si3N4和Al2O3-Re2O3按所述质量分数比进行配料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合4~24h,干燥后得到Si3N4-Al2O3-Re2O3混合粉体。
上述步骤(1)中,球磨机是辊式球磨机,在辊式球磨机上混合24h。
上述步骤(1)中,Si3N4:Al2O3-Re2O3的质量分数比为90%:10%,其中Re=Y;所述的Al2O3-Re2O3中的Al2O3:Re2O3(Re=Y)质量分数比为50%:50%。
上述步骤(2)中,热压烧结方法为:将混合粉体放入热压炉模具,以15℃/min的升温速率将温度升至1000~1250℃,然后以10℃/min的升温速率将温度升至1300~1700℃,然后以5℃/min的升温速率将温度升至1700~2000℃,并保温0.5~4h,整个烧结过程为1atm的氮气,烧结压力10~40MPa,通过热压烧结获得断裂韧性高的陶瓷坯体。
上述步骤(2)中,热压烧结方法为:将混合粉体放入热压炉模具,以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,然后以5℃/min的升温速率将温度升至1800℃,并保温1.5h,整个烧结过程为1atm的氮气,烧结压力30MPa,通过热压烧结获得断裂韧性高的陶瓷坯体。
上述步骤(3)中,热压烧结方法为:将所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4-Al2O3-Re2O3混合粉体作为陶瓷材料表层,以15℃/min的升温速率将温度升至1000~1250℃,然后以10℃/min的升温速率将温度升至1300~1700℃,并保温0.5~4h,整个烧结过程为1atm的氮气,烧结压力10~40MPa,通过热压烧结获得表层硬度高、心部韧性高的陶瓷坯体。
上述步骤(3)中,热压烧结方法为:以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,并保温1h,整个烧结过程为1atm的氮气,烧结压力30MPa,通过热压烧结获得表层硬度高、心部韧性高的陶瓷坯体。
本发明制备得到的表硬心韧Si3N4陶瓷材料的相对密度高于99%,表层硬度为15~25GPa,断裂韧性为6~10MPa·m1/2,心部硬度为10~20GPa,断裂韧性为8~14MPa·m1/2。
优选地,本发明制备得到的表硬心韧Si3N4陶瓷材料的相对密度高于99.5%,表层硬度为19GPa,断裂韧性为8.5MPa·m1/2;心部硬度为16GPa,断裂韧性为11MPa·m1/2。
与现有技术相比,本发明的有益效果:(1)本发明通过引入两步热压烧结法实现了表硬心韧Si3N4陶瓷材料的制备;(2)该梯度材料表层和心部成分相同,不存在因成分差异而引起的应力问题;(3)该梯度结构能显著提高Si3N4陶瓷材料的抗疲劳性能,使Si3N4陶瓷具有更广阔的应用领域;(4)本发明制备得到的表硬心韧Si3N4陶瓷材料的相对密度高于99.5%,表层硬度为19GPa,断裂韧性为8.5MPa·m1/2;心部硬度为16GPa,断裂韧性为11MPa·m1/2。
附图说明
图1为本发明实施例1的流程图。
图2为本发明实施例1制备的表硬心韧Si3N4陶瓷材料表层和心部的XRD图谱。
图3为本发明实施例1制备的表硬心韧Si3N4陶瓷材料低倍界面SEM图
图4为本发明实施例1制备的表硬心韧Si3N4陶瓷材料高倍界面SEM图
图5为本发明实施例1制备的表硬心韧Si3N4陶瓷材料表层SEM图
图6为本发明实施例1制备的表硬心韧Si3N4陶瓷材料心部SEM图
具体实施方式
下面结合说明书和具体实施例对本发明做进一步详细、完整地说明,但决非限制本发明,本发明也并非仅局限于下述实施例的内容,下述所使用的实验方法若无特殊说明,均为本技术领域现有常规的方法,所使用的配料或材料,如无特殊说明,均为通过商业途径可得到的配料或材料。下面给出实施案例。
实施例1
如图1所示,一种两步烧结法制备表硬心韧Si3N4陶瓷材料,具体方法如下:
(1)以Si3N4粉(粒径<10μm)为基体原料,以Al2O3-Y2O3为烧结助剂。
本实施例中,按照Si3N4:Al2O3:Y2O3的质量分数比为90%:5%:5%的配比进行混料,以乙醇为溶剂,以Si3N4球为球磨介质,在辊式球磨机上混合24h,经混料、干燥后,得到混合均匀的Si3N4-Al2O3-Y2O3混合粉体。
(2)将Si3N4-Al2O3-Y2O3混合粉体放入热压炉模具,以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,然后以5℃/min的升温速率将温度升至1800℃,并保温1.5h,整个过程烧结气氛为1atm的氮气,烧结压力30MPa,通过热压烧结获得断裂韧性高的Si3N4陶瓷坯体。
(3)将所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4-Al2O3-Re2O3混合粉体作为陶瓷材料表层,以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,整个过程烧结气氛为1atm的氮气,烧结压力30MPa,通过热压烧结获得表层硬度高,心部韧性高的陶瓷坯体。
本发明制备得到的表硬心韧Si3N4陶瓷材料,其相对密度为99.5%,表层硬度为19GPa,断裂韧性为8.5MPa·m1/2,心部硬度为16GPa,断裂韧性为11MPa·m1/2。
实施例2
本发明实施例制备表硬心韧Si3N4陶瓷材料的方法,具体如下:心部按照Si3N4粉质量分数为87%、β-Si3N4晶种粉质量分数为3%,Al2O3-Y2O3粉的质量分数为10%的配比进行配料,其中Al2O3:Y2O3质量分数比为50%:50%;表层按照Si3N4粉质量分数为90%,Al2O3-Y2O3粉的质量分数为10%的配比进行配料,其中Al2O3:Y2O3质量分数比为50%:50%,按照实施例1中(1)的方法制备心部和表层混合粉体;再按照实施案例1中(2)的方法以本实施例中的心部粉体为原料制备心部Si3N4陶瓷坯体;然后再按照实施案例1中(3)的方法制备Si3N4陶瓷坯体,其中表层粉体为本实施例中制备的表层混合粉体。
本实施例制备得到的Si3N4陶瓷材料的相对密度为99%,表层硬度为19GPa,断裂韧性为8.5MPa·m1/2,心部硬度为15.5GPa,断裂韧性为12.5MPa·m1/2。
实施例3
本发明实施例制备表硬心韧Si3N4陶瓷材料的方法,具体如下:心部按照Si3N4粉质量分数为90%、β-Si3N4晶种粉质量分数为3%,Al2O3-Y2O3粉的质量分数为10%的配比进行配料,其中Al2O3:Y2O3质量分数比为50%:50%;表层按照Si3N4粉质量分数为86%,Al2O3-Y2O3粉的质量分数为10%,TiO2粉的质量分数为4%的配比进行配料,其中Al2O3:Y2O3质量分数比为40%:60%,按照实施例1中(1)的方法制备心部和表层混合粉体;再按照实施案例1中(2)的方法以本实施例中心部粉体为原料制备心部Si3N4陶瓷坯体;然后再按照实施案例1中(3)的方法制备Si3N4陶瓷坯体,其中表层粉体为本实施例中制备的表层混合粉体。
本实施例制备得到的Si3N4陶瓷材料的相对密度为99.5%,表层硬度为20.5GPa,断裂韧性为9MPa·m1/2,心部硬度为15.5GPa,断裂韧性为12MPa·m1/2。
实施例4
本发明实施例制备表硬心韧Si3N4陶瓷材料的方法,具体如下:心部按照Si3N4粉质量分数为90%、β-Si3N4晶种粉质量分数为3%,Al2O3-Lu2O3粉的质量分数为10%的配比进行配料,其中Al2O3:Lu2O3质量分数比为50%:50%;表层按照Si3N4粉质量分数为86%,Al2O3-Y2O3粉的质量分数为10%,TiO2粉的质量分数为4%的配比进行配料,其中Al2O3:Y2O3质量分数比为40%:60%,按照实施例1中(1)的方法制备心部和表层混合粉体;再按照实施案例1中(2)的方法以本实施例中心部粉体为原料制备心部Si3N4陶瓷坯体;然后再按照实施案例1中(3)的方法制备Si3N4陶瓷坯体,其中表层粉体为本实施例中制备的表层混合粉体。
本实施例制备得到的Si3N4陶瓷材料的相对密度为99%,表层硬度为20.5GPa,断裂韧性为8.5MPa·m1/2,心部硬度为16.5GPa,断裂韧性为12MPa·m1/2。
Claims (10)
1.一种两步烧结法制备表硬心韧Si3N4陶瓷材料的方法,其特征在于包括如下步骤:
(1)以Si3N4粉为基体原料,以Al2O3-Re2O3为烧结助剂,按照按Si3N4:Al2O3-Re2O3的质量分数比为98~80%:2~20%的配比经混料、干燥后,得到Si3N4-Al2O3-Re2O3的混合粉体,其中Re=Sc,Y,La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu中的任一种,所述的Al2O3-Re2O3中的Al2O3:Re2O3质量分数比为1~99%:99~1%;
(2)将Si3N4-Al2O3-Re2O3混合粉体,通过热压烧结获得Si3N4陶瓷坯体;
(3)将所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4-Al2O3-Re2O3混合粉体作为陶瓷材料表层,通过热压烧结获得表硬心韧Si3N4陶瓷材料。
2.根据权利要求1所述的方法,其特征在于上述步骤(1)中,Si3N4粉纯度为95~100%,粒径为<10μm;Al2O3粉纯度为99.99%;Re2O3粉纯度为99.99%。
3.根据权利要求1所述的方法,其特征在于上述步骤(1)中,将Si3N4和Al2O3-Re2O3按所述质量分数比进行配料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合4~24h,干燥后得到Si3N4-Al2O3-Re2O3混合粉体。
4.根据权利要求3所述的方法,其特征在于上述步骤(1)中,球磨机是辊式球磨机,在辊式球磨机上混合24h。
5.根据权利要求1所述的方法,其特征在于上述步骤(1)中,Si3N4:Al2O3-Re2O3的质量分数比为90%:10%,其中Re=Y;所述的Al2O3-Re2O3中的Al2O3:Re2O3(Re=Y)质量分数比为50%:50%。
6.根据权利要求1所述的方法,其特征在于上述步骤(2)中,热压烧结方法为:将混合粉体放入热压炉模具,以15℃/min的升温速率将温度升至1000~1250℃,然后以10℃/min的升温速率将温度升至1300~1700℃,然后以5℃/min的升温速率将温度升至1700~2000℃,并保温0.5~4h,整个烧结过程为1atm的氮气,烧结压力10~40MPa,通过热压烧结获得断裂韧性高的陶瓷坯体。
7.根据权利要求6所述的方法,其特征在于上述步骤(2)中,热压烧结方法为:将混合粉体放入热压炉模具,以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,然后以5℃/min的升温速率将温度升至1800℃,并保温1.5h,整个烧结过程为1atm的氮气,烧结压力30MPa,通过热压烧结获得断裂韧性高的陶瓷坯体。
8.根据权利要求1所述的方法,其特征在于上述步骤(3)中,热压烧结方法为:所得Si3N4陶瓷坯体经研磨抛光后作为陶瓷材料心部,再在心部坯体上下表面覆盖Si3N4-Al2O3-Re2O3混合粉体作为陶瓷材料表层,以15℃/min的升温速率将温度升至1000~1250℃,然后以10℃/min的升温速率将温度升至1300~1700℃,并保温0.5~4h,整个烧结过程为1atm的氮气,烧结压力10~40MPa,通过热压烧结获得表层硬度高、心部韧性高的陶瓷坯体,其中心部厚度为5~50mm,表层厚度为0.5~10mm。
9.根据权利要求8所述的方法,其特征在于上述步骤(3)中,热压烧结方法为:以15℃/min的升温速率将温度升至1200℃,然后以10℃/min的升温速率将温度升至1600℃,并保温1h,整个烧结过程为1atm的氮气,烧结压力30MPa,通过热压烧结法获得表层硬度高、心部韧性高的陶瓷坯体。
10.根据权利要求1至9任一项所述的方法,其特征在于制备得到的表硬心韧Si3N4陶瓷材料的相对密度高于99%,表层硬度为15~25GPa,断裂韧性为6~10MPa·m1/2;心部硬度为10~20GPa,断裂韧性为8~14MPa·m1/2。
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