CN106083065A - 一种高性能Si3N4‑TiC0.5N0.5复合梯度陶瓷刀具材料及其制备方法 - Google Patents
一种高性能Si3N4‑TiC0.5N0.5复合梯度陶瓷刀具材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高性能Si3N4‑TiC0.5N0.5复合梯度陶瓷刀具材料及其制备方法,梯度刀具材料表层以SNTC1为原料,以Al2O3和Re2O3为烧结助剂;心部以SNTC2为原料,以β‑Si3N4晶种、Al2O3和Re2O3为烧结助剂;将表层和心部混合粉体按照一定顺序装入热压炉模具,通过热压烧结制备表硬心韧高性能Si3N4‑TiC0.5N0.5复合梯度陶瓷刀具材料。利用该方法所制备的陶瓷刀具材料的相对密度高于97%,表层硬度为15~25GPa,断裂韧性为3~10MPa·m1/2,Iα/Iβ为0.30~0.90;心部硬度为10~20GPa,断裂韧性为6~14MPa·m1/2,Iα/Iβ为0~0.20。本发明通过引入纳米级和微米级TiC0.5N0.5、β‑Si3N4晶种及梯度结构,实现了一种表硬心韧高性能Si3N4‑TiC0.5N0.5复合梯度陶瓷刀具材料的制备。
Description
技术领域
本发明涉及材料领域,特别涉及一种高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料及其制备方法。
背景技术
随着我国航空航天、风力发电、汽车等制造业的高速发展,越来越多的零部件加工需要使用高速、高效、超精密数控加工设备,因此对刀具材料的要求不断提升。目前,国内外高速加工专用刀具普遍采用硬质合金及其涂层刀具,但随着绿色加工的提出,硬质合金刀具在未来的加工体系中具有很大的局限性,迫切需要开发可以承受更高切削速度和切削温度的刀具材料。Si3N4陶瓷刀具因具有较高的硬度、耐磨性及良好的高温力学性能,与金属的亲和力小,化学稳定性好,在高速切削领域和切削难加工材料方面,具有着硬质合金刀具无法比拟的优点。Si3N4陶瓷刀具材料的主要添加相有TiC、(W,Ti)C、TiN、TiCN、SiC等,与单相Si3N4陶瓷材料相比,添加第二相TiC0.5N0.5能显著提高Si3N4基复合陶瓷材料的抗弯强度和耐磨性。赵军等借鉴梯度功能材料概念,首次提出对陶瓷刀具材料的组成分布、微观结构进行设计以形成梯度模型。国外学者也相继应用梯度功能的概念设计材料,开发了高性能梯度功能硬质合金切削刀具,与均质硬质合金刀具相比具有高的抗磨损和抗破损能力、高的抗热震性。山东大学郑光明采用梯度结构制备并研究了Sialon-Si3N4梯度纳米复合陶瓷刀具的抗摩擦磨损性能、抗热冲击及抗疲劳性能。结果表明,在相同条件下,梯度陶瓷材料的摩擦系数和磨损率、抗热冲击及热疲劳性能均低于均质陶瓷材料。但是,与均质材料相比,这些梯度陶瓷材料界面之间因成分突变而存在较强的残余应力。
发明内容
本发明的目的在于克服现有技术中存在的缺点,提供一种界面间残余应力小、成本低、工艺简单、环境友好的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
本发明的另一目的在于提供一种上述高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法。
本发明的目的通过下述技术方案实现:
一种高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,包括下述步骤:
(1)将Si3N4粉和TiC0.5N0.5(纳米级)粉按照体积分数比为60~98%:2~40%的配比经混料、超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)复合粉体SNTC1;将Si3N4粉和TiC0.5N0.5(微米级)粉按照体积分数比为60~98%:2~40%的配比经混料、超声分散、干燥后,得到Si3N4-TiC0.5N0.5(微米级)复合粉体SNTC2;
(2)梯度刀具材料表层以SNTC1为原料,以Al2O3和Re2O3为烧结助剂;按照SNTC1:Al2O3:Re2O3的质量分数比为80~98%:1~10%:1~10%的配比,经混料、干燥后,得到SNTC1-Al2O3-Re2O3的混合粉体;
(3)梯度刀具材料心部以SNTC2为原料,以β-Si3N4晶种、Al2O3和Re2O3为烧结助剂;按照SNTC2:β-Si3N4晶种:Al2O3:Re2O3的质量分数比为60~98%:1~20%:0.5~10%:0.5~10%的配比,经混料、干燥后,得到SNTC2-β-Si3N4晶种-Al2O3-Re2O3的混合粉体;
(4)将SNTC1-Al2O3-Re2O3混合粉体作为陶瓷刀具材料表层成分,SNTC2-β-Si3N4晶种-Al2O3-Re2O3混合粉体作为陶瓷刀具材料心部成分,按照SNTC1-Al2O3-Re2O3、SNTC2-β-Si3N4晶种-Al2O3-Re2O3、SNTC1-Al2O3-Re2O3的顺序装入热压炉模具,通过热压烧结,获得表硬心韧的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
所述Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任一种。
步骤(1)中,Si3N4粉的纯度为95~100%,粒径为<10μm;TiC0.5N0.5(纳米级)粉的粒径<100nm;TiC0.5N0.5(微米级)粉的粒径为1.6um。
步骤(1)中,Si3N4与TiC0.5N0.5(纳米级)、Si3N4与TiC0.5N0.5(微米级)按所述体积分数比进行配料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合4~24h,超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)混合粉体SNTC1,Si3N4-TiC0.5N0.5(微米级)混合粉体SNTC2。
所述球磨机是辊式球磨机,在辊式球磨机上混合24h。
所述超声分散的功率为600W,20kHz,时间3min。
步骤(1)中,Si3N4:TiC0.5N0.5(纳米级)的体积分数比为70%:30%;Si3N4:TiC0.5N0.5(微米级)的体积分数比为70%:30%。
步骤(2)中,Al2O3粉的纯度为99.9%;Re2O3粉的纯度为99.9%。
步骤(3)中,β-Si3N4晶种的纯度为99.9%。
步骤(4)中,制备的刀具心部厚度为5~50mm,表层厚度为0.5~10mm。
步骤(2)和(3)中,混料是指以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合4~24h。
所述球磨机是辊式球磨机,在辊式球磨机上混合24h。
步骤(2)中,SNTC1:Al2O3:Re2O3的质量分数比为92%:2%:6%,其中Re=Y。
步骤(3)中,SNTC2:β-Si3N4晶种:Al2O3:Re2O3的质量分数比为89%:3%:2%:6%,其中Re=Y。
步骤(4)中,热压烧结是指:将表层和心部的混合粉体按照SNTC1-Al2O3-Re2O3、SNTC2-β-Si3N4晶种-Al2O3-Re2O3和SNTC1-Al2O3-Re2O3的顺序放入热压炉模具中,以50℃/min的升温速率将温度升至1000~1750℃,并保温0.5~4h,保温过程轴向加压为1~30MPa,整个烧结过程N2压力为1atm。
上述热压烧结的条件优选:以50℃/min的升温速率将温度升至1650℃,并保温1h,保温过程轴向加压为30MPa,整个烧结过程N2压力为1atm。
采用上述方法制备得到的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料,其相对密度高于96%,表层硬度为15~25GPa,断裂韧性为3~10MPa·m1/2,Iα/Iβ为030~0.90;心部硬度为10~20GPa,断裂韧性为6~14MPa·m1/2,Iα/Iβ为0.05~0.30。
优选地,高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的相对密度为99.5%,表层硬度为22GPa,断裂韧性为5MPa·m1/2,Iα/Iβ为0.80;心部硬度为17GPa,断裂韧性为11MPa·m1/2,Iα/Iβ为0.05。
本发明与现有技术相比具有如下优点和效果:
(1)本发明表层引入纳米级TiC0.5N0.5抑制了α-Si3N4到β-Si3N4的转变,提高了陶瓷刀具材料的硬度和耐磨损性能,心部引入微米级TiC0.5N0.5及β-Si3N4晶种,其α-Si3N4到β-Si3N4的转变程度增强,且存在较多的长棒状β-Si3N4晶粒而使其断裂韧性提高。
(2)相对于传统烧结的Si3N4陶瓷刀具材料,本发明通过引入梯度结构及纳米级和微米级的TiC0.5N0.5制备的Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料具有更优异的力学性能,能显著提高陶瓷刀具的耐磨损性能和使用寿命,且在高速连续切削过程中表现出很强的自砺性。
(3)相对于传统梯度陶瓷材料,本发明心部和表层所采用原料和烧结助剂均相同而使其界面间残余应力较小,力学性能更优异。
具体实施方式
下面结合实施例对本发明做进一步详细的描述,但本发明的实施方式不限于此。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。
实施例1
本发明的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,具体包括如下步骤:
(1)以Si3N4粉为原料,按照Si3N4:TiC0.5N0.5(纳米级和微米级)的体积分数为70%:30%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,经超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)复合粉体SNTC1和Si3N4-TiC0.5N0.5(微米级)复合粉体SNTC2;
(2)梯度刀具材料表层以SNTC1为原料,以Al2O3和Re2O3为烧结助剂;心部以SNTC2为原料,以β-Si3N4晶种、Al2O3和Re2O3为烧结助剂,其中Re=Y。
本实施例中,表层按照SNTC1:Al2O3:Y2O3的质量分数比为92%:2%:6%的配比进行混料,心部按照SNTC2:β-Si3N4晶种:Al2O3:Y2O3的质量分数比为89%:3%:2%:6%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,干燥后,得到表层为SNTC1-Al2O3-Y2O3的混合粉体,心部为SNTC2-β-Si3N4晶种-Al2O3-Y2O3的混合粉体。
(3)SNTC1-Al2O3-Y2O3混合粉体作为陶瓷刀具材料表层成分,SNTC2-β-Si3N4晶种-Al2O3-Y2O3混合粉体作为陶瓷刀具材料心部成分,按照SNTC1-Al2O3-Y2O3、SNTC2-β-Si3N4晶种-Al2O3-Y2O3和SNTC1-Al2O3-Y2O3顺序装入热压炉模具,以50℃/min的升温速率将温度升至1650℃,并保温1h,保温过程轴向加压为30MPa,整个烧结过程N2压力为1atm,通过热压烧结制备表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
本实施例制备得到的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的相对密度为99.5%,表层硬度为22GPa,断裂韧性为5MPa·m1/2,Iα/Iβ为0.80;心部硬度为17GPa,断裂韧性为11MPa·m1/2,Iα/Iβ为0.05。
实施例2
本发明实施例的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,具体如下:以Si3N4粉为原料,按照Si3N4:TiC0.5N0.5(纳米级和微米级)的体积分数为60%:40%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,经超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)复合粉体SNTC1和Si3N4-TiC0.5N0.5(微米级)复合粉体SNTC2;表层按照SNTC1:Al2O3:Y2O3的质量分数比为90%:5%:5%的配比进行混料,心部按照SNTC2:β-Si3N4晶种:Al2O3:Y2O3的质量分数比为87%:3%: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,干燥后,得到表层为SNTC1-Al2O3-Y2O3的混合粉体,心部为SNTC2-β-Si3N4晶种-Al2O3-Y2O3的混合粉体。按照实施例1方法制备Si3N4-TiC0.5N0.5复合梯度陶瓷,其中以40℃/min的升温速率将温度升至1700℃,并保温1h,保温过程轴向加压为25MPa,整个烧结过程N2压力为1atm,通过热压烧结制备表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
本实施例制备得到的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的相对密度为99%,表层硬度为21GPa,断裂韧性为5.5MPa·m1/2,Iα/Iβ为0.70;心部硬度为17.5GPa,断裂韧性为12MPa·m1/2,Iα/Iβ为0。
实施例3
本发明实施例的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,具体如下:以Si3N4粉为原料,按照Si3N4:TiC0.5N0.5(纳米级和微米级)的体积分数为60%:30%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,经超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)复合粉体SNTC1和Si3N4-TiC0.5N0.5(微米级)复合粉体SNTC2;表层按照SNTC1:Al2O3:Lu2O3的质量分数比为90%:2%:6%的配比进行混料,心部按照SNTC2:β-Si3N4晶种:Al2O3:Lu2O3的质量分数比为87%:3%:2%:6%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,干燥后,得到表层为SNTC1-Al2O3-Lu2O3的混合粉体,心部为SNTC2-β-Si3N4晶种-Al2O3-Lu2O3的混合粉体。按照实施例1方法制备Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料,其中以50℃/min的升温速率将温度升至1600℃,并保温2h,保温过程轴向加压为35MPa,整个烧结过程N2压力为1atm,通过热压烧结制备表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
本实施例制备得到的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的相对密度为99.5%,表层硬度为22GPa,断裂韧性为4.5MPa·m1/2,Iα/Iβ为0.75;心部硬度为16GPa,断裂韧性为11MPa·m1/2,Iα/Iβ为0.05。
实施例4
本发明实施例的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,具体如下:以Si3N4粉为原料,按照Si3N4:TiC0.5N0.5(纳米级和微米级)的体积分数为60%:30%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,经超声分散、干燥后,得到Si3N4-TiC0.5N0.5(纳米级)复合粉体SNTC1和Si3N4-TiC0.5N0.5(微米级)复合粉体SNTC2;表层按照SNTC1:Al2O3:La2O3:Lu2O3的质量分数比为90%:2%:3%:3%的配比进行混料,心部按照SNTC2:β-Si3N4晶种:Al2O3:La2O3:Lu2O3的质量分数比为87%:3%:2%:3%:3%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,干燥后,得到表层为SNTC1-Al2O3-La2O3-Lu2O3的混合粉体,心部为SNTC2-β-Si3N4晶种-Al2O3-La2O3-Lu2O3的混合粉体。按照实施例1方法制备Si3N4-TiC0.5N0.5复合梯度陶瓷,其中以50℃/min的升温速率将温度升至1650℃,并保温1h,保温过程轴向加压为30MPa,整个烧结过程N2压力为1atm,通过热压烧结制备表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
本实施例制备得到的表硬心韧高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的相对密度为99.5%,表层硬度为21.5GPa,断裂韧性为5MPa·m1/2,Iα/Iβ为0.7;心部硬度为17GPa,断裂韧性为11.5MPa·m1/2,Iα/Iβ为0。
Claims (10)
1.一种高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于包括下述步骤:
(1)将Si3N4粉和TiC0.5N0.5纳米级粉按照体积分数比为60~98%:2~40%的配比经混料、超声分散、干燥后,得到Si3N4-TiC0.5N0.5纳米级复合粉体SNTC1;将Si3N4粉和TiC0.5N0.5微米级粉按照体积分数比为60~98%:2~40%的配比经混料、超声分散、干燥后,得到Si3N4-TiC0.5N0.5微米级复合粉体SNTC2;
(2)梯度刀具材料表层以SNTC1为原料,以Al2O3和Re2O3为烧结助剂;按照SNTC1:Al2O3:Re2O3的质量分数比为80~98%:1~10%:1~10%的配比,经混料、干燥后,得到SNTC1-Al2O3-Re2O3的混合粉体;
(3)梯度刀具材料心部以SNTC2为原料,以β-Si3N4晶种、Al2O3和Re2O3为烧结助剂;按照SNTC2:β-Si3N4晶种:Al2O3:Re2O3的质量分数比为60~98%:1~20%:0.5~10%:0.5~10%的配比,经混料、干燥后,得到SNTC2-β-Si3N4晶种-Al2O3-Re2O3的混合粉体;
(4)将SNTC1-Al2O3-Re2O3混合粉体作为陶瓷刀具材料表层成分,SNTC2-β-Si3N4晶种-Al2O3-Re2O3混合粉体作为陶瓷刀具材料心部成分,按照SNTC1-Al2O3-Re2O3、SNTC2-β-Si3N4晶种-Al2O3-Re2O3、SNTC1-Al2O3-Re2O3的顺序装入热压炉模具,通过热压烧结,获得表硬心韧的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料。
2.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:Re为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任一种。
3.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(1)中,Si3N4与TiC0.5N0.5纳米级粉、Si3N4与TiC0.5N0.5微米级粉按所述体积分数比进行配料,以乙醇为溶剂,以Si3N4球为球磨介质,在球磨机上混合4~24h,超声分散、干燥后,得到Si3N4-TiC0.5N0.5纳米级混合粉体SNTC1、Si3N4-TiC0.5N0.5微米级混合粉体SNTC2。
4.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(1)中,Si3N4:TiC0.5N0.5纳米级粉的体积分数比为70%:30%;Si3N4:TiC0.5N0.5微米级粉的体积分数比为70%:30%。
5.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(4)中,制备的刀具心部厚度为5~50mm,表层厚度为0.5~10mm。
6.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(2)中,SNTC1:Al2O3:Re2O3的质量分数比为92%:2%:6%,其中Re=Y。
7.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(3)中,SNTC2:β-Si3N4晶种:Al2O3:Re2O3的质量分数比为89%:3%:2%:6%,其中Re=Y。
8.根据权利要求1所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料的制备方法,其特征在于:步骤(4)中,热压烧结是指:将表层和心部的混合粉体按照SNTC1-Al2O3-Re2O3、SNTC2-β-Si3N4晶种-Al2O3-Re2O3和SNTC1-Al2O3-Re2O3的顺序放入热压炉模具中,以50℃/min的升温速率将温度升至1000~1750℃,并保温0.5~4h,保温过程轴向加压为1~30MPa,整个烧结过程N2压力为1atm。
9.一种高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料,其特征在于:采用权利要求1~8任一项所述制备方法制备得到,其相对密度高于96%,表层硬度为15~25GPa,断裂韧性为3~10MPa·m1/2,Iα/Iβ为030~0.90;心部硬度为10~20GPa,断裂韧性为6~14MPa·m1/2,Iα/Iβ为0.05~0.30。
10.根据权利要求9所述的高性能Si3N4-TiC0.5N0.5复合梯度陶瓷刀具材料,其特征在于:其相对密度为99.5%,表层硬度为22GPa,断裂韧性为5MPa·m1/2,Iα/Iβ为0.80;心部硬度为17GPa,断裂韧性为11MPa·m1/2,Iα/Iβ为0.05。
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