熔渗烧结制备Ti_3SiC_2及其摩擦磨损性能的研究
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摘要
近些年来,三元层状化合物Ti3SiC2因兼备金属和陶瓷的一些物理化学性能,而引起了材料学研究者强烈的研究兴趣。
本文分别以Ti/Si/C和Ti/Si/TiC粉末为原料,采用液态熔渗硅方法制备出纯度较高的Ti3SiC2材料,Ti3SiC2的相对含量分别达到93.6%和96.2%。研究表明,熔渗烧结制备Ti3SiC2的反应过程为：在1300℃以上,且未发生熔渗时,在Ti的富集区优先生成Ti5Si3,随着温度的升高,少部分Ti5Si3和β-Ti先熔合形成Ti-Si液相；在1500℃时,随着液态Si的渗入及流动扩散,液态的Si和剩余的Ti5Si3形成大量Ti-Si液相,将试样中的TiC包覆,通过液相反应生成大量的Ti3SiC2。其反应方程为：5Ti+3Si=Ti5Si3, Ti5Si3+2Si+10TiC=Ti3SiC2。
本文还研究了保护气体、原料配比、熔渗保温时间等主要因素对熔渗烧结的影响。研究表明：1)在原料润湿性满足熔渗反应的条件下,保护气体决定着熔融态的Si是否能够大量渗入预制体中,进而决定熔渗反应能否充分进行。本实验中,Ar气不但不参与反应,而且Ar的分子量大,气体流动时,从预制体中带出的熔融态Si也少,使生成Ti3SiC2的反应得以充分进行。2)以TiC/Ti/Si/C(石油焦)、TiC/Ti/Si、Ti/Si/C三种原料配比都能熔渗烧结出高纯度的Ti3SiC2陶瓷材料,但其差别主要表现在改善材料的致密性方面上。以TiC/Ti/Si为原料制备的Ti3SiC2,其含量高达96.2%,气孔率仅为7.86%,致密性最好,是原料配比选取中的最佳方案。3)熔渗保温时间决定着熔渗反应的进行程度,时间太短,熔渗反应不能充分进行；时间太长,熔渗反应产物会分解。本研究所选取的试样尺寸所对应的最佳保温时间为30 min。
本文还对熔渗烧结制备的Ti3SiC2块体材料的力学性能和摩擦磨损性能进行了研究。研究结果表明：以TiC/Ti/Si/C为原料和以Ti/Si/TiC为原料制备的Ti3SiC2材料,随着Ti3SiC2含量的增加,大量气孔被填满,材料的致密度增大,其抗弯强度和硬度都随Ti3SiC2含量的增加而增大。当Ti3SiC2的含量达到96.2%时,其抗弯强度为132.60 MPa,硬度也达到最大值156HB,力学性能得到很好的改善。
以TiC/Ti/Si/C为原料和以Ti/Si/TiC为原料制备的Ti3SiC2材料,随着Ti3SiC2的含量增加,其摩擦系数和体积磨损率都降低,且纯度越高,其摩擦系数和体积磨损率越小,Ti3SiC2的含量为96.2%的试样,其摩擦系数仅为0.211,体积磨损率仅为1.8×10-6mm3N-1m-1,摩擦磨损性能很好。
In recent years, the ternary layered compounds Ti3SiC2 which has special physical and chemical properties of metal and ceramic has attracted materials science researchers to study.
In this paper, the purer bulk Ti3SiC2 ceramic had been prepared from Ti/Si/C and Ti/Si/TiC mixed powders by use melt infiltrating method, respectively. The content of Ti3SiC2 in the two test samples can be up to 93.6% and 96.2%, respectively. The results showed that the reaction mechanism of Ti3SiC2 by melt infiltrating sintering method is that:above 1300℃and before the melting infiltrating takes place, the content of Ti is higher than that of Si in the sample and the Ti5Si3 is easier to form in the rich Ti areas. With the increase of temperature, few Ti5Si3 react withβ-Ti to become liquid mix phase of Ti-Si. With the liquid Si melting infiltrating, flowing and diffusing at 1500℃, great liquid Si will react with the rest Ti5Si3 to become liquid mix phase of Ti-Si. And then the liquid mix phase of Ti-Si will cover the TiC particle to take place liquid phase reaction. A great deal of Ti3SiC2 can be formed from this process. The reaction process is:
5Ti+3Si=Ti5Si3, Ti5Si3+2Si+10TiC=Ti3SiC2
The main influencing factors of infiltrating sinter such as protect gas, the ratio of raw materials and the infiltration holding time also were studied in this paper. Research shows that: 1) Under the condition that the wetting property of raw materials meet the infiltrate reaction, the protect gas determines whether a great deal of melted Si can be infiltrated into preformed sample, and affect the infiltration reaction can be fully carried out. In this experiment, Ar gas is not involved in reaction, and has large molecular weight, so when Ar gas flows from preformed sample to bring out the molten state Si less, and the generation of Ti3SiC2 reaction can be fully carried out.2) High purity Ti3SiC2 ceramic materials can be prepared by infiltration sintering with the three types of raw materials ratio of TiC/Ti/Si/C, TiC/Ti/Si and Ti/Si/C in this study, but the main difference is the improvement of the material compactness. Ti3SiC2 content in sample can be as higher as 96.2% in the preparation and the porosity is only 7.86% by use TiC/Ti/Si. It is the best raw materials selection.3) The holding time determines the degree of infiltrating reaction taking place. When the holding time is too little, the infiltrating reaction can not be fully carried out; but the holding time is too long, the production of melting infiltration will be decompose. The best holding time corresponded to the selected sample size in this study is 30 min.
The mechanical properties and friction and wear properties of infiltration sintering Ti3SiC2 block were studied in this article. The results showed that with the increase of the content Ti3SiC2, a large number of pores in the bulk Ti3SiC2 ceramic materials will be filled and its soundness will be increased when the bulk Ti3SiC2 is prepared by infiltration sintering with the three types of raw materials ratio of TiC/Ti/Si/C (petroleum coke), TiC/Ti/Si and Ti/Si/C, and its bending strength and hardness are increased with the increase of content of Ti3SiC2. When the content of Ti3SiC2 is up to 96.2%, its flexural strength can be up to 132.60 MPa, and Brinell hardness will also reach the maximum 156 HB. The mechanical properties of Ti3SiC2 can be improved greatly.
With the increase of content of Ti3SiC2, the friction coefficient and wear rate of bulk Ti3SiC2 ceramic materials prepared by infiltration sintering with the raw materials ratio of TiC/Ti/Si/C and Ti/Si/TiC will be decreased, and the higher purity of Ti3SiC2 is, the lower friction coefficient and wear rate of Ti3SiC2 is. When the content of Ti3SiC2 is 96.2%, its friction coefficient is just 0.211, its wear rate is 1.8×10-6mm3N-1m-1. This proves that the friction and wear properties of Ti3SiC2 have better.
本文分别以Ti/Si/C和Ti/Si/TiC粉末为原料,采用液态熔渗硅方法制备出纯度较高的Ti3SiC2材料,Ti3SiC2的相对含量分别达到93.6%和96.2%。研究表明,熔渗烧结制备Ti3SiC2的反应过程为：在1300℃以上,且未发生熔渗时,在Ti的富集区优先生成Ti5Si3,随着温度的升高,少部分Ti5Si3和β-Ti先熔合形成Ti-Si液相；在1500℃时,随着液态Si的渗入及流动扩散,液态的Si和剩余的Ti5Si3形成大量Ti-Si液相,将试样中的TiC包覆,通过液相反应生成大量的Ti3SiC2。其反应方程为：5Ti+3Si=Ti5Si3, Ti5Si3+2Si+10TiC=Ti3SiC2。
本文还研究了保护气体、原料配比、熔渗保温时间等主要因素对熔渗烧结的影响。研究表明：1)在原料润湿性满足熔渗反应的条件下,保护气体决定着熔融态的Si是否能够大量渗入预制体中,进而决定熔渗反应能否充分进行。本实验中,Ar气不但不参与反应,而且Ar的分子量大,气体流动时,从预制体中带出的熔融态Si也少,使生成Ti3SiC2的反应得以充分进行。2)以TiC/Ti/Si/C(石油焦)、TiC/Ti/Si、Ti/Si/C三种原料配比都能熔渗烧结出高纯度的Ti3SiC2陶瓷材料,但其差别主要表现在改善材料的致密性方面上。以TiC/Ti/Si为原料制备的Ti3SiC2,其含量高达96.2%,气孔率仅为7.86%,致密性最好,是原料配比选取中的最佳方案。3)熔渗保温时间决定着熔渗反应的进行程度,时间太短,熔渗反应不能充分进行；时间太长,熔渗反应产物会分解。本研究所选取的试样尺寸所对应的最佳保温时间为30 min。
本文还对熔渗烧结制备的Ti3SiC2块体材料的力学性能和摩擦磨损性能进行了研究。研究结果表明：以TiC/Ti/Si/C为原料和以Ti/Si/TiC为原料制备的Ti3SiC2材料,随着Ti3SiC2含量的增加,大量气孔被填满,材料的致密度增大,其抗弯强度和硬度都随Ti3SiC2含量的增加而增大。当Ti3SiC2的含量达到96.2%时,其抗弯强度为132.60 MPa,硬度也达到最大值156HB,力学性能得到很好的改善。
以TiC/Ti/Si/C为原料和以Ti/Si/TiC为原料制备的Ti3SiC2材料,随着Ti3SiC2的含量增加,其摩擦系数和体积磨损率都降低,且纯度越高,其摩擦系数和体积磨损率越小,Ti3SiC2的含量为96.2%的试样,其摩擦系数仅为0.211,体积磨损率仅为1.8×10-6mm3N-1m-1,摩擦磨损性能很好。
In recent years, the ternary layered compounds Ti3SiC2 which has special physical and chemical properties of metal and ceramic has attracted materials science researchers to study.
In this paper, the purer bulk Ti3SiC2 ceramic had been prepared from Ti/Si/C and Ti/Si/TiC mixed powders by use melt infiltrating method, respectively. The content of Ti3SiC2 in the two test samples can be up to 93.6% and 96.2%, respectively. The results showed that the reaction mechanism of Ti3SiC2 by melt infiltrating sintering method is that:above 1300℃and before the melting infiltrating takes place, the content of Ti is higher than that of Si in the sample and the Ti5Si3 is easier to form in the rich Ti areas. With the increase of temperature, few Ti5Si3 react withβ-Ti to become liquid mix phase of Ti-Si. With the liquid Si melting infiltrating, flowing and diffusing at 1500℃, great liquid Si will react with the rest Ti5Si3 to become liquid mix phase of Ti-Si. And then the liquid mix phase of Ti-Si will cover the TiC particle to take place liquid phase reaction. A great deal of Ti3SiC2 can be formed from this process. The reaction process is:
5Ti+3Si=Ti5Si3, Ti5Si3+2Si+10TiC=Ti3SiC2
The main influencing factors of infiltrating sinter such as protect gas, the ratio of raw materials and the infiltration holding time also were studied in this paper. Research shows that: 1) Under the condition that the wetting property of raw materials meet the infiltrate reaction, the protect gas determines whether a great deal of melted Si can be infiltrated into preformed sample, and affect the infiltration reaction can be fully carried out. In this experiment, Ar gas is not involved in reaction, and has large molecular weight, so when Ar gas flows from preformed sample to bring out the molten state Si less, and the generation of Ti3SiC2 reaction can be fully carried out.2) High purity Ti3SiC2 ceramic materials can be prepared by infiltration sintering with the three types of raw materials ratio of TiC/Ti/Si/C, TiC/Ti/Si and Ti/Si/C in this study, but the main difference is the improvement of the material compactness. Ti3SiC2 content in sample can be as higher as 96.2% in the preparation and the porosity is only 7.86% by use TiC/Ti/Si. It is the best raw materials selection.3) The holding time determines the degree of infiltrating reaction taking place. When the holding time is too little, the infiltrating reaction can not be fully carried out; but the holding time is too long, the production of melting infiltration will be decompose. The best holding time corresponded to the selected sample size in this study is 30 min.
The mechanical properties and friction and wear properties of infiltration sintering Ti3SiC2 block were studied in this article. The results showed that with the increase of the content Ti3SiC2, a large number of pores in the bulk Ti3SiC2 ceramic materials will be filled and its soundness will be increased when the bulk Ti3SiC2 is prepared by infiltration sintering with the three types of raw materials ratio of TiC/Ti/Si/C (petroleum coke), TiC/Ti/Si and Ti/Si/C, and its bending strength and hardness are increased with the increase of content of Ti3SiC2. When the content of Ti3SiC2 is up to 96.2%, its flexural strength can be up to 132.60 MPa, and Brinell hardness will also reach the maximum 156 HB. The mechanical properties of Ti3SiC2 can be improved greatly.
With the increase of content of Ti3SiC2, the friction coefficient and wear rate of bulk Ti3SiC2 ceramic materials prepared by infiltration sintering with the raw materials ratio of TiC/Ti/Si/C and Ti/Si/TiC will be decreased, and the higher purity of Ti3SiC2 is, the lower friction coefficient and wear rate of Ti3SiC2 is. When the content of Ti3SiC2 is 96.2%, its friction coefficient is just 0.211, its wear rate is 1.8×10-6mm3N-1m-1. This proves that the friction and wear properties of Ti3SiC2 have better.
引文
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