Ti_3SiC_2增强Cu基复合材料及金属/Ti_3SiC_2-SiC层状材料的制备研究
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摘要
三元化合物碳化硅钛（Ti_3SiC_2）是一种新型陶瓷材料，理论密度为4.53 g/cm~3，熔点超过3000℃，由于其兼具金属与陶瓷的双重特性而引起广泛关注。它象金属一样具有良好的导热、导电性，并对热震不敏感，高温下表现塑性行为，又象陶瓷一样具有高熔点、高屈服强度、耐腐蚀、抗氧化等性能，被认为是作为高温结构材料及电极材料最具应用前景的新型陶瓷材料之一。本文采用无压烧结制备出纯度较高的Ti_3SiC_2陶瓷材料，对其作为增强相在Cu基复合材料中的应用做了探索，并采用无压烧结和放电等离子烧结技术制备出(1-x)Ti_3SiC_2-xSiC (x=0-1)复合材料，在此基础上，采用放电等离子烧结制备出Ti、Mo、W/Ti_3SiC_2和Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC层状复合材料，对Ti、Mo、W/Ti_3SiC_2层状材料的界面及高温热稳定性进行了研究。
采用钛粉、硅粉、石墨粉为原料，无压烧结制备Ti_3SiC_2材料。由于硅熔点较低，在烧结过程中极易挥发，因此，原料中的硅含量对烧结产物的成分影响很大。实验结果表明，采用原始元素配比Ti_3Si_(1.1)C_2，烧结产物中杂质含量较少。无压烧结制备的Ti_3SiC_2块体经研磨过筛后可以得到颗粒度约10μm的Ti_3SiC_2粉末，采用化学方法对其进行镀铜，并和Cu粉混合后以温压、烧结工艺制备出不同Ti_3SiC_2含量的Cu基复合材料，并对其进行了轧制处理。结果表明Ti_3SiC_2含量为5 wt%的Cu基复合材料具有良好的力学性能，且当变形率为30%时，试样具有良好的力学性能和抗摩擦磨损能力，密度可达8.28 g/cm~3，抗拉强度为288MPa，电阻率为7.0×10~(-8)Ωm硬度可达HB106，摩擦系数为0.17。
为探索金属-陶瓷的连接，本文选用Ti_3SiC_2陶瓷和适合作为耐高温、耐磨损和核装置材料的SiC陶瓷制备(1-x)Ti_3SiC_2-xSiC复合材料作为金属-SiC复合材料的中间过渡层。采用钛粉、碳化硅粉、石墨粉为原料，经1500℃无压烧结可以制备出(1-x)Ti_3SiC_2-xSiC复合材料，但其密度较低，采用放电等离子烧结技术可以制备出符合成分设计要求的(1-x)Ti_3SiC_2-xSiC复合材料，仅有极少量杂质相存在，且致密度均在95%以上，但烧结温度较高，且SiC含量不同，复合材料的最佳烧结温度也随之变化。采用钛粉、硅粉、石墨粉为原料，并用铝粉作为烧结助剂，以1300℃SPS烧结15 min可以制备出純净的0.9Ti_3SiC_2-0.1SiC复合材料和含有少量残存C的0.8Ti_3SiC_2-0.2SiC复合材料。随着设计成分中SiC含量的增加，复合材料密度、抗弯强度有所下降但维氏硬度和电阻率均有所提高。
采用钛粉、钨粉、钼粉、硅粉、石墨粉为原料，添加Al粉作为烧结助剂，利用放电等离子烧结技术可以成功制备出Ti、Mo、W/Ti_3SiC_2层状复合材料，并对其抗弯强度和界面热稳定性进行了研究。实验结果表明Ti、Mo/Ti_3SiC_2层状复合材料致密度和抗弯强度均高于W/Ti_3SiC_2层状复合材料，Ti/Ti_3SiC_2层状复合材料界面中间过渡层为Ti/Ti+TiC/TiC+Ti_5Si_3C_x/Ti_5Si_3C_x/Ti_3SiC_2，Mo/Ti_3SiC_2层状复合材料界面中间过渡层为Mo/Mo_2C/MoSi_2/Ti_5Si_3C_x/Ti_3SiC_2，W/Ti_3SiC_2层状复合材料界面的中间过渡层为W与C的化合物。
以Ti_3SiC_2、Ti_3SiC_2-SiC和Ti、Mo、W/Ti_3SiC_2层状材料的制备为基础，采用放电等离子烧结技术制备出Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC多层层状复合材料。过渡层界面都较平直和清晰，界面结合紧密，且没有明显的孔洞、裂纹出现。
Ternary compound titanium silicon carbide (Ti_3SiC_2) is a new class of ceramic material,it has a density of 4.53 g/cm~3 and high melting point of 3000℃, and it combines the meritsof metals and ceramics. Like metals, it has good thermal and electrical conductivities, goodthermal shock resistance. Like ceramics, it has high melting point, high yield strength,excellent corrosion and oxidation resistance, so it is deemed as one of the Most perspectivenew ceramic materials which can be used as structural material for high-temperatureapplications and also as electrode materials. In this work, high purity Ti_3SiC_2 and Ti_3SiC_2particulate reinforced copper matrix composite were fabricated by pressureless sintering.(1-x)Ti_3SiC_2-xSiC composites were also prepared by using pressureless sintering and sparkplasma sintering (SPS). Based on these results, Ti、Mo、W/Ti_3SiC_2 and Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC layered materials were also prepared. Interface thermal stability of Ti、Mo、W/Ti_3SiC_2 layered materials at elevated temperatures were studied also.
Powder mix of Ti、Si、C were used to prepare bulk Ti_3SiC_2 by pressureless sintering, theSi content of the starting powder has strong influence on the phase constituent of the sinteredsample, due to the low melting point of Si, which melt and vaporize at high temperature.Results show that when Ti, Si and C powders were mixed with a stoichiometric Molar ratio of3:1.1:1, the sintered samples contain less impurity, TiC, a non-preferable impurity wasavoided. The grinded Cu coated Ti_3SiC_2 with an average particles size of around 10μm wasmixed with Cu powder to fabricate Ti_3SiC_2 particulate reinforced copper matrix composite bywarm compaction, sintering and rolling process. Results showed that sintered composite with5 mass% Ti_3SiC_2 has a good mechanical properties, the rolled composite with 30%deformation has a density of 8.28 g/cm~3, an ultimate tensile strength of 288 MPa, an electricalresistivity of 7.0×10~(-8)Ωm, a hardness of HB 106 and a friction coefficient of 0.17.
(1-x)Ti_3SiC_2-xSiC composite were used as the interlayers for metal-ceramic composite.Powder made of Ti、SiC、C were used, after pressureless sintering at 1500℃(1-x)Ti_3SiC_2-xSiC composites were fabricated, but the density of the sample is quite low.However, (1-x)Ti_3SiC_2-xSiC composites with relative density higher than 95% were preparedby using spark plasma sintering, but the sintering temperature increased with decreasing SiCcontents. Starting powder mix of Ti, Si, C and Al were used to fabricate pure0.9Ti3SiC-0.1SiC composite and 0.8Ti_3SiC_2-0.2SiC composite (with a little C impurity) byspark plasma sintering at 1300℃for 15 min. Experimental results showed that both the density and flexural strength of the sample decreased with increasing SiC contents, however,the Vickers hardness and electrical resistivity increased with increasing SiC contents.
Ti、Mo、W/Ti_3SiC_2 layered composite were successfully prepared by spark plasmasintering using powders of Ti, Mo, W, Si, C as starting materials and Al as sintering aids. theflexural strength and thermal stability of the sample were studied. Results show that thedensity and the flexural strength of the Ti、Mo/Ti_3SiC_2 composite are both higher than that ofthe W/Ti_3SiC_2 composite. After annealing, The intermediate layers formed at Ti/Ti_3SiC_2 areTi/Ti+TiC/TiC+Ti_5Si_3C_x/Ti_5Si_3C_x/Ti_3SiC_2, the intermediate layers formed at Mo/Ti_3SiC_2 areMo/Mo_2C/MoSi_2/Ti_5Si_3C_x/Ti_3SiC_2, the intermediate layers formed at W/Ti_3SiC_2 compositeare compounds of W and C.
Based on the above fabrication techniques, Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC layeredcomposite were synthesized by spark plasma sintering. Neat and Clean interfaces wereformed without noticeable micro-cracks and pores.
采用钛粉、硅粉、石墨粉为原料，无压烧结制备Ti_3SiC_2材料。由于硅熔点较低，在烧结过程中极易挥发，因此，原料中的硅含量对烧结产物的成分影响很大。实验结果表明，采用原始元素配比Ti_3Si_(1.1)C_2，烧结产物中杂质含量较少。无压烧结制备的Ti_3SiC_2块体经研磨过筛后可以得到颗粒度约10μm的Ti_3SiC_2粉末，采用化学方法对其进行镀铜，并和Cu粉混合后以温压、烧结工艺制备出不同Ti_3SiC_2含量的Cu基复合材料，并对其进行了轧制处理。结果表明Ti_3SiC_2含量为5 wt%的Cu基复合材料具有良好的力学性能，且当变形率为30%时，试样具有良好的力学性能和抗摩擦磨损能力，密度可达8.28 g/cm~3，抗拉强度为288MPa，电阻率为7.0×10~(-8)Ωm硬度可达HB106，摩擦系数为0.17。
为探索金属-陶瓷的连接，本文选用Ti_3SiC_2陶瓷和适合作为耐高温、耐磨损和核装置材料的SiC陶瓷制备(1-x)Ti_3SiC_2-xSiC复合材料作为金属-SiC复合材料的中间过渡层。采用钛粉、碳化硅粉、石墨粉为原料，经1500℃无压烧结可以制备出(1-x)Ti_3SiC_2-xSiC复合材料，但其密度较低，采用放电等离子烧结技术可以制备出符合成分设计要求的(1-x)Ti_3SiC_2-xSiC复合材料，仅有极少量杂质相存在，且致密度均在95%以上，但烧结温度较高，且SiC含量不同，复合材料的最佳烧结温度也随之变化。采用钛粉、硅粉、石墨粉为原料，并用铝粉作为烧结助剂，以1300℃SPS烧结15 min可以制备出純净的0.9Ti_3SiC_2-0.1SiC复合材料和含有少量残存C的0.8Ti_3SiC_2-0.2SiC复合材料。随着设计成分中SiC含量的增加，复合材料密度、抗弯强度有所下降但维氏硬度和电阻率均有所提高。
采用钛粉、钨粉、钼粉、硅粉、石墨粉为原料，添加Al粉作为烧结助剂，利用放电等离子烧结技术可以成功制备出Ti、Mo、W/Ti_3SiC_2层状复合材料，并对其抗弯强度和界面热稳定性进行了研究。实验结果表明Ti、Mo/Ti_3SiC_2层状复合材料致密度和抗弯强度均高于W/Ti_3SiC_2层状复合材料，Ti/Ti_3SiC_2层状复合材料界面中间过渡层为Ti/Ti+TiC/TiC+Ti_5Si_3C_x/Ti_5Si_3C_x/Ti_3SiC_2，Mo/Ti_3SiC_2层状复合材料界面中间过渡层为Mo/Mo_2C/MoSi_2/Ti_5Si_3C_x/Ti_3SiC_2，W/Ti_3SiC_2层状复合材料界面的中间过渡层为W与C的化合物。
以Ti_3SiC_2、Ti_3SiC_2-SiC和Ti、Mo、W/Ti_3SiC_2层状材料的制备为基础，采用放电等离子烧结技术制备出Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC多层层状复合材料。过渡层界面都较平直和清晰，界面结合紧密，且没有明显的孔洞、裂纹出现。
Ternary compound titanium silicon carbide (Ti_3SiC_2) is a new class of ceramic material,it has a density of 4.53 g/cm~3 and high melting point of 3000℃, and it combines the meritsof metals and ceramics. Like metals, it has good thermal and electrical conductivities, goodthermal shock resistance. Like ceramics, it has high melting point, high yield strength,excellent corrosion and oxidation resistance, so it is deemed as one of the Most perspectivenew ceramic materials which can be used as structural material for high-temperatureapplications and also as electrode materials. In this work, high purity Ti_3SiC_2 and Ti_3SiC_2particulate reinforced copper matrix composite were fabricated by pressureless sintering.(1-x)Ti_3SiC_2-xSiC composites were also prepared by using pressureless sintering and sparkplasma sintering (SPS). Based on these results, Ti、Mo、W/Ti_3SiC_2 and Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC layered materials were also prepared. Interface thermal stability of Ti、Mo、W/Ti_3SiC_2 layered materials at elevated temperatures were studied also.
Powder mix of Ti、Si、C were used to prepare bulk Ti_3SiC_2 by pressureless sintering, theSi content of the starting powder has strong influence on the phase constituent of the sinteredsample, due to the low melting point of Si, which melt and vaporize at high temperature.Results show that when Ti, Si and C powders were mixed with a stoichiometric Molar ratio of3:1.1:1, the sintered samples contain less impurity, TiC, a non-preferable impurity wasavoided. The grinded Cu coated Ti_3SiC_2 with an average particles size of around 10μm wasmixed with Cu powder to fabricate Ti_3SiC_2 particulate reinforced copper matrix composite bywarm compaction, sintering and rolling process. Results showed that sintered composite with5 mass% Ti_3SiC_2 has a good mechanical properties, the rolled composite with 30%deformation has a density of 8.28 g/cm~3, an ultimate tensile strength of 288 MPa, an electricalresistivity of 7.0×10~(-8)Ωm, a hardness of HB 106 and a friction coefficient of 0.17.
(1-x)Ti_3SiC_2-xSiC composite were used as the interlayers for metal-ceramic composite.Powder made of Ti、SiC、C were used, after pressureless sintering at 1500℃(1-x)Ti_3SiC_2-xSiC composites were fabricated, but the density of the sample is quite low.However, (1-x)Ti_3SiC_2-xSiC composites with relative density higher than 95% were preparedby using spark plasma sintering, but the sintering temperature increased with decreasing SiCcontents. Starting powder mix of Ti, Si, C and Al were used to fabricate pure0.9Ti3SiC-0.1SiC composite and 0.8Ti_3SiC_2-0.2SiC composite (with a little C impurity) byspark plasma sintering at 1300℃for 15 min. Experimental results showed that both the density and flexural strength of the sample decreased with increasing SiC contents, however,the Vickers hardness and electrical resistivity increased with increasing SiC contents.
Ti、Mo、W/Ti_3SiC_2 layered composite were successfully prepared by spark plasmasintering using powders of Ti, Mo, W, Si, C as starting materials and Al as sintering aids. theflexural strength and thermal stability of the sample were studied. Results show that thedensity and the flexural strength of the Ti、Mo/Ti_3SiC_2 composite are both higher than that ofthe W/Ti_3SiC_2 composite. After annealing, The intermediate layers formed at Ti/Ti_3SiC_2 areTi/Ti+TiC/TiC+Ti_5Si_3C_x/Ti_5Si_3C_x/Ti_3SiC_2, the intermediate layers formed at Mo/Ti_3SiC_2 areMo/Mo_2C/MoSi_2/Ti_5Si_3C_x/Ti_3SiC_2, the intermediate layers formed at W/Ti_3SiC_2 compositeare compounds of W and C.
Based on the above fabrication techniques, Ti、Mo、W/(1-x)Ti_3SiC_2-xSiC layeredcomposite were synthesized by spark plasma sintering. Neat and Clean interfaces wereformed without noticeable micro-cracks and pores.
引文
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