第二相对复相结构陶瓷力学性能的影响研究
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摘要
工程结构陶瓷包括用于各种环境中的耐磨、耐腐蚀、耐高温等构件的各类陶瓷材料,运用材料的微观结构设计来制造和加工满足各种使用要求,主要强调材料的力学性能。单相陶瓷的强度和韧性一般较低,因此向陶瓷基体中添加第二相是强韧化结构陶瓷的一种主要途径。在本论文中,使用热压烧结的方法制备了不同第二相形式的陶瓷基复相材料,第二相的类型包括微米、纳米颗粒及低熔点相等,并对复相陶瓷的力学性能进行了研究。通过研究得到的主要结论如下：
对于纳米SiC强化Al2O3复相陶瓷,在同样的制备工艺下,添加1～2wt%纳米SiC使纯Al2O3的弯曲强度由280 MPa提高到516 MPa,断裂韧性也由3.2 MPa·m1/2提高到约5 MPa·m1/2。表明少量纳米SiC颗粒添加对力学性能的提高起了很大的作用,纳米SiC颗粒位于Al2O3晶粒内部,由于对晶界扩散的抑制作用显著细化了纯Al2O3的晶粒尺寸,因此降低了陶瓷材料内部的微裂纹大小,这是导致复相陶瓷强度增大的重要原因。此外,由于SiC和Al2O3由于热膨胀系数的失配使晶内的SiC颗粒在Al2O3晶界上产生压应力强化了晶界,也是导致强度和韧性提高的原因。
对于微米SiC强化Al2O3复相陶瓷,随着SiC添加量的增多烧结性变差,烧结温度提高,强度随着SiC添加量的增加而提高,当添加量达到20wt%时,复相陶瓷的弯曲强度达到615 MPa；断裂韧性随着SiC的添加先增大后减小,当添加5wt%SiC时断裂韧性最大达到7.6 MPa·m1/2。晶粒细化以及SiC在复相陶瓷基体内产生的径向压应力、切向拉应力是复相陶瓷强度提高的主要原因,断裂韧性随着穿晶断裂的趋势越明显而逐渐减低,显微组织观察表明Al2O3/SiC界面结合良好。
对于液相烧结的AlN陶瓷,YAlO低熔点相的引入促进了AlN陶瓷的致密化。力学性能分析结果表明：由于气孔率的降低,纯AlN陶瓷的强度和韧性随着晶界低熔点相的加入而提高,当添加2wt%Y2O3时,弯曲强度由245 MPa提高到383 MPa,断裂韧性由2.88 MPa·m1/2提高到3.1 MPa·m1/2；随着烧结助剂添加量的增多,YAlO相的含量也增加,并且布满整个晶界,但复相陶瓷材料的强度和韧性却随之下降；显微结构分析表明低熔点相和AlN基体间的润湿性极差,界面结合强度低,并由于两相间的热膨胀系数差在两相界面处产生拉应力,更进一步弱化了界面结合,使裂纹扩展更容易,导致力学性能的下降。
对于B4C/SiC两相陶瓷材料,SiC的添加对B4C陶瓷的烧结致密度基本无影响,影响B4C陶瓷致密化的因素主要是初始的粉末粒度和烧结温度及压力,采用超细的亚微米B4C粉在2000℃、30 MPa烧结条件下制备出达到理论密度的B4C及B4C/SiC复相陶瓷。显微结构观察发现B4C/SiC界面间的结合力很强,裂纹沿着SiC晶内或晶间扩展,因此随着SiC相的加入,B4C陶瓷的弯曲强度由500 MPa提高到约700 MPa,但断裂韧性由于穿晶断裂的倾向略有下降。
Engineering ceramics are the ceramic materials applied in various environments such as wear resistance, corrosion resistance, and high temperature resistance etc. It has been produced and machined to satisfy kinds of need by means of designing microstructure, and it emphasize particularly on mechanical properties. Because the strength and toughness of single-phase ceramics are lower, adding second phases in single-phase ceramics is an effective approach to strengthen and toughen the engineering ceramics. In this paper, ceramic composites have been prepared by hot pressing sintering with different second phases, including microsized particles, nanosized particles or glass phase, and the mechanical properties of the ceramic composites have been investigated. The experimental results are as follows:
As for nanosized SiC strengthening Al2O3 ceramic composites,1～2wt% SiC addition enhanced the flexural strength of pure Al2O3 from 280 MPa to 516 MPa and the fracture toughness from 3.2 MPa·m1/2 to about 5 MPa·m1/2, which indicates that small amount nanosized SiC addition can lead to a great improvement of mechanical properties for Al2O3 ceramics. Nanosized SiC particles were located within Al2O3 grains and significantly refined the grain size of pure Al2O3 by inhibiting grain boundary migration, therefore decreased the size of microcrack in the sintered ceramics, and this was the main reason for strength improvement. In addition, the residual compressive stress on the Al2O3 grain boundary generated due to the mismatch of thermal expansion coefficient between SiC and Al2O3 matrix, which also resulted in the improvement of strength and toughness.
As for microsized SiC strengthening Al2O3 ceramic composites, the sintering propery became poor with the increase of SiC addition and the sintering temperature was increased. The flexural strength of ceramic composites was enhanced with adding the SiC content, and the flexural strength reached 615 MPa for 20wt% SiC addition. The fracture toughness increased at first then decreased and the highest fracture toughness was 7.6 MPa·m1/2 for 5wt%SiC composite. Grain refinement and the residual radial compressive stress and tangential tensile stress in the matrix are the main reasons for strength improvement, and fracture toughness gradually decreased with the tendency of transgranular fracture. The observation of microstructure showed the good bonding of Al2O3/SiC interface.
As for liquid phase sintered AlN ceramics, the addition of YAlO low melting point phase promoted the densification of AlN ceramics. The measurement of mechanical properties showed that the strength and toughness of pure AlN were increased with the addition of second phase due to the elimination of pures, and the flexural strength and fracture toughness were increased from 245 MPa and 2.88 MPa·m1/2 to 383 MPa and 3.1 MPa·m1/2 respectively. The content of YA10 phase increased and covered the whole AlN grain boundary with the increase of sintering aids, which however lowered the strength and toughness. The observation of microstructure indicated the poor wettability between AIN matrix and glass phase, therefore, the poor interfacial bonding. Moreover, the tensile stress between AIN and glass phase resulted from thermal mismatch between the two phases. This further weakened the interfacial bonding, made crack propagate more easily, and led to the decline of mechanical properties.
As for B4C/SiC two phase ceramics, the addition of SiC basically had no influence on the densificaton of B4C ceramics. The influencing factors were mainly the size of starting powders, sintering temperature, and pressure. Pure B4C and B4C/SiC composites with full density were obtained using the ultrafine submicrosized B4C powder under the sintering temperature of 2000℃and pressure of 30 MPa. It was found the strong B4C/SiC interfacial bonding by the observation of microstructure, and the crack propagated through SiC grain transgranularly or along SiC grain boundary. The flexural strength of pure B4C increased from 500 MPa to the highest of 700 MPa with the addition of SiC for ceramic composites, however the fracture toughness decined slightly because of the tendency of transgranular fracture.
对于纳米SiC强化Al2O3复相陶瓷,在同样的制备工艺下,添加1～2wt%纳米SiC使纯Al2O3的弯曲强度由280 MPa提高到516 MPa,断裂韧性也由3.2 MPa·m1/2提高到约5 MPa·m1/2。表明少量纳米SiC颗粒添加对力学性能的提高起了很大的作用,纳米SiC颗粒位于Al2O3晶粒内部,由于对晶界扩散的抑制作用显著细化了纯Al2O3的晶粒尺寸,因此降低了陶瓷材料内部的微裂纹大小,这是导致复相陶瓷强度增大的重要原因。此外,由于SiC和Al2O3由于热膨胀系数的失配使晶内的SiC颗粒在Al2O3晶界上产生压应力强化了晶界,也是导致强度和韧性提高的原因。
对于微米SiC强化Al2O3复相陶瓷,随着SiC添加量的增多烧结性变差,烧结温度提高,强度随着SiC添加量的增加而提高,当添加量达到20wt%时,复相陶瓷的弯曲强度达到615 MPa；断裂韧性随着SiC的添加先增大后减小,当添加5wt%SiC时断裂韧性最大达到7.6 MPa·m1/2。晶粒细化以及SiC在复相陶瓷基体内产生的径向压应力、切向拉应力是复相陶瓷强度提高的主要原因,断裂韧性随着穿晶断裂的趋势越明显而逐渐减低,显微组织观察表明Al2O3/SiC界面结合良好。
对于液相烧结的AlN陶瓷,YAlO低熔点相的引入促进了AlN陶瓷的致密化。力学性能分析结果表明：由于气孔率的降低,纯AlN陶瓷的强度和韧性随着晶界低熔点相的加入而提高,当添加2wt%Y2O3时,弯曲强度由245 MPa提高到383 MPa,断裂韧性由2.88 MPa·m1/2提高到3.1 MPa·m1/2；随着烧结助剂添加量的增多,YAlO相的含量也增加,并且布满整个晶界,但复相陶瓷材料的强度和韧性却随之下降；显微结构分析表明低熔点相和AlN基体间的润湿性极差,界面结合强度低,并由于两相间的热膨胀系数差在两相界面处产生拉应力,更进一步弱化了界面结合,使裂纹扩展更容易,导致力学性能的下降。
对于B4C/SiC两相陶瓷材料,SiC的添加对B4C陶瓷的烧结致密度基本无影响,影响B4C陶瓷致密化的因素主要是初始的粉末粒度和烧结温度及压力,采用超细的亚微米B4C粉在2000℃、30 MPa烧结条件下制备出达到理论密度的B4C及B4C/SiC复相陶瓷。显微结构观察发现B4C/SiC界面间的结合力很强,裂纹沿着SiC晶内或晶间扩展,因此随着SiC相的加入,B4C陶瓷的弯曲强度由500 MPa提高到约700 MPa,但断裂韧性由于穿晶断裂的倾向略有下降。
Engineering ceramics are the ceramic materials applied in various environments such as wear resistance, corrosion resistance, and high temperature resistance etc. It has been produced and machined to satisfy kinds of need by means of designing microstructure, and it emphasize particularly on mechanical properties. Because the strength and toughness of single-phase ceramics are lower, adding second phases in single-phase ceramics is an effective approach to strengthen and toughen the engineering ceramics. In this paper, ceramic composites have been prepared by hot pressing sintering with different second phases, including microsized particles, nanosized particles or glass phase, and the mechanical properties of the ceramic composites have been investigated. The experimental results are as follows:
As for nanosized SiC strengthening Al2O3 ceramic composites,1～2wt% SiC addition enhanced the flexural strength of pure Al2O3 from 280 MPa to 516 MPa and the fracture toughness from 3.2 MPa·m1/2 to about 5 MPa·m1/2, which indicates that small amount nanosized SiC addition can lead to a great improvement of mechanical properties for Al2O3 ceramics. Nanosized SiC particles were located within Al2O3 grains and significantly refined the grain size of pure Al2O3 by inhibiting grain boundary migration, therefore decreased the size of microcrack in the sintered ceramics, and this was the main reason for strength improvement. In addition, the residual compressive stress on the Al2O3 grain boundary generated due to the mismatch of thermal expansion coefficient between SiC and Al2O3 matrix, which also resulted in the improvement of strength and toughness.
As for microsized SiC strengthening Al2O3 ceramic composites, the sintering propery became poor with the increase of SiC addition and the sintering temperature was increased. The flexural strength of ceramic composites was enhanced with adding the SiC content, and the flexural strength reached 615 MPa for 20wt% SiC addition. The fracture toughness increased at first then decreased and the highest fracture toughness was 7.6 MPa·m1/2 for 5wt%SiC composite. Grain refinement and the residual radial compressive stress and tangential tensile stress in the matrix are the main reasons for strength improvement, and fracture toughness gradually decreased with the tendency of transgranular fracture. The observation of microstructure showed the good bonding of Al2O3/SiC interface.
As for liquid phase sintered AlN ceramics, the addition of YAlO low melting point phase promoted the densification of AlN ceramics. The measurement of mechanical properties showed that the strength and toughness of pure AlN were increased with the addition of second phase due to the elimination of pures, and the flexural strength and fracture toughness were increased from 245 MPa and 2.88 MPa·m1/2 to 383 MPa and 3.1 MPa·m1/2 respectively. The content of YA10 phase increased and covered the whole AlN grain boundary with the increase of sintering aids, which however lowered the strength and toughness. The observation of microstructure indicated the poor wettability between AIN matrix and glass phase, therefore, the poor interfacial bonding. Moreover, the tensile stress between AIN and glass phase resulted from thermal mismatch between the two phases. This further weakened the interfacial bonding, made crack propagate more easily, and led to the decline of mechanical properties.
As for B4C/SiC two phase ceramics, the addition of SiC basically had no influence on the densificaton of B4C ceramics. The influencing factors were mainly the size of starting powders, sintering temperature, and pressure. Pure B4C and B4C/SiC composites with full density were obtained using the ultrafine submicrosized B4C powder under the sintering temperature of 2000℃and pressure of 30 MPa. It was found the strong B4C/SiC interfacial bonding by the observation of microstructure, and the crack propagated through SiC grain transgranularly or along SiC grain boundary. The flexural strength of pure B4C increased from 500 MPa to the highest of 700 MPa with the addition of SiC for ceramic composites, however the fracture toughness decined slightly because of the tendency of transgranular fracture.
引文
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