Ln_xZr_（1-x）O_（2-x/2）（Ln=Nd，Sm）纳米陶瓷粉体和块体的组织结构及热物理性能研究
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摘要
本文采用ZrOCl_2·8H_2O和稀土氧化物Ln_2O_3(Ln=Sm, Nd)粉体作为原材料,用化学共沉淀-煅烧法制备出不同成份配比的Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm) (x=0.1, 0.2, 0.3, 0.4)粉体。对800℃烧结、保温5小时热处理后的粉体,采用无压烧结工艺制备出Nd_xZr_(1-x)O_(2-x/2)和Sm_xZr_(1-x)O_(2-x/2)陶瓷块体材料。采用DSC、XRD、SEM等分析手段和激光热导仪对Ln_xZr_(1-x)O_(2-x/2) (Ln=Nd, Sm)陶瓷块体材料的微观组织结构和比热、热膨胀系数、热扩散系数及热导率等进行了系统的研究。
采用化学共沉淀-煅烧法制备出Nd_xZr_(1-x)O_(2-x/2)和Sm_xZr_(1-x)O_(2-x/2)的粉体。当x=0.1时,Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm)由m相和t相构成,而当x=0.2,0.3,0.4时,Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm)由t相和c相构成。粉体颗粒比较均匀,晶粒尺寸在100nm以下。采用无压烧结方法,在1600℃下烧结15小时,制备出NdxZr1-xO2-x/2和Sm_xZr_(1-x)O_(2-x/2)的陶瓷块体材料,对Ln_xZr_(1-x)O_(2-x/2)块体的物相分析可知,在x=0.1时,主要含有t相,同时含有少量的m相,在x=0.2,0.3时,含有t相和c相,在x=0.4时,完全是烧绿石相,块体晶粒尺寸在4~5μm之间。
通过对Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的比热分析,可以看出Sm0.1Zr0.9O1.95在786.8℃时发生相变,而其它成分的Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4)块体材料没有发生t-m的相变。当x=0.2, 0.3, 0.4时,随着Sm2O3稀土氧化物添加量的增加,Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4)的陶瓷块体材料的比热逐渐减小;而从Nd_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的比热分析来看, Nd0.1Zr0.9O1.95块体在911.3℃时发生相变,而其它成分的Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4)块体材料也没有发生t-m的相变。当x=0.2, 0.3, 0.4时,随着Nd2O3稀土氧化物添加量的增加,其比热值逐渐减小。
从SmxZr1-xOx/2(x=0.1, 0.2, 0.3, 0.4)陶瓷块体材料的热导率分析结果可以看出,当x=0.1时其热导率最低,当x=0.2, 0.3, 0.4时,大小在1.51W·m-1·K-1到2.39W·m-1·K-1之间变化。随着Sm2O3稀土氧化物添加量的增加,其热导率逐渐减小;而从Nd_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4)陶瓷块体材料的热导率的分析结果可以看出,大小在1.54 W·m-1·K-1到2.45W·m-1·K-1之间变化。
从Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的热膨胀系数分析结果可以看出, Sm0.1Zr0.9O1.95陶瓷块体材料在786.8℃时发生相变,当x=0.2, 0.3, 0.4时,随着Sm2O3稀土氧化物添加量的增加,其热膨胀系数逐渐增大;当x=0.2, 0.3, 0.4时,随着Nd2O3稀土氧化物添加量的增加,Nd_xZr_(1-x)O_(2-x/2)块体的热膨胀系数也逐渐增加。
ZrOCl_2·8H_2O and rare earth oxides of Ln_2O_3 (Ln=Nd, Sm) powders are used as starting materials to synthesize Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm) (x=0.1, 0.2, 0.3, 0.4) with a chemical coprecipitation followed by calcination method. The Ln_xZr_(1-x)O_(2-x/2) powders were first heat treated at 800℃for 5 hours, and were then sintered into Nd_xZr_(1-x)O_(2-x/2) and Sm_xZr_(1-x)O_(2-x/2) bulk materials by pressureless sintering process. The microstructure, thermal capacity, thermal expansion coefficient, thermal diffusivity and thermal conductivity of different bulk materials have been investigated by DSC, X-ray diffraction (XRD), scanning electron microscopy (SEM) and various thermal analysis techniques.
The Nd_xZr_(1-x)O_(2-x/2) and Sm_xZr_(1-x)O_(2-x/2) powders are synthesized with the chemical coprecipitation followed by calcination method. Ln0.1Zr0.9O1.95(Ln=Nd, Sm) powders consist of m and t phases,however, the Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm) (x=0.2, 0.3, 0.4) are composed of t and c phases. The Ln_xZr_(1-x)O_(2-x/2) powders exhibit a particle size of below 100nm. With the pressureless sintering process at a temperature of 1600℃for 15 hours, The Ln_xZr_(1-x)O_(2-x/2) ceramics consist mainly of m and t phase, while Ln_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramic are composed of t and c phase. However Ln0.4Zr0.6O1.8 ceramics are composed of pyrochlore phase. The LnxZr1-xO2-x/2 bulk materials with a grain size range of 4~5μm are fabricated.
From the results on the thermal capacity of sintered Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4), the phase transformation from monoclinic to tetragonal phase was identified for Sm0.1Zr0.9O1.95 ceramics at 768.8℃, however, no phase transformation is found in other Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramics. With the increase of the Sm2O3 addition, the thermal capacity of Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) decreases. While, the phase transformation from monoclinic to tetragonal phase was identified for Nd0.1Zr0.9O1.95 ceramics at 911.3℃, and no phase transformation is found in other Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramics. With the increase of the Nd2O3 addition, the thermal capacity of Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) also decreases.
The results on thermal conductivity indicate that, the thermal conductivity of Sm0.1Zr0.9O1.95 is smallest. The thermal conductivity of Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4), which is located in the range of 1.51 to 2.39W·m-1·K-1, decreases with the increase of the Sm2O3 addition. For the Nd_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4) ceramics, the thermal conductivity is in the range of 1.54 to 2.45W·m-1·K-1.
The results on thermal expansion coefficients indicate that, the identical phase transformation process takes place for Sm0.1Zr0.9O1.95 ceramics at 768.8℃. The thermal expansion coefficients of Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4) increase with the increase of the Sm2O3 addition. The same situation is found for the Nd_xZr_(1-x)O_(2-x/2) at x= 0.2, 0.3, 0.4.
采用化学共沉淀-煅烧法制备出Nd_xZr_(1-x)O_(2-x/2)和Sm_xZr_(1-x)O_(2-x/2)的粉体。当x=0.1时,Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm)由m相和t相构成,而当x=0.2,0.3,0.4时,Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm)由t相和c相构成。粉体颗粒比较均匀,晶粒尺寸在100nm以下。采用无压烧结方法,在1600℃下烧结15小时,制备出NdxZr1-xO2-x/2和Sm_xZr_(1-x)O_(2-x/2)的陶瓷块体材料,对Ln_xZr_(1-x)O_(2-x/2)块体的物相分析可知,在x=0.1时,主要含有t相,同时含有少量的m相,在x=0.2,0.3时,含有t相和c相,在x=0.4时,完全是烧绿石相,块体晶粒尺寸在4~5μm之间。
通过对Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的比热分析,可以看出Sm0.1Zr0.9O1.95在786.8℃时发生相变,而其它成分的Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4)块体材料没有发生t-m的相变。当x=0.2, 0.3, 0.4时,随着Sm2O3稀土氧化物添加量的增加,Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4)的陶瓷块体材料的比热逐渐减小;而从Nd_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的比热分析来看, Nd0.1Zr0.9O1.95块体在911.3℃时发生相变,而其它成分的Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4)块体材料也没有发生t-m的相变。当x=0.2, 0.3, 0.4时,随着Nd2O3稀土氧化物添加量的增加,其比热值逐渐减小。
从SmxZr1-xOx/2(x=0.1, 0.2, 0.3, 0.4)陶瓷块体材料的热导率分析结果可以看出,当x=0.1时其热导率最低,当x=0.2, 0.3, 0.4时,大小在1.51W·m-1·K-1到2.39W·m-1·K-1之间变化。随着Sm2O3稀土氧化物添加量的增加,其热导率逐渐减小;而从Nd_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4)陶瓷块体材料的热导率的分析结果可以看出,大小在1.54 W·m-1·K-1到2.45W·m-1·K-1之间变化。
从Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4)块体的热膨胀系数分析结果可以看出, Sm0.1Zr0.9O1.95陶瓷块体材料在786.8℃时发生相变,当x=0.2, 0.3, 0.4时,随着Sm2O3稀土氧化物添加量的增加,其热膨胀系数逐渐增大;当x=0.2, 0.3, 0.4时,随着Nd2O3稀土氧化物添加量的增加,Nd_xZr_(1-x)O_(2-x/2)块体的热膨胀系数也逐渐增加。
ZrOCl_2·8H_2O and rare earth oxides of Ln_2O_3 (Ln=Nd, Sm) powders are used as starting materials to synthesize Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm) (x=0.1, 0.2, 0.3, 0.4) with a chemical coprecipitation followed by calcination method. The Ln_xZr_(1-x)O_(2-x/2) powders were first heat treated at 800℃for 5 hours, and were then sintered into Nd_xZr_(1-x)O_(2-x/2) and Sm_xZr_(1-x)O_(2-x/2) bulk materials by pressureless sintering process. The microstructure, thermal capacity, thermal expansion coefficient, thermal diffusivity and thermal conductivity of different bulk materials have been investigated by DSC, X-ray diffraction (XRD), scanning electron microscopy (SEM) and various thermal analysis techniques.
The Nd_xZr_(1-x)O_(2-x/2) and Sm_xZr_(1-x)O_(2-x/2) powders are synthesized with the chemical coprecipitation followed by calcination method. Ln0.1Zr0.9O1.95(Ln=Nd, Sm) powders consist of m and t phases,however, the Ln_xZr_(1-x)O_(2-x/2)(Ln=Nd, Sm) (x=0.2, 0.3, 0.4) are composed of t and c phases. The Ln_xZr_(1-x)O_(2-x/2) powders exhibit a particle size of below 100nm. With the pressureless sintering process at a temperature of 1600℃for 15 hours, The Ln_xZr_(1-x)O_(2-x/2) ceramics consist mainly of m and t phase, while Ln_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramic are composed of t and c phase. However Ln0.4Zr0.6O1.8 ceramics are composed of pyrochlore phase. The LnxZr1-xO2-x/2 bulk materials with a grain size range of 4~5μm are fabricated.
From the results on the thermal capacity of sintered Sm_xZr_(1-x)O_(2-x/2)(x=0.1, 0.2, 0.3, 0.4), the phase transformation from monoclinic to tetragonal phase was identified for Sm0.1Zr0.9O1.95 ceramics at 768.8℃, however, no phase transformation is found in other Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramics. With the increase of the Sm2O3 addition, the thermal capacity of Sm_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) decreases. While, the phase transformation from monoclinic to tetragonal phase was identified for Nd0.1Zr0.9O1.95 ceramics at 911.3℃, and no phase transformation is found in other Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) ceramics. With the increase of the Nd2O3 addition, the thermal capacity of Nd_xZr_(1-x)O_(2-x/2) (x=0.2, 0.3, 0.4) also decreases.
The results on thermal conductivity indicate that, the thermal conductivity of Sm0.1Zr0.9O1.95 is smallest. The thermal conductivity of Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4), which is located in the range of 1.51 to 2.39W·m-1·K-1, decreases with the increase of the Sm2O3 addition. For the Nd_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4) ceramics, the thermal conductivity is in the range of 1.54 to 2.45W·m-1·K-1.
The results on thermal expansion coefficients indicate that, the identical phase transformation process takes place for Sm0.1Zr0.9O1.95 ceramics at 768.8℃. The thermal expansion coefficients of Sm_xZr_(1-x)O_(2-x/2)(x=0.2, 0.3, 0.4) increase with the increase of the Sm2O3 addition. The same situation is found for the Nd_xZr_(1-x)O_(2-x/2) at x= 0.2, 0.3, 0.4.
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