多孔轻质莫来石陶瓷制备及性能的研究
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摘要
本文以Al_2O_3-SiO_2体系为粘结剂,空心球作为造孔剂,利用凝胶注模成型方法制备出一种新型的多孔莫来石材料。空心球在烧结过程中可以起到烧结助剂的作用,大大的降低了Al_2O_3-SiO_2体系的烧结温度。
实验分别研究添加百分比为25%、50%、75%、100%的空心球进行研究,结果表明空心球含量越多,总气孔率越大;其中烧成温度较低的是75%空心球添加量,其在1200℃能烧成轻质多孔莫来石陶瓷。XRD分析表明温度的增加,莫来石衍射峰增强,Al_2O_3的衍射峰降低,说明温度升高促进了Al_2O_3-SiO_2烧成莫来石相。随着空心球含量减少,Al_2O_3-SiO_2粉末含量相对增加,其烧结温度增加,抗弯强度增大。50%空心球1300℃下制备的多孔陶瓷密度在1.09 g/cm~3左右,抗弯强度为15 MPa。25%空心球添加量在1400℃烧结得到的多孔陶瓷强度达到38 MPa,密度1.43 g/cm~3,孔径结构多为闭气孔,闭气孔率为35%。
在上述基础上,实验选取50%的空心球作第一类造孔剂,另外添加B_2O_3和CaCO3作为第二类造孔剂进行研究。实验表明,当添加B_2O_3含量较少时(2.5%左右),气孔率降低,B_2O_3能够促进烧结。B_2O_3的含量从2.5%开始增加到10%,陶瓷的收缩率反常的降低,总气孔率越来越大。SEM分析其原因为CaCO3和B_2O_3在有水浆料中反应产生CO_2气泡,从而使坯体产生微孔,另一原因为B_2O_3的加入加速孔壁中氧化物液化,使孔中露出凹凸不平的针状莫来石,从而提高气孔率。B_2O_3的加入促进Al_2O_3-SiO_2在低温下烧成莫来石相,烧结温度降低了100~200℃左右。10% B_2O_3添加量在1200℃烧结后,气孔率增加到81%,密度降低到0.64 g/cm~3。
从热学上来分析,本实验所制备的多孔莫来石陶瓷具有较低的导热系数(0.09-0.30 W.(m.k)~(-1))。而且材料的导热存在一定的弛豫时间,导热系数越小,弛豫时间越长,说明这种多孔材料具有良好的隔热性能。
In this paper, a novel porous mullite was fabricated by means of gelcasting method using Al_2O_3-SiO_2 and fly ash cenosphere as basic materials, as well as binder and foaming a gent. The main crystalline phases of fly ash cenosphere are mullite and SiO_2 besides a small amount of amorphous glassy phase. The amorphous glassy phase during sintering can play the role of sintering aids; greatly lower the sintering temperature of Al_2O_3-SiO_2 system. Experiment studied the effect of adding 25%, 50%, 75%, 100% amount of cenospheres. The results showed that the more content of cenospheres, the lower sintering temperature, and the higher the total porosity it was. More than 75% cenospheres adding, light porous mullite ceramics can be sintered at as low as 1200℃. From XRD (X-Ray Diffraction) patterns we knew as the sintering temperature increased, mullite diffraction peaks intensified, and Al_2O_3 diffraction peaks shrinked, indicating that high temperature promotes the growth of mullite crystals. SEM images showed that after 1200℃sintering, the re was glassy phase starting to liquify to accelerate sintering. When the amount of cenospheres decreased, the sintering temperature and flexural strength would obviously increase. And with 50% cenospheres addition, flexural strength and bulk density of porous mullite respectively resulted in 15MPa and 1.09 g/cm~3 at 1300℃. The maximum flexural strength reaches 38 MPa with 25% cenospheres in it, which also has a highest closed porosity (35%) and bulk density (1.43 g/cm~3).
A small amount of CaCO3 and B_2O_3 are added as sintering aid, as well as second foaming agent, which based on formula of 50% cenospheres. As a result, when adding less than 2.5% amount of B_2O_3, B_2O_3 can promote sintering, but decrease the porosity. The amount of B_2O_3 added from 2.5% to 10%, both of bulk shrinkage and density would decline abnormally because of the second foaming agent. On the other hand, B_2O_3 would eutecticevaporate with other oxides in pore shell, so that needle-like mullite presented in the inner pore. That is why more B_2O_3 resulted in higher porosity. When B_2O_3 added to 10% wt, a higher total porosity rate is up to 81%, and lower density is down to 0.64 g/cm~3.
The light porous mullite ceramics was prepared in this experiment with low thermal conductivity (0.09~0.30 W.(m.k)~(-1)). And thermal conductivity was characterized by a relaxation time. The lower the thermal conductivity, the longer relaxation time it is, indicating that the porous material with good heat insulation properties.
实验分别研究添加百分比为25%、50%、75%、100%的空心球进行研究,结果表明空心球含量越多,总气孔率越大;其中烧成温度较低的是75%空心球添加量,其在1200℃能烧成轻质多孔莫来石陶瓷。XRD分析表明温度的增加,莫来石衍射峰增强,Al_2O_3的衍射峰降低,说明温度升高促进了Al_2O_3-SiO_2烧成莫来石相。随着空心球含量减少,Al_2O_3-SiO_2粉末含量相对增加,其烧结温度增加,抗弯强度增大。50%空心球1300℃下制备的多孔陶瓷密度在1.09 g/cm~3左右,抗弯强度为15 MPa。25%空心球添加量在1400℃烧结得到的多孔陶瓷强度达到38 MPa,密度1.43 g/cm~3,孔径结构多为闭气孔,闭气孔率为35%。
在上述基础上,实验选取50%的空心球作第一类造孔剂,另外添加B_2O_3和CaCO3作为第二类造孔剂进行研究。实验表明,当添加B_2O_3含量较少时(2.5%左右),气孔率降低,B_2O_3能够促进烧结。B_2O_3的含量从2.5%开始增加到10%,陶瓷的收缩率反常的降低,总气孔率越来越大。SEM分析其原因为CaCO3和B_2O_3在有水浆料中反应产生CO_2气泡,从而使坯体产生微孔,另一原因为B_2O_3的加入加速孔壁中氧化物液化,使孔中露出凹凸不平的针状莫来石,从而提高气孔率。B_2O_3的加入促进Al_2O_3-SiO_2在低温下烧成莫来石相,烧结温度降低了100~200℃左右。10% B_2O_3添加量在1200℃烧结后,气孔率增加到81%,密度降低到0.64 g/cm~3。
从热学上来分析,本实验所制备的多孔莫来石陶瓷具有较低的导热系数(0.09-0.30 W.(m.k)~(-1))。而且材料的导热存在一定的弛豫时间,导热系数越小,弛豫时间越长,说明这种多孔材料具有良好的隔热性能。
In this paper, a novel porous mullite was fabricated by means of gelcasting method using Al_2O_3-SiO_2 and fly ash cenosphere as basic materials, as well as binder and foaming a gent. The main crystalline phases of fly ash cenosphere are mullite and SiO_2 besides a small amount of amorphous glassy phase. The amorphous glassy phase during sintering can play the role of sintering aids; greatly lower the sintering temperature of Al_2O_3-SiO_2 system. Experiment studied the effect of adding 25%, 50%, 75%, 100% amount of cenospheres. The results showed that the more content of cenospheres, the lower sintering temperature, and the higher the total porosity it was. More than 75% cenospheres adding, light porous mullite ceramics can be sintered at as low as 1200℃. From XRD (X-Ray Diffraction) patterns we knew as the sintering temperature increased, mullite diffraction peaks intensified, and Al_2O_3 diffraction peaks shrinked, indicating that high temperature promotes the growth of mullite crystals. SEM images showed that after 1200℃sintering, the re was glassy phase starting to liquify to accelerate sintering. When the amount of cenospheres decreased, the sintering temperature and flexural strength would obviously increase. And with 50% cenospheres addition, flexural strength and bulk density of porous mullite respectively resulted in 15MPa and 1.09 g/cm~3 at 1300℃. The maximum flexural strength reaches 38 MPa with 25% cenospheres in it, which also has a highest closed porosity (35%) and bulk density (1.43 g/cm~3).
A small amount of CaCO3 and B_2O_3 are added as sintering aid, as well as second foaming agent, which based on formula of 50% cenospheres. As a result, when adding less than 2.5% amount of B_2O_3, B_2O_3 can promote sintering, but decrease the porosity. The amount of B_2O_3 added from 2.5% to 10%, both of bulk shrinkage and density would decline abnormally because of the second foaming agent. On the other hand, B_2O_3 would eutecticevaporate with other oxides in pore shell, so that needle-like mullite presented in the inner pore. That is why more B_2O_3 resulted in higher porosity. When B_2O_3 added to 10% wt, a higher total porosity rate is up to 81%, and lower density is down to 0.64 g/cm~3.
The light porous mullite ceramics was prepared in this experiment with low thermal conductivity (0.09~0.30 W.(m.k)~(-1)). And thermal conductivity was characterized by a relaxation time. The lower the thermal conductivity, the longer relaxation time it is, indicating that the porous material with good heat insulation properties.
引文
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