采用高温熔融法制备了不同成核剂Fe_2O_3及ZrO_2含量的SiO_2-Al_2O_3-MgO-F系玻璃试样,用差示扫描量热仪、X射线衍射仪以及扫描电子显微镜研究了成核剂对此微晶玻璃析晶特征的影响.结果表明:在所研究的微晶玻璃中,随着ZrO_2含量增加,玻璃转变温度和析晶温度略有提高.当玻璃中ZrO_2含量超过5.0%(质量分数,下同)时,玻璃转变温度有较大提高,而析晶温度却大大降低.同时添加ZrO_2和Fe_2O_3提高了玻璃转变温度,并且在850～900 ℃及925～960 ℃出现了2个析晶放热区间.对应第1个析晶温度区间,堇青石晶体在玻璃基体中均匀析出,析出晶体为枝状,最终形成多边星形.第2个放热区间温度对应云母晶体的析出,析出晶体呈片层状,在星形晶体间析出.随着玻璃中Fe_2O_3含量的增加,玻璃转变温度和放热峰温度都逐渐提高,而且2个放热峰温度的间隔程度增加.同时也发现ZrO_2和Fe_2O_3的加入都抑制了云母晶体的析出.
The glass samples with various contents of Fe_2O_3 and ZrO_2 as nucleating agents were prepared by melt-quenching methods in the SiO_2-Al_2O_3-MgO-F system and the crystallizing behaviors were investigated using differential scanning calorimeter, X-ray diffraction and scanning electron microscopy techniques. The results indicate that both the transition temperature (Tg) and the crystallizing temperature have a bit rise with the increase of ZrO_2 contents in the glass system studied. In the sample with more than 5.0wt% ZrO_2 additive, an obvious increases of Tg, but a great decreases of crystallizing temperature are observed. The additions of a pair of Fe_2O_3 and ZrO_2 increase the Tg and induce two exothermal peaks occurred at 850～900℃ and 925～960℃. The dendritic phases of cordierite, which are crystallized at the first exothermal peaks temperature, are homogeneously precipitated in the residual glass and formed the star-shape crystals eventually. The second exothermal peaks are corresponded to the crystallization of mica phases, which are precipitated of interdendritic cordierite phases and formed the plate shapes. With the increases of Fe_2O_3 contents, the Tg and crystallization temperature are both increased and the gap between the two exothermal peaks is broadened. Also, it is found that the incorporation of Fe_2O_3 or ZrO_2 suppresses the crystallization of mica crystal.
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