热处理时间对透辉石系尾矿微晶玻璃析晶及其性能的影响

doi:10.11901/1005.3093.2019.426

材料研究学报

2020, Vol. 34

Issue (3): 209-216 DOI: 10.11901/1005.3093.2019.426

研究论文

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热处理时间对透辉石系尾矿微晶玻璃析晶及其性能的影响

李红霞(

),李保卫,徐鹏飞,刘中兴

内蒙古科技大学材料与冶金学院包头 014010

Influences of Heat Treatment Soaking Time on Crystallization and Properties of Tailings-based Glass-Ceramics

LI Hongxia(

),LI Baowei,XU Pengfei,LIU Zhongxing

Materials and Metallurgy School，Inner Mongolia University of Science and Technology，Baotou 014010，China

引用本文:

李红霞,李保卫,徐鹏飞,刘中兴. 热处理时间对透辉石系尾矿微晶玻璃析晶及其性能的影响[J]. 材料研究学报, 2020, 34(3): 209-216.
Hongxia LI, Baowei LI, Pengfei XU, Zhongxing LIU. Influences of Heat Treatment Soaking Time on Crystallization and Properties of Tailings-based Glass-Ceramics[J]. Chinese Journal of Materials Research, 2020, 34(3): 209-216.

全文: PDF(6377 KB) HTML

摘要:

使用金尾矿和铁尾矿为主要原料，采用熔融法和一步法析晶热处理制备了透辉石系尾矿微晶玻璃。将其分别在低温段720℃和高温段820℃保温，使用DSC、XRD、Raman光谱、SEM和综合力学性能仪等手段研究了保温时间对透辉石系尾矿微晶玻璃析晶过程及性能的影响。结果表明：该系微晶玻璃的主晶相为单斜结构的透辉石晶体(Mg_0.6Fe_0.2Al_0.2)Ca(Si_1.5A_l0.5)O₆(JCPDS 72-1379)，晶体的生长过程包括玻璃的分相、成核和晶体生长过程。热处理温度为低温段720℃时透辉石晶体的成核温度为720℃，随着保温时间的延长透辉石晶体逐渐长大且由球状晶向枝状晶演变，透灰石晶体的析出量逐渐增加；热处理温度为高温段820℃时透辉石晶体的形貌均为尺寸较大的枝状晶，但是随着保温时间的延长透辉石晶体的形貌和尺寸变化不大。综合性能最优的热处理制度为在820℃保温45 min，制备出的微晶玻璃密度为2.97 g/cm³，抗折强度为211.0 MPa，硬度为789.0 MPa，耐酸性99.3%，耐碱性99.1%。

关键词 ：无极非金属材料, 尾矿微晶玻璃, 保温时间, 透辉石, 晶体生长

Abstract：

Diopside tailings-based glass-ceramics were prepared via melting method plus one-step crystallization heat treatment with Shandong gold tailings and Guyang iron tailings as the main raw material. Then the influence of heat treatment soaking time on the crystal growth and properties of the prepared glass-ceramics was investigated by DSC, XRD, Raman spectroscopy, SEM, and universal mechanical properties tester. The results show that diopside crystals can grow through nucleation and whereafter growth when heat treated at 720℃ for 30 min. With the increase of heat treatment time, the size of diopside crystals gradually increased and the morphology of the crystals evolved from spherical to dendritic. When the heat treatment temperature was 820℃, the morphology and structure of the diopside crystals did not change with the increase of soaking time. Thus, heat treatment at 820℃ for 2 h can be considered to be the optimal. The prepared glass ceramics exhibit an excellent comprehensive performance with density of 2.97 g/cm³, bending strength of 211.0 MPa, hardness of 789.0 MPa, acid resistance of 99.4% and alkali resistance of 99.3 % respectively.

Key words： inorganic non-metallic materials tailing-based glass-ceramic soaking time diopside crystal growth

收稿日期: 2019-08-31

ZTFLH:

TQ174

基金资助:国家自然科学基金(51964039);内蒙古自然科学基金(2019MS05050);内蒙古自治区高等学校科学研究项目(NJZZ18141)

作者简介: 李红霞，女，1983年生，博士

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https://www.cjmr.org/CN/10.11901/1005.3093.2019.426 或 https://www.cjmr.org/CN/Y2020/V34/I3/209

表1 金尾矿和铁尾矿的主要化学组成

图1 实验用铁尾矿和金尾矿的XRD图谱

表2 基础玻璃的组成

图2 基础玻璃的DSC曲线

表3 微晶玻璃样品热处理工艺参数表

图3 用传统法在720℃保温不同时间制备的微晶玻璃的SEM照片

图4 用传统法在820℃保温不同时间制备的微晶玻璃的SEM照片

图5 在720℃保温不同时间制备的微晶玻璃的XRD图谱

图6 在820℃保温不同时间制备的微晶玻璃的XRD图谱

图7 在720℃热处理1 h的 (C60HD)样品的透射电子显微照片

图8 在720℃热处理不同时间制备的微晶玻璃的拉曼光谱

图9 在820℃热处理不同时间制备的微晶玻璃的拉曼光谱

表4 尾矿微晶玻璃的拉曼谱带归属表

表5 热处理保温不同时间制备的微晶玻璃的理化性能

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