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材料研究学报  2020, Vol. 34 Issue (5): 368-378    DOI: 10.11901/1005.3093.2019.472
  研究论文 本期目录 | 过刊浏览 |
白云鄂博尾矿含量对微晶玻璃析晶特性和性能的影响
宋雪, 李亚凡, 任杰, 钟曜宇, 张红霞(), 欧阳顺利
内蒙古科技大学理学院 包头 014010
Effect of Bayan-Obo Tailings Content on Crystallization Characteristics and Properties of Glass-ceramics
SONG Xue, LI Yafan, REN Jie, ZHONG Yaoyu, ZHANG Hongxia(), OUYANG Shunli
School of Science, Inner Mongolia University of Science & Technology, Baotou 014010,China
引用本文:

宋雪, 李亚凡, 任杰, 钟曜宇, 张红霞, 欧阳顺利. 白云鄂博尾矿含量对微晶玻璃析晶特性和性能的影响[J]. 材料研究学报, 2020, 34(5): 368-378.
Xue SONG, Yafan LI, Jie REN, Yaoyu ZHONG, Hongxia ZHANG, Shunli OUYANG. Effect of Bayan-Obo Tailings Content on Crystallization Characteristics and Properties of Glass-ceramics[J]. Chinese Journal of Materials Research, 2020, 34(5): 368-378.

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摘要: 

以白云鄂博某尾矿为主要原料、以Cr2O3为晶核剂制备尾矿微晶玻璃,使用DSC、XRD、SEM、TEM以及Raman光谱等手段对其表征并测试其析晶特性、抗折强度、维氏硬度和耐酸性,研究了尾矿含量对其析晶特性和性能的影响。结果表明,微晶玻璃的主晶相由辉石相和钙铝黄长石相构成,其中晶核剂Cr2O3因形成尖晶石晶核诱导辉石相析出。随着尾矿含量的提高微晶玻璃的力学和耐腐蚀特性呈现降低的趋势。其原因是,尾矿含量的提高使CaO的含量过高,在晶体的生长过程中滑动和迁移受阻进而在微晶玻璃中产生空洞和缺陷。同时,微晶玻璃中钙铝黄长石相/辉石相比例增大也不利于其性能的提高。白云鄂博尾矿中共生的稀土元素在晶界处形成铈钙硅石第二相,可减小晶界面积并降低晶界总能量,有助于提高微晶玻璃的力学和耐腐蚀性能。

关键词 无机非金属材料白云鄂博尾矿微晶玻璃析晶特性Cr2O3稀土    
Abstract

Metallic tailings built glass-ceramics were prepared with Bayan-Obo tailings as the main raw material and Cr2O3 as nucleating agent. The crystallization characteristics of tailings built glass-ceramics were characterized by means of DSC, XRD, SEM and Raman spectra and the properties of glass-ceramics were evaluated by bending strength, Vickers hardness and acid resistance tests. Results show that the glass-ceramics are mainly composed of crystalline phases of diopside and gehlenite, while the nucleating agent of Cr2O3 can promote the precipitation of the main crystalline phase of diopside by forming spinel. The mechanical and corrosion resistance characteristics of glass-ceramics showed a decreasing trend with the increase of tailings content. The higher CaO content caused by the increase of tailings content can lead to the obstruction of sliding and migration of crystalline phases in the crystal growth process. As a result, it was easy to produce cavities and defects in glass-ceramics. Meanwhile, the increase of the ratio of gehlenite/diopside was not conducive to the improvement of the properties of the glass-ceramics. In addition, the rare earth elements intergrowth in Bayan-Obo tailings can form the second phase of cerium calcium silica at the grain boundary, which can reduce the area and the total energy of grain boundaries, which was helpful to improve the mechanical and corrosion resistance of glass-ceramics.

Key wordsinorganic non-metallic materials    Bayan-Obo tailings    glass-ceramics    crystallization characteristics    Cr2O3    rare earth
收稿日期: 2019-10-11     
ZTFLH:  TQ171  
基金资助:内蒙古自治区级大学生创新创业训练计划(201910127011);内蒙古自治区教育厅项目(NJZY18143);内蒙古自然科学基金(2017MS0507);内蒙古自治区重大基础研究开放课题(0406091701)
作者简介: 宋雪,女,1997年生,本科生
CompositionSiO2CaOMgOAl2O3K2ONa2OTFeTiO2MnOREO
Content36.536.79.512.10.40.70.50.30.72.6
表1  白云鄂博尾矿的化学成分
No.Mine tailingSiO2MgONa2CO3Cr2O3

BFS75

BFS80

BFS85

75

80

85

16

13

10

4.1

2.1

0.1

3.1

3.1

3.1

1.8

1.8

1.8

表2  尾矿微晶玻璃原料配方
No.SiO2CaOMgOAl2O3Na2OK2OMnOTFeCr2O3REOTiO2
BFS7543.427.511.29.13.620.30.520.381.81.950.23
BFS8042.229.29.79.73.780.320.560.41.82.10.24
BFS8541.131.18.110.33.80.340.60.411.82.20.25
表3  尾矿微晶玻璃化学组成
图1  不同尾矿含量微晶玻璃的DSC曲线
SampleTg/℃Tp/℃?T/℃

BFS75

BFS80

BFS85

721.7

723.3

727.5

939.5

912.2

904.5

217.8

188.9

177

表4  玻璃试样的特征温度
图2  不同尾矿含量微晶玻璃的XRD谱
图3  不同尾矿含量微晶玻璃的SEM照片
图4  试样BFS75的EDS能谱面扫描图
图5  试样BFS75的EDS能谱点扫描图
图6  试样BFS80的EDS能谱面扫描图
图7  试样BFS85的EDS能谱面扫描图
图8  不同尾矿含量微晶玻璃的Raman谱
SampleBFS75BFS80BFS85
Density/g·cm-33.03±0.032.97±0.022.68±0.05
Hardness/GPa6.67±0.026.43±0.036.04±0.04

Acid-resistance/%

Bending strength/MPa

93±7

145±5

87±8

106±7

69±6

87±5

表5  不同尾矿含量微晶玻璃的性能
图9  用HF酸腐蚀后试样BFS75的EDS能谱面扫描图
图10  粉末试样BFS75的TEM照片、Ce元素面扫描和点扫描分析
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