硅酸盐学报

酸度系数和烧结温度对微晶玻璃的析晶、微观形貌及性能的影响

PDF下载

吴孟吉 ¹^,² , 孙红娟 ¹^,² , 彭同江 ¹^,² , 尤皓 ¹^,² , 陈涛 ¹^,² , 李湘 ¹^,² , 陈仕泽 ¹^,²

硅酸盐学报 | 微晶玻璃专题—研究论文 2024,52(8): 2474-2485

收起

硅酸盐学报 |微晶玻璃专题—研究论文 2024 , 52 (8) : 2474 -2485

酸度系数和烧结温度对微晶玻璃的析晶、微观形貌及性能的影响

全屏

吴孟吉¹^,², 孙红娟¹^,², 彭同江¹^,², 尤皓¹^,², 陈涛¹^,², 李湘¹^,², 陈仕泽¹^,²

作者信息

^1．固体废物处理与资源化教育部重点实验室，四川绵阳 621010

^2．西南科技大学矿物材料及应用研究所，四川绵阳 621010

通讯作者:

孙红娟（1976—），女，博士，教授。

作者简介:

吴孟吉（1998—），男，硕士研究生。

Effect of Acidity Coefficient and Sintering Temperature on Crystallization, Microstructure and Properties of Glass-Ceramics

Mengji WU¹^,², Hongjuan SUN¹^,², Tongjiang PENG¹^,², Hao YOU¹^,², Tao CHEN¹^,², Xiang LI¹^,², Shize CHEN¹^,²

Affiliations

^1.Key Laboratory of Solid Waste Treatment and Resource Recycling, Ministry of Education, Mianyang 621010, Sichuan, China

^2.Institute of Mineral Materials and Applications, Southwest University of Science and Technology, Mianyang 621010, Sichuan, China

Corresponding Author:

SUN Hongjuan (1976-), female, Ph.D., Professor. E-mail: sunhongjuan@swust.edu.cn

WU Mengji (1998-), male, Master candidate. E-mail: 740193438@qq.com

出版时间: 2024-08-20 doi: 10.14062/j.issn.0454-5648.20240041

文章导航

摘要

收起

提钛渣制备微晶玻璃对于固体废物的无害化处理、释放大面积土地、减少天然原料的开采、改善环境污染具有重要意义。本工作以提钛渣和石英尾矿为原料，采用熔融烧结法制备高性能微晶玻璃。用差示扫描量热分析、X射线荧光光谱分析、X射线衍射分析及扫描电子显微镜等分析现代测试手段，结合性能测试，探究酸度系数（M_k）和烧结温度对制备的微晶玻璃的物相组成、微观形貌及物理和理化性能的影响。结果表明：改变M_k和烧结温度使结晶相的种类和数量发生明显变化。低M_k有利于透辉石的生长，而高M_k促进钙长石的形成。M_k增大有助于降低微晶玻璃的熔化温度并使其在较低的烧结温度下实现致密烧结。适当的M_k和烧结温度有助于基体中晶体生长和气孔排除，进而促进微晶玻璃烧结并提高其理化性能。然而，较大的M_k或较高的烧结温度导致微晶玻璃中玻璃相增加及气孔尺寸增大，破坏其致密的微观结构并呈过烧膨胀状态。当M_k为1.5、烧结温度为1 190 ℃时，所制备的微晶玻璃具有致密的微观结构与良好的理化性能，其吸水率为0.07%，体积密度为3.05 g/cm³，耐酸性为96.6%，抗折强度达144 MPa，各项性能均满足工业微晶玻璃的指标。

关键词

提钛渣 / 微晶玻璃 / 酸度系数 / 烧结温度

Abstract

收起

Introduction

Extracted Titanium slag is a type of industrial solid waste produced when titanium is recovered from titanium-containing blast furnace slag using the high-temperature carbonization-low-temperature selective chlorination method. Currently, it can only be disposed of through simple stockpiling and burial, which endangers both the environment and human health. The use of titanium slag to prepare microcrystalline glass with excellent physical and chemical properties is of great significance for the utilization of solid waste resources and the improvement of environmental pollution.

Raw material components and heat treatment systems have a significant impact on the microstructure and mechanical properties of glass ceramics. The current work is based on the chemical composition of titanium slag. high-performance glass-ceramics were prepared by melting sintering method by adding quartz tailings to increase SiO₂ content. Our study examines how the acidity coefficient (M_k) and sintering temperature affect the crystallization, microstructure, physical and chemical properties of microcrystalline glass. Additionally, we reveal the composition of the physical phase of glass ceramics made from titanium slag and the evolution of crystallization. These findings provide a technical foundation for the synergistic treatment of various solid wastes in the preparation of glass ceramics.

Methods

Titanium slag and quartz tailings were prepared, combined, ball milled, and sieved accordingly. The required raw materials were weighed exactly, put into a corundum crucible, heated untill the glass liquid melted and clarified. The liquid was then quickly dumped into water, to form glass particles, following a procedure of drying, ball milling, and sieving. The basic glass powder and PVA solution were uniformly mixed before being placed in a press-bar mold and pressed into blank samples, which were then sintered to produce glass ceramics sheet samples.

The chemical composition of the raw materials was evaluated using X-ray fluorescence spectrometry. A thermal analyzer was used to perform the DSC analysis simultaneously. An X-ray diffractometer was used to conduct physical phase analysis on raw materials and glass ceramics samples. The microstructure of the glass ceramics samples was observed using a scanning electron microscope (SEM), and their microscopic composition was analyzed using an energy dispersive-X-ray spectrometer (EDS).

According to the principle of Archimedes, the bulk density and water absorption of each glass-ceramic sample were measured. The bending strength of glass-ceramics was tested by GB/T4741—1999 three-point bending method. JC/T 2097—2011 industrial microcrystalline plate was used to test the acid etching amount of microcrystalline glass.

Results and discussion

The morphology investigation reveals that the samples' sintering or fusing steadily improves with an increase in M_k under the same temperature settings. At point of M_k=2.4, the sample begins to soften and distort, whereas at M_k =2.7, it looks to froth.

The XRD spectra of the glass ceramics samples demonstrate that the type and amount of the early crystalline phases vary when the Mand sintering temperature increases. Increasing the heat treatment temperature enhances the intensity of the diffraction peaks of the crystalline phases in low M_k glass ceramics samples. At the same sintering temperature, the content of anorthite in glass ceramics samples rises with increasing M_k, while the content of diopside increases in low M_k and decreases in high M_k.

The surface and cross-section micro-morphology of the glass ceramics samples demonstrates that the sintering temperature is too low and the materials do not attain the sintered state at lower temperature. With the same M_k, the number of holes in the samples decreases with increasing sintering temperature. As the sintering temperature rises, big closed holes become easier to develop.

The features of the glass ceramics samples, together with the results of XRD spectra and SEM analysis, show that Flexural strength and bulk density are mainly related to the type of crystalline phase, crystal content, and appropriately increase the sintering temperature. M_k is conducive to the growth of tremolite and calcium feldspar crystals in the billet, and it also benefits exclusion of porosity, so that the glass ceramics can form a flatter surface, and show higher mechanical-strength, thus to improve the sample's densification, flexural strength, acid resistance, and reduce water absorption as well. At higher acidity coefficients, increasing the SiO₂ content in the base glass causes an increase of the liquid phase, which is beneficial for filling pores, reducing the water absorption capacity of glass ceramics, and improving corrosion resistance under acidic conditions.

Conclusions

With the increase of M_k and sintering temperature, the type and quantity of crystalline phases of glass ceramics samples will undergo high-temperature physical phase reconstruction. Within a certain temperature range, the increase of sintering temperature can promote the growth of crystals in glass ceramics and the intensity of the diffraction peaks of crystalline phases. However, there exists a moderate temperature, above which the transformation of the crystalline phase shows different behavior, that is, low M_k favors the growth of diopside in glass ceramics, while high M_k promotes the formation of anorthite. When the M_k and the sintering temperature are both low, the glass ceramics samples are not completely sintered. This conditions for crystal growth and exclusion of pores are not sufficient. When the M_k and the sintering temperature increase simultaneously, the liquid phase appears in the matrix, which benefits the growth procedure of crystals to form a fixed crystal skeleton. When the sintering temperature is too high or the M_k is too high, the glass matrix begins to melt, and the phenomenon of overcooking occurs, which leads to an increase in the glassy phase and the expansion of pores, resulting in a strong and solid crystal skeleton. The expansion of pores makes the disjointed circular pores in the glass ceramics samples gradually increase. At M_k =1.5 and sintering temperature of 1 190 ℃, the produced material shows a water absorption rate of 0.07%, bulk density of 3.05 g/cm³, acid resistance of 96.6%, flexural strength of 144 MPa, which fully meet the requirements of industrial glass ceramics panels.

Key words

titanium slag extraction / glass-ceramics / acidity coefficient / sintering temperature

引用本文

吴孟吉, 孙红娟, 彭同江, 尤皓, 陈涛, 李湘, 陈仕泽. 酸度系数和烧结温度对微晶玻璃的析晶、微观形貌及性能的影响. 硅酸盐学报, 2024 , 52 (8) : 2474 -2485 . DOI: 10.14062/j.issn.0454-5648.20240041

Mengji WU, Hongjuan SUN, Tongjiang PENG, Hao YOU, Tao CHEN, Xiang LI, Shize CHEN. Effect of Acidity Coefficient and Sintering Temperature on Crystallization, Microstructure and Properties of Glass-Ceramics[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (8) : 2474 -2485 . DOI: 10.14062/j.issn.0454-5648.20240041

基金

收起

四川省知识产权局知识产权专项(2022-ZS-00031)
西南科技大学研究生创新基金(24ycx1132)

参考文献

收起

文献

收起

参考文献引证文献

排序方式：

2024年第52卷第8期

PDF下载

引用本文

BibTeX

文章信息

doi: 10.14062/j.issn.0454-5648.20240041

接收时间：2024-01-17
首发时间：2026-10-22
出版时间：2024-08-20

补充材料

相关文章

文章信息

作者

出版历史

收稿日期：2024-01-17
修回日期：2024-02-10

基金

四川省知识产权局知识产权专项(2022-ZS-00031)

西南科技大学研究生创新基金(24ycx1132)

作者信息

^1．固体废物处理与资源化教育部重点实验室，四川绵阳 621010

^2．西南科技大学矿物材料及应用研究所，四川绵阳 621010

通讯作者:

孙红娟（1976—），女，博士，教授。

参考文献

分享链接

https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240041

分享至

全文二维码

扫描看全文

引用本文

BibTeX

本文的引用情况

2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

关闭全屏

BibTeX
EndNote
RefWorks
TxT