一步法热处理温度对透明Li2O-Al2O3-B2O3-La2O3系微晶玻璃结构与性能的影响

doi:10.16552/j.cnki.issn1001-1625.2025.0612

硅酸盐通报 ›› 2026, Vol. 45 ›› Issue (1): 288-298.DOI: 10.16552/j.cnki.issn1001-1625.2025.0612

一步法热处理温度对透明Li₂O-Al₂O₃-B₂O₃-La₂O₃系微晶玻璃结构与性能的影响

胡思佳¹^,²(), 谢海磊³, 周坤¹^,², 多树旺¹^,², 施江¹^,²()

1.江西科技师范大学材料表面工程江西省重点实验室，南昌 330000
2.江西科技师范大学材料与能源学院，南昌 330000
3.江西万年晶半导体有限公司，上饶 334000

收稿日期:2025-06-23 修订日期:2025-08-25 出版日期:2026-01-20 发布日期:2026-02-10
通信作者: 施江，博士，讲师。E-mail：whutsj@126.com
作者简介:胡思佳（2001—），女，硕士研究生。主要从事微晶玻璃方面的研究。E-mail：Pumpkinhu@126.com
基金资助:
江西省自然科学基金(20242BAB20170);材料表面工程江西省重点实验室(2024SSY05071)

Effect of Single-Step Heat Treatment Temperature on Structure and Properties of Transparent Li₂O-Al₂O₃-B₂O₃-La₂O₃ Glass-Ceramics

HU Sijia¹^,²(), XIE Hailei³, ZHOU Kun¹^,², DUO Shuwang¹^,², SHI Jiang¹^,²()

1. Jiangxi Provincial Key Laboratory of Materials Surface Engineering，Jiangxi Science and Technology Normal University，Nanchang 330000，China
2. School of Materials and Energy，Jiangxi Science and Technology Normal University，Nanchang 330000，China
3. Jiangxi Wannian Crystal Semiconductor Co. ，Ltd. ，Shangrao 334000，China

Received:2025-06-23 Revised:2025-08-25 Published:2026-01-20 Online:2026-02-10

摘要/Abstract

摘要：

不含SiO₂的新型硼铝酸盐玻璃具备优异的抗开裂能力，在玻璃盖板领域具有应用潜力。本文采用高温熔融浇注法成功制备了含La₂O₃的硼铝酸盐微晶玻璃，并系统研究了一步热处理温度对结构与性能的影响。结果表明：随着热处理温度由585 ℃升高至630 ℃，玻璃网络中的［BO₃］逐渐向［BO₄］四面体配位转化，LiAl₇B₄O₁₇与Li₂AlB₅O₁₀晶相开始析出且含量增加；晶粒尺寸增大，形貌从颗粒状发展为颗粒-短棒共存状态，结晶度显著提升，从49.6%增至88.9%，550 nm可见光透过率从87.28%降至57.75%。随着热处理温度的提高，维氏硬度逐渐增加，在600 ℃热处理条件下样品表现出最佳综合性能，维氏硬度达到6.24 GPa，断裂韧性为1.12 MPa·m^1/2，可见光透过率为87.28%，抗开裂能力为19.1 N。这表明通过优化热处理温度可以实现高硬度、高透光性与耐损伤性的协同提升，为高性能透明微晶玻璃盖板材料的设计提供了新的途径。

关键词: 硼铝酸盐玻璃, 微晶玻璃, 热处理, 透过率, 耐损伤

Abstract:

A novel SiO₂-free aluminoborate glass demonstrates outstanding cracking resistance and shows considerable potential for application as cover glass. In this work， La₂O₃-containing aluminoborate glass-ceramics were successfully fabricated via high-temperature melt-casting method. The effect of one-step heat treatment temperature on the structural and functional was systematically investigated. The results reveal that increasing the heat treatment temperature from 585 ℃ to 630 ℃，［BO₃］ units in the glass network gradually convert into ［BO₄］ tetrahedral coordination. Simultaneously， LiAl₇B₄O₁₇ and Li₂AlB₅O₁₀ crystalline phases precipitate in progressively greater quantities. Grain size increases， and morphology evolves from a purely granular particles form to a microstructure where granular particles and short-rod crystals coexist. The crystallinity degree rises markedly from 49.6% to 88.9%， accompanied by a reduction in visible light transmittance from 87.28% to 57.75%. With increasing heat treatment temperature， Vickers hardness continuously increases. Under 600 ℃ heat treatment condition the specimen exhibits optimum comprehensive properties， achieving a Vickers hardness of 6.24 GPa， a fracture toughness of 1.12 MPa·m^1/2， a visible light transmittance of 87.28%， and a cracking resistance of 19.1 N. These findings demonstrate that optimizing the heat treatment temperature enables a synergistic enhancement of hardness， transparency， and damage resistance. This study offers a novel pathway for designing high-performance， transparent glass-ceramics cover glass materials.

Key words: aluminoborate glass, glass-ceramics, heat treatment, transmittance, damage resistance

中图分类号:

TQ171.1

胡思佳, 谢海磊, 周坤, 多树旺, 施江. 一步法热处理温度对透明Li₂O-Al₂O₃-B₂O₃-La₂O₃系微晶玻璃结构与性能的影响[J]. 硅酸盐通报, 2026, 45(1): 288-298.

HU Sijia, XIE Hailei, ZHOU Kun, DUO Shuwang, SHI Jiang. Effect of Single-Step Heat Treatment Temperature on Structure and Properties of Transparent Li₂O-Al₂O₃-B₂O₃-La₂O₃ Glass-Ceramics[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2026, 45(1): 288-298.

图/表 15

表1 原料及生产厂家

Table 1 Raw materials and manufacturers

原料	纯度	生产厂家
Li₂CO₃	分析纯 AR	国药集团化学试剂有限公司
Al₂O₃	分析纯 AR	国药集团化学试剂有限公司
B₂O₃	分析纯 AR	国药集团化学试剂有限公司
TiO₂	化学纯 CP	国药集团化学试剂有限公司
NH₄H₂PO₄	分析纯 AR	西陇科学股份有限公司
CaCO₃	分析纯 AR	国药集团化学试剂有限公司
La₂O₃	分析纯 AR	国药集团化学试剂有限公司

表2 玻璃样品热处理制度

Table 2 Heat treatment regime for glass samples

Sample	L-585	L-600	L-615	L-630
Crystallization temperature/℃	585	600	615	630
Insulation time/h	2	2	2	2

图1 基础玻璃的DSC曲线

Fig.1 DSC curve of parent glass

图2 不同热处理温度下微晶玻璃的XRD谱

Fig.2 XRD patterns of glass-ceramics at different heat treatment temperatures

表3 不同热处理温度下微晶玻璃的结晶度及晶相含量

Table 3 Crystallinity and crystal phase content of glass-ceramics at different heat treatment temperatures

Sample	L-600	L-615	L-630
Crystallinity degree/%	49.6	65.2	88.9
LiAl₇B₄O₁₇ content/%	43.2	54.4	64.3
Li₂AlB₅O₁₀ content/%	6.4	10.8	24.6

图3 不同热处理温度下微晶玻璃的SEM照片

Fig.3 SEM images of glass-ceramics at different heat treatment temperatures

图4 不同热处理温度下微晶玻璃的FTIR光谱

Fig.4 FTIR spectra of glass-ceramics at different heat treatment temperatures

图5 不同热处理温度下微晶玻璃的可见光透过率

Fig.5 Visible light transmittance of glass-ceramics at different heat treatment temperatures

表4 不同热处理温度下微晶玻璃样品在550 nm波长下的可见光透过率

Table 4 Visible light transmittance of glass-ceramics at 550 nm wavelength at different heat treatment temperatures

Sample	L-20	L-585	L-600	L-615	L-630
Transmittance/%	89.19	89.94	87.28	85.85	57.75

图6 不同热处理温度下微晶玻璃的体积密度

Fig.6 Bulk density of glass-ceramics at different heat treatment temperatures

图7 不同热处理温度下微晶玻璃的维氏硬度与断裂韧性

Fig.7 HV and fracture toughness of glass-ceramics at different heat treatment temperatures

图8 不同热处理温度下微晶玻璃的开裂概率曲线和CR测量值

Fig.8 Cracking probability curves and CR measurement value of glass-ceramics at different heatment temperatures

图9 不同热处理温度下微晶玻璃的划痕测试结果

Fig.9 Scratch test results of glass-ceramics at different heat treatment temperatures

图10 不同热处理温度下微晶玻璃的划痕统计结果

Fig.10 Scratch statistical analysis of glass-ceramics

图11 微晶玻璃的性能比较

Fig.11 Comparison of properties of glass-ceramics at different heat treatment temperatures

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一步法热处理温度对透明Li₂O-Al₂O₃-B₂O₃-La₂O₃系微晶玻璃结构与性能的影响

Effect of Single-Step Heat Treatment Temperature on Structure and Properties of Transparent Li₂O-Al₂O₃-B₂O₃-La₂O₃ Glass-Ceramics

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