无机材料学报 ›› 2024, Vol. 39 ›› Issue (5): 531-538.DOI: 10.15541/jim20230587
吕朝阳1,2(), 徐勇1,2, 杨久延1,2, 涂广升1,2, 涂兵田1,2, 王皓1,2()
收稿日期:
2023-12-21
修回日期:
2024-01-20
出版日期:
2024-05-20
网络出版日期:
2024-02-22
通讯作者:
王 皓, 教授. E-mail: shswangh@whut.edu.cn作者简介:
吕朝阳(1999-), 男, 硕士研究生. E-mail: lvzhaoyang2021@163.com
基金资助:
LÜ Zhaoyang1,2(), XU Yong1,2, YANG Jiuyan1,2, TU Guangsheng1,2, TU Bingtian1,2, WANG Hao1,2()
Received:
2023-12-21
Revised:
2024-01-20
Published:
2024-05-20
Online:
2024-02-22
Contact:
WANG Hao, professor. E-mail: shswangh@whut.edu.cnAbout author:
LÜ Zhaoyang (1999-), male, Master candidate. E-mail: lvzhaoyang2021@163.com
Supported by:
摘要:
MgAl1.9Ga0.1O4透明陶瓷具有优异的光学性能, 其制备依赖于高质量坯体的凝胶注模成型和长时间的无压预烧。本研究选择MgF2为烧结助剂, 并通过瞬时液相调节无压预烧的致密化过程。采用干压成型、无压预烧和热等静压烧结制备了不同尺寸的MgAl1.9Ga0.1O4透明陶瓷样品, 并系统分析了MgF2对材料显微结构、光学和机械性能的影响。研究表明:MgF2在~1230 ℃熔化形成的液相促使陶瓷的致密度与晶粒尺寸增大, 后续烧结过程中残留的MgF2氧化为MgO并固溶进入MgAl1.9Ga0.1O4晶格。添加质量分数0.2% MgF2的2.04 mm厚透明陶瓷样品在紫外和可见光区域具有76.5%~83.4%的直线透过率和较高的光学质量。此外, 该陶瓷的特征抗弯强度为167.1 MPa, 与细晶MgAl2O4透明陶瓷相近, 但是前者的Weibull模数(8.81±0.29)更高。本研究为制备光学性能良好的大尺寸MgAl1.9Ga0.1O4透明陶瓷提供了新的选择。
中图分类号:
吕朝阳, 徐勇, 杨久延, 涂广升, 涂兵田, 王皓. MgF2助剂对MgAl1.9Ga0.1O4透明陶瓷的制备与光学性能的影响[J]. 无机材料学报, 2024, 39(5): 531-538.
LÜ Zhaoyang, XU Yong, YANG Jiuyan, TU Guangsheng, TU Bingtian, WANG Hao. Effect of MgF2 Additive on Preparation and Optical Properties of MgAl1.9Ga0.1O4 Transparent Ceramics[J]. Journal of Inorganic Materials, 2024, 39(5): 531-538.
图1 含0.1%、0.2%、0.5% MgF2的MAGS-0.1陶瓷与无助剂MAGS-0.1陶瓷的烧结轨迹曲线
Fig. 1 Sintering trajectories of MAGS-0.1 ceramics with 0.1%, 0.2% and 0.5% MgF2 and the unaided MAGS-0.1 ceramics Colorful figure is available on website
图2 含0、0.2% MgF2的MAGS-0.1陶瓷坯体收缩率和收缩速率随温度的变化曲线
Fig. 2 Variations of the shrinkage and shrinkage rate of MAGS-0.1 ceramic green bodies containing 0 and 0.2% MgF2 as a function of temperature (a) Shrinkage curves; (b) Shrinkage rate curves
图3 含10% MgF2 MAGS-0.1粉体的TG-DSC曲线与不同温度保温后含10% MgF2 MAGS-0.1粉体的XRD图谱
Fig. 3 TG-DSC curves of MAGS-0.1 powder containing 10% MgF2 and XRD patterns of MAGS-0.1 powder containing 10% MgF2 after heating and holding at different temperatures (a) TG-DSC curves of MAGS-0.1 powder containing 10% MgF2 heated at 10 ℃/min; (b) XRD patterns of MAGS-0.1 powder containing 10% MgF2 after heating and holding at 1150, 1250, 1350 and 1450 ℃ for 5 min followed by quenching; (c) Enlarged XRD patterns of the (220) crystal face in (b)
图6 无压预烧后经化学刻蚀的不同助剂含量的MAGS-0.1陶瓷的表面SEM照片及粒度分布图
Fig. 6 Surface SEM images and grain size distributions of MAGS-0.1 ceramics with different additive contents after pressureless presintering and chemical etching (a, d) Sample with 0.2% MgF2; (b, e) Sample with 0.5% MgF2; (c, f) Sample without additive
图7 HIP烧结后经化学刻蚀的MAGS-0.1陶瓷的表面SEM照片与粒度分布图
Fig. 7 Surface SEM images and grain size distributions of MAGS-0.1 ceramics after HIP sintering and chemical etching (a, c) Sample with 0.2% MgF2; (b, d) Sample without additive
图8 无助剂与含0.2% MgF2的MAGS-0.1透明陶瓷的表观照片
Fig. 8 Appearance images of MAGS-0.1 transparent ceramics without additive and with 0.2% MgF2 (a) Sample with 0.2% MgF2; (b) Sample without additive
图9 无助剂与含0.2% MgF2的MAGS-0.1透明陶瓷的光学偏振透射显微镜照片
Fig. 9 Optical polarized transmission micrographs of transparent ceramics without additive and with 0.2% MgF2 (a) Sample with 0.2% MgF2; (b) Sample without additive
图10 不同助剂含量与不同尺寸样品的光学性能
Fig. 10 Optical properties of samples with different additive contents and sizes Inset: Appearance image of a sample containing 0.2% MgF2 with ϕ108.8 mm×9.36 mm
图11 MAGS-0.1透明陶瓷抗弯强度的Weibull统计图
Fig. 11 Weibull plots of fracture strength for MAGS-0.1 transparent ceramics (a) Sample without additive[6]; (b) Sample with 0.2% MgF2
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