复合持续时间对P2O5-Al2O3异相复合玻璃结构和力学性能的影响

doi:10.15541/jim20220286

摘要/Abstract

摘要：

近年来, 分相玻璃以其独特的结构以及优异的物理化学性质引起了广泛关注。本研究结合气动雾化加料和机械搅拌, 采用熔融冷却法制备了纳米SiO₂-Na₂O高硅玻璃颗粒增强的P₂O₅-Al₂O₃玻璃。通过改变复合持续时间, 研究了玻璃的结构与力学性能之间的关系。结果表明, 异相复合玻璃的杨氏模量高于P₂O₅-Al₂O₃玻璃, 并且随着复合持续时间由10 s增大到8 min, 玻璃的杨氏模量呈现先升高后降低的趋势, 在复合持续时间为6 min时, 杨氏模量达到最大值80.7 GPa。相比于P₂O₅-Al₂O₃玻璃, 杨氏模量提高了18%。引入SiO₂-Na₂O高硅玻璃颗粒不仅能够在基体玻璃中形成第二相, 而且会改变P₂O₅-Al₂O₃玻璃的结构。随着复合持续时间由10 s增大到6 min, 异相复合玻璃网络中磷的配位数逐渐增大, 并且玻璃网络中的非桥氧数量逐渐减少, 网络交联度逐渐增加。而复合持续时间超过8 min, 则不利于网络交联度的增加。异相复合玻璃的开发为耐损伤玻璃材料的制备提供了新的思路。

关键词: 异相复合玻璃, P₂O₅-Al₂O₃玻璃, 杨氏模量, 复合持续时间

Abstract:

In recent years, phase separation glass has attracted extensive attention because of its unique structure and excellent properties. But its mechanism of phase separation on glass remains insufficient clear, especially, the influence of recombination time on structure and properties is unclear. Here, strengthened P₂O₅-Al₂O₃ glass with SiO₂-Na₂O high-silicate glass particles as the second phase was prepared by melting-quenching method combined with pneumatic atomization and mechanical stirring. The relationship between structure and mechanical properties of the glass was investigated by varying the recombination time. Experiment results showed that Young's modulus of the heterogeneous composite glass was higher than that of the P₂O₅-Al₂O₃ glass. Young's modulus of the sample firstly increased and then decreased with the recombination time increasing from 10 s to 8 min. The highest Young's modulus of 80.7 GPa was obtained at recombination time of 6 min, which was increased by 18% as compared with the P₂O₅-Al₂O₃ glass. Introducing SiO₂-Na₂O high-silicate glass particles not only formed the second phase in the matrix glass, but also changed the structure of the P₂O₅-Al₂O₃ glass. As the recombination time increases from 10 s to 6 min, coordination number of phosphorus in heterogeneous composite glass network gradually increases, while amount of non-bridging oxygen in the glass network gradually decreases, resulting in a gradual increase in network cross-linking. However, when the recombination time is more than 8 min, it is not conducive to network crosslinking. Therefore, development of heterogeneous composite glass can provide a new route for the preparation of glass materials with good damage resistance.

Key words: heterogeneous composite glass, P₂O₅-Al₂O₃ glass, Young's modulus, recombination time

中图分类号:

TQ171

朱钦塨, 赵高凌, 韩高荣. 复合持续时间对P₂O₅-Al₂O₃异相复合玻璃结构和力学性能的影响[J]. 无机材料学报, 2023, 38(2): 170-176.

ZHU Qingong, ZHAO Gaoling, HAN Gaorong. Effect of Recombination Time on the Structure and Properties of P₂O₅-Al₂O₃ Heterogeneous Composite Glass[J]. Journal of Inorganic Materials, 2023, 38(2): 170-176.

图/表 9

图1 不同复合持续时间的样品(a)和复合持续10 min的样品(b)的XRD图谱(插图为样品照片)

Fig. 1 XRD patterns of samples prepared with different recombination time (a) and recombination time of 10 min (b) with inset showing optical photo of the sample

图2 P2O5-Al2O3基体玻璃(a)和SiO2-Na2O高硅玻璃(b)的FT-IR光谱图

Fig. 2 FT-IR spectra of P2O5-Al2O3 matrix glass (a) and SiO2-Na2O high-silicate glass (b) Colorful figures are available on website

图3 P2O5-Al2O3基体玻璃(a)和不同复合持续时间(b~f)的异相复合玻璃的AFM-IR图像

Fig. 3 AFM-IR images of the matrix glass (a) and heterogeneous composite glass prepared with different recombination time (b-f) (b) 10 s; (c) 2 min; (d) 4 min; (e) 6 min; (f) 8 min

图4 异相复合玻璃的高分辨率P2p XPS光谱 (采用最小二乘法拟合)

Fig. 4 High-resolution P2p XPS spectra for heterogeneous composite glass fitting with the least squares method Recombination time: (a) 10 s; (b) 2 min; (c) 4 min; (d) 6 min; (e) 8 min

表1 异相复合玻璃拟合得到的峰值位置、半峰宽(FWHM)和面积

Table 1 Peak positions, full width at half maximum (FWHM) and area from the fitting curves of P2p core levels for heterogeneous composite glass

Recombination time	Peak position/eV		FWHM/eV	Area/%
Recombination time	Main peak	Deconvoluted peak	FWHM/eV	Area/%
10 s	134.46	134.23	1.46	66.7
10 s	134.46	135.17	1.47	33.3
2 min	134.42	134.22	1.41	66.7
2 min	134.42	135.17	1.41	33.3
4 min	134.59	134.35	1.47	66.7
4 min	134.59	135.28	1.44	33.3
6 min	134.67	134.36	1.74	66.7
6 min	134.67	135.60	2.16	33.3
8 min	134.44	134.26	1.45	66.7
8 min	134.44	135.18	1.50	33.3

图5 异相复合玻璃高分辨率O1s XPS光谱 (用最小二乘法拟合)

Fig. 5 High-resolution O1s XPS spectra for heterogeneous composite glass fitting with the least squares method Recombination time: (a) 10 s; (b) 2 min; (c) 4 min; (d) 6 min; (e) 8 min

表2 异相复合玻璃拟合得到的峰值位置、半峰宽(FWHM)和面积比例

Table 2 Peak positions, full width at half maximum (FWHM) and area from the fitting curves of O1s core levels for heterogeneous composite glass

Recombina- tion time	NBO-Li/Mg			NBO-Al			BO
Recombina- tion time	BE/eV	FWHM/eV	Area/%	BE/eV	FWHM/eV	Area/%	BE/eV	FWHM/eV	Area/%
10 s	531.93	1.39	29.69	532.36	1.39	29.68	533.35	1.78	40.63
2 min	532.10	1.43	37.42	532.78	2.17	31.30	533.20	2.17	31.29
4 min	531.95	1.43	31.66	532.41	1.97	34.18	533.29	1.97	34.16
6 min	531.97	1.39	29.65	532.36	1.99	35.18	533.29	1.99	35.17
8 min	532.07	1.35	31.65	532.55	2.07	34.18	533.24	2.07	34.17

图6 不同复合持续时间P2O5-Al2O3异相复合玻璃的拉曼光谱

Fig. 6 Raman spectra of P2O5-Al2O3 heterogeneous composite glass prepared with different recombination time Colorful figure is available on website

图7 不同复合持续时间P2O5-Al2O3异相复合玻璃的杨氏模量

Fig. 7 Young's modulus of P2O5-Al2O3 heterogeneous composite glass prepared with different recombination time

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复合持续时间对P₂O₅-Al₂O₃异相复合玻璃结构和力学性能的影响

Effect of Recombination Time on the Structure and Properties of P₂O₅-Al₂O₃ Heterogeneous Composite Glass

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