碳粉对熔融石英析晶行为的影响

doi:10.16552/j.cnki.issn1001-1625.2026.0222

摘要/Abstract

摘要：

本工作系统性研究了碳粉单独存在及与六方氮化硼（h-BN）共存对熔融石英析晶行为的影响。根据组分差异，设计了纯熔融石英、添加h-BN、添加碳粉和复合添加碳粉/h-BN的熔融石英四类方案，在1 250 ℃下热处理0.5 h后，综合运用多种表征手段，研究碳粉对熔融石英析晶程度、微观结构及热行为的影响规律。结果表明，碳粉的添加显著加速了方石英晶相的生成，特别是在碳粉/h-BN共存体系中，碳粉有效克服甚至完全抵消了h-BN的抑制析晶效应，共存体系中的析晶程度接近或超过了未添加任何抑制剂的纯熔融石英样品。此外，过量的碳粉还严重阻碍了样品的致密化进程，导致了力学性能劣化及热膨胀系数升高。本研究明确了在评估熔融石英的高温服役可靠性与实际生产中原料纯度的控制时，必须将碳杂质与h-BN间的影响机制纳入考量。研究结果为高纯硅基材料的原料管控、工艺优化及复杂工况下的寿命预测提供了关键的理论依据。

关键词: 熔融石英, 六方氮化硼, 碳, 析晶, 抑制作用

Abstract:

In this work， the effects of carbon powder， both individually and in combination with hexagonal boron nitride （h-BN）， on the crystallization behavior of fused silica were systematically investigated. Based on compositional variations， four experimental groups were designed： pure fused silica， fused silica with h-BN addition， fused silica with carbon powder addition， and fused silica with a co-addition of carbon powder and h-BN. Following heat treatment at 1 250 ℃ for 0.5 h， various characterization techniques were comprehensively employed to evaluate the effects of carbon powder on the degree of crystallization， microstructure， and thermal behavior of the fused silica. Experimental results demonstrate that the addition of carbon powder significantly accelerates the formation of the cristobalite phase. Notably， in the carbon/h-BN co-addition system， the carbon powder effectively overcomes and even completely negates the crystallization-inhibiting effect of h-BN. Consequently， the degree of crystallization approaches or even exceeds that of the pure fused silica samples without any added inhibitors. Furthermore， excessive carbon powder severely impedes the densification process of the samples， leading to the deterioration of mechanical properties and an increase in the coefficient of thermal expansion. This study highlights that the interaction mechanisms between carbon impurities and h-BN must be considered when evaluating the high-temperature service reliability of fused silica and controlling raw material purity in practical production. These findings provide a crucial theoretical basis for raw material management， process optimization， and lifespan prediction of high-purity silica-based materials under complex operating conditions.

Key words: fused silica, hexagonal boron nitride, carbon, crystallisation, inhibition effect

中图分类号:

O783

邓伟杰, 包启富, 董伟霞, 刘明源, 曾帅, 李哲, 李亚敏. 碳粉对熔融石英析晶行为的影响[J]. 硅酸盐通报, 2026, 45(9): 3257-3266.

DENG Weijie, BAO Qifu, DONG Weixia, LIU Mingyuan, ZENG Shuai, LI Zhe, LI Yamin. Influence of Carbon Powder on Crystallization Behavior of Fused Silica[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2026, 45(9): 3257-3266.

图/表 12

图1 熔融石英的粒度分布

Fig.1 Particle size distribution of fused silica

表1 主要原料的化学组成

Table 1 Main chemical composition of raw materials

Raw material	Mass fraction/%
Raw material	SiO₂	BN	C	Na₂O	K₂O	Li₂O	B₂O₃	Cl	Ignition loss
Fused silica	≥99.00	—	—	≤0.50	≤0.40	≤0.04	≤0.05	≤0.01	≤1.00
h-BN	—	≥99.99	—	—	—	—	≤0.01	—	—
Carbon powder	—	—	100	—	—	—	—	—	—

图2 热处理温度-时间曲线

Fig.2 Temperature-time curve of heat treatment

图3 不同制备条件下熔融石英样品的TG-DTA曲线

Fig.3 TG-DTA curves of fused silica samples under different preparation conditions

图4 不同制备条件下熔融石英样品的拉曼光谱

Fig.4 Raman spectra of fused silica samples under different preparation conditions

图5 不同制备条件下熔融石英样品的XRD谱

Fig.5 XRD patterns of fused silica samples under different preparation conditions

图6 碳粉及碳粉/h-BN复合在熔融石英中的作用机制

Fig.6 Mechanisms of carbon powder and carbon powder/h-BN composite in fused silica

图7 不同制备条件下熔融石英样品的SEM照片

Fig.7 SEM images of fused silica samples under different preparation conditions

图8 熔融石英样品1 250 ℃热处理后的SEM照片及相应EDS谱（点1）

Fig.8 SEM images and corresponding EDS spectra （point 1） of fused silica samples after heat treatment at 1 250 ℃

图9 熔融石英样品1 250 ℃热处理后的抗折强度、吸水率、孔隙率与体积密度

Fig.9 Flexural strength， water absorption， porosity， and bulk density of fused silica samples after heat treatment at 1 250 ℃

图10 15%碳粉熔融石英样品1 250 ℃热处理前后的SEM照片

Fig.10 SEM images of fused silica samples with 15% carbon powder before and after heat treatment at 1 250 ℃

图11 不同制备条件下熔融石英样品的热膨胀系数

Fig.11 CTE of fused silica samples under different preparation conditions

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