纳米Al<sub>2</sub>O<sub>3</sub>改性SiBCN陶瓷高温粘接剂的制备与性能研究

doi:10.11902/1005.4537.2019.089

中国腐蚀与防护学报

2020, Vol. 40

Issue (4): 367-372 DOI: 10.11902/1005.4537.2019.089

研究报告

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纳米Al₂O₃改性SiBCN陶瓷高温粘接剂的制备与性能研究

王海卫¹, 常森²^,³(

), 栾新刚³, 宋雪梅², 王稹², 李彦樟², 陈建利², 张计荣², 韩明², 丘丹圭²

1.中核霞浦核电有限公司霞浦 355100
2.中国辐射防护研究院太原 030006
3.西北工业大学超高温结构复合材料重点实验室西安 710072

Preparation and Properties of Ceramics Composed of Nano-Al₂O₃ and Polysiloxane-polyborosilicate-TiB₂ Modified Polysilborazane as High Temperature Adhesive for SiC Based Ceramics

WANG Haiwei¹, CHANG Sen²^,³(

), LUAN Xin'gang³, SONG Xuemei², WANG Zhen², LI Yanzhang², CHEN Jianli², ZHANG Jirong², HAN Ming², QIU Dangui²

1. CNNP Xiapu Nuclear Power Co. Ltd. , Xiapu 355100, China
2. China Institute for Radiation Protection, Taiyuan 030006, China
3. Science and Technology on Thermo Structural Composite Materials Laboratory, Northwestern Polytechnical University, Xi'an 710072, China

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摘要:

为了进一步提高PSO-PBSZ-TiB₂改性PSNB胶粘剂 (标记为PPPT) 的热稳定性和粘接强度，通过添加纳米Al₂O₃制备出了新的复合胶粘剂 (标记为PPPTA)，研究了其与SiC陶瓷片的粘接性能。采用SEM和XRD等测试方法，分析了改性粘接剂的微观结构和物相组成，研究了裂解温度和纳米Al₂O₃对SiBCN陶瓷的微观结构和粘接强度的影响，揭示了纳米Al₂O₃对SiBCN陶瓷的强韧化机理。结果表明，在120 ℃空气中固化2 h，然后在1000 ℃空气中裂解2 h后，PPPT和PPPTA室温粘接强度最高分别达到11.23和15.91 MPa，在800 ℃空气中的高温剪切强度分别达到10.4和12.1 MPa。分析表明，添加纳米Al₂O₃可同时有效抑制粘接层的体积收缩和玻璃相在高温时的挥发，从而显著提高粘接强度。

关键词 ：聚硅硼氮烷, 纳米Al₂O₃, 玻璃相, 高温粘接强度

Abstract：

In order to improve the thermal stability and adhesion strength of PSO (polysiloxane)-PBSZ (polyborosilicate)-TiB₂ modified PSNB (polysilborazane) (labeled as PPPT), PSNB was modified by Al₂O₃-PSO-PBSZ-TiB₂ (denoted as PPPTA), and it was used for joining SiC ceramic discs. The microstructure and phase composition of the modified adhesive were analyzed by SEM and XRD. The effect of pyrolysis temperature and addition amount of nano-Al₂O₃ on the microstructure and adhesion strength for the bonding pair of SiBCN ceramics were investigated. The strengthening and toughening mechanism of nano-Al₂O₃ to the bonding SiBCN ceramics was revealed. After curing in air at 120 ℃ for 2 h and then pyrolysis in air at 1000 ℃ for 2 h, the room temperature adhesion strength of PPPT and PPPTA is up to 11.23 and 15.91 MPa, respectively, and more importantly, the high temperature (in air at 800 ℃) shear strength reaches 10.4 and 12.1 MPa, respectively. The analysis shows that nano-Al₂O₃ can effectively suppress the volume shrinkage of the adhesive layer and inhibit the volatilization of the glass phase at high temperature, thereby significantly improving the adhesion strength.

Key words： polyborosilazane nano-Al₂O₃ glass high temperature strength

收稿日期: 2019-06-21

ZTFLH:

TQ174

基金资助:国家重点研发计划(2017YFB0703200);西北工业大学凝固技术国家重点实验室项目(135-QP-2015);中央高校自主创新项目(3102017zy058)

通讯作者: 常森 E-mail: changsen0869@163.com

Corresponding author: CHANG Sen E-mail: changsen0869@163.com

作者简介: 王海卫，男，1977年生，高级工程师

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引用本文:

王海卫, 常森, 栾新刚, 宋雪梅, 王稹, 李彦樟, 陈建利, 张计荣, 韩明, 丘丹圭. 纳米Al₂O₃改性SiBCN陶瓷高温粘接剂的制备与性能研究[J]. 中国腐蚀与防护学报, 2020, 40(4): 367-372.
Haiwei WANG, Sen CHANG, Xin'gang LUAN, Xuemei SONG, Zhen WANG, Yanzhang LI, Jianli CHEN, Jirong ZHANG, Ming HAN, Dangui QIU. Preparation and Properties of Ceramics Composed of Nano-Al₂O₃ and Polysiloxane-polyborosilicate-TiB₂ Modified Polysilborazane as High Temperature Adhesive for SiC Based Ceramics. Journal of Chinese Society for Corrosion and protection, 2020, 40(4): 367-372.

链接本文:

https://www.jcscp.org/CN/10.11902/1005.4537.2019.089 或 https://www.jcscp.org/CN/Y2020/V40/I4/367

图1 PSNB，PSO和PBSZ的分子式[18]

图2 PPPT和PPPTA在室温和800 ℃下的粘接强度

图3 PPPT和PPPTA粘接试样在1000 ℃空气中裂解2 h后的截面形貌

图4 PPPT和PPPTA粘接试样分别在1000和1200 ℃空气中裂解2 h后接头的室温断口形貌

图5 PPPT和PPPTA粘接试样分别在1000和1200 ℃空气中裂解2 h后接头在800 ℃空气中的断口形貌

图6 PPPT和PPPTA在1000和1200 ℃空气中裂解2 h后的XRD谱

图7 纳米Al2O3增强SiBCN陶瓷的示意图

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