氧化硼-磷酸浸渍对中间相炭微球复合材料抗氧化及力学性能的影响

doi:10.15541/jim20140658

无机材料学报 ›› 2015, Vol. 30 ›› Issue (7): 769-773.DOI: 10.15541/jim20140658 CSTR: 32189.14.10.15541/jim20140658

氧化硼-磷酸浸渍对中间相炭微球复合材料抗氧化及力学性能的影响

雷卓研^{1, 2}, 王志^{1, 2}, 范恒冰², 马文斌², 陈健², 王旭²

(沈阳航空航天大学 1. 辽宁省通用航空重点实验室; 2. 安全工程学院, 沈阳 110136)

收稿日期:2014-12-18 修回日期:2015-01-31 出版日期:2015-07-20 网络出版日期:2015-06-25
作者简介:雷卓研(1990–), 女, 硕士研究生. E-mail: leizhuoyan@126.com
基金资助:
沈阳市科技计划项目(F12-277-1-33);辽宁省高等学校杰出青年学者成长计划(LJQ2012014)

Effect of B₂O₃ Doping and Phosphate Impregnation on Oxidation Resistance and Mechanical Properties of Mesocarbon Microbead Composites

LEI Zhuo-Yan^{1, 2}, WANG Zhi^{1, 2}, FAN Heng-Bing², MA Wen-Bin², CHEN Jian², WANG Xu²

(1. Liaoning General Aviation?key laboratory, Shenyang Aerospace University, Shenyang 110136, China; 2. School of Safety Engineering, Shenyang Aerospace University, Shenyang 110136, China)

Received:2014-12-18 Revised:2015-01-31 Published:2015-07-20 Online:2015-06-25
About author:LEI Zhuo-Yan. E-mail: leizhuoyan@126.com
Supported by:
Shenyang Science and Technology Program (F12-277-1-33);Program for Liaoning Excellent Talents in University (LJQ2012014)

摘要/Abstract

摘要：

以原位缩聚法制备的中间相炭微球/碳纳米管(MCMB/CNTs)复合微球为原料, 通过添加氧化硼(B₂O₃)粉体和磷酸浸渍对该复合材料进行了基体和表面改性。采用扫描电子显微镜(SEM)、三点弯曲法、热重分析(TG)以及恒温氧化测试方法对复合材料的表面形貌、弯曲强度以及抗氧化性能进行了表征与测试。结果表明: 添加适量的B₂O₃可以有效提升复合材料的抗氧化性能和弯曲强度, B₂O₃含量超过2%时, 复合材料的弯曲强度逐渐下降。将含有2% B₂O₃的复合材料试样进行磷酸浸渍处理后, 试样的弯曲强度可达66 MPa, 初始氧化温度520℃, 经过500℃恒温氧化60 min后其氧化失重率仅为5%, 弯曲强度仍达到50.3 MPa。

关键词: 中间相炭微球, 弯曲强度, 氧化失重率, 抗氧化

Abstract:

Mesocarbon microbead/carbon nanotubes (MCMB/CNTs) composites were modified by adding B₂O₃ powders and phosphate impregnation and the MCMB/CNTs were prepared using in-situ thermal polymerization. The morphology, flexural strength and oxidation resistance behavior were studied using scanning electron microscope (SEM), three-point bending tests, thermo gravimetric analysis (TG) and isothermal oxidation method. The results show that the oxidation resistance and flexural strength of the composites are enhanced with proper amount of B₂O₃. When the ratio of B₂O₃is beyond 2%, the flexural strength of the sample begins to decrease. The sample with 2% B₂O₃ impegnated with phosphate reachs the highest flexural strength of 66 MPa, and the initial mass loss temperature of the samples is 520℃. After isothermal oxidation at 500℃ for 60 min, the mass loss and the flexural strength of the sample are 5% and 50.3 MPa, respectively.

Key words: mesocarbon microbead, flexural strength, mass loss, oxidation resistance

中图分类号:

TQ174

雷卓研, 王志, 范恒冰, 马文斌, 陈健, 王旭. 氧化硼-磷酸浸渍对中间相炭微球复合材料抗氧化及力学性能的影响[J]. 无机材料学报, 2015, 30(7): 769-773.

LEI Zhuo-Yan, WANG Zhi, FAN Heng-Bing, MA Wen-Bin, CHEN Jian, WANG Xu. Effect of B₂O₃ Doping and Phosphate Impregnation on Oxidation Resistance and Mechanical Properties of Mesocarbon Microbead Composites[J]. Journal of Inorganic Materials, 2015, 30(7): 769-773.

图/表 7

表1 不同处理工艺的配方

Table 1 Formula of different processing methods

Sample	B₂O₃ content /wt%	H₃PO₄ impregnant content /mL
a	0	No
b	2	No
c	5	No
d	10	No
e	2	80

表2 不同处理工艺试样的弯曲强度

Table 2 Flexural strength of specimens treated with different processing methods

	No additive	2% B₂O₃	5% B₂O₃	10% B₂O₃	2% B₂O₃ +H₃PO₄
Flexural strength /MPa	47.0	52.0	42.0	31.6	66.0

图1 不同工艺处理后试样的断口形貌

Fig. 1 Fracture morphologies of specimens with different processing methods (a) No additive; (b) 2% B2O3; (c) 10%B2O3; (d) 2%B2O3+ H3PO4

图2 氧化失重率对样品力学性能的影响

Fig. 2 Influence of mass loss on line the flexural strength

图3 氧化时间对样品力学性能的影响

Fig. 3 Influence of oxidation time on flexural strength

图4 浸渍处理试样在500℃下不同氧化时间的表面 SEM 形貌

Fig. 4 Surface SEM images of the phosphate impregnated specimens affer oxidation at 500℃ for different time (a) 0 min; (b) 60 min; (c) 120 min

图5 试样的热重分析曲线

Fig. 5 TG curves of specimens

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氧化硼-磷酸浸渍对中间相炭微球复合材料抗氧化及力学性能的影响

Effect of B₂O₃ Doping and Phosphate Impregnation on Oxidation Resistance and Mechanical Properties of Mesocarbon Microbead Composites

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氧化硼-磷酸浸渍对中间相炭微球复合材料抗氧化及力学性能的影响

Effect of B2O3 Doping and Phosphate Impregnation on Oxidation Resistance and Mechanical Properties of Mesocarbon Microbead Composites

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Effect of B₂O₃ Doping and Phosphate Impregnation on Oxidation Resistance and Mechanical Properties of Mesocarbon Microbead Composites