Preparation and properties of expanded graphite modified by zirconium oxychloride

doi:10.3969/j.issn.1001-1935.2021.02.008

Abstract

Abstract:

In order to improve the graphitization degree and oxidation resistance of expanded graphite,the modified expanded graphite was prepared by vacuum impregnation of zirconium oxychloride solution and high-temperature carbon embedded heat treatment.Effects of the carbon embedded temperature (1 550,1 600,and 1 650 ℃) and vacuum impregnation duration (30,60,and 90 min) on the graphitization degree and oxidation resistance of the expanded graphite were researched.The results show that:(1)after modification,the graphitization degree and oxidation resistance of the expanded graphite are improved;(2)the graphitization degree and oxidation resistance of the modified expanded graphite improve with the temperature rising from 1 550 ℃ to 1 600 ℃,but decrease from 1 600 ℃ to 1 650 ℃;(3)the graphitization degree and oxidation resistance of the modified expanded graphite improve with the vacuum impregnation duration prolonging from 30 min to 60 min,but decrease from 60 min to 90 min;(4)the graphitization degree and oxidation resistance of the modified expanded graphite prepared by impregnation at -0.08 MPa vacuum for 60 min and then carbon embedded heat treated at 1 600 ℃ for 3 h are the best.

Key words: zirconium oxychloride, modification treatment, expanded graphite, graphitization degree, oxidation resistance

摘要：

为了提高膨胀石墨的石墨化度和抗氧化性,经氧氯化锆溶液真空浸渍后再经高温埋碳热处理制备了改性膨胀石墨,主要研究了改性前的石墨化度和抗氧化性及埋碳热处理温度(分别为1 550、1 600、1 650 ℃)和氧氯化锆溶液真空浸渍时间(分别为30、60、90 min)对改性膨胀石墨的石墨化度和抗氧化性的影响。结果表明:1)经改性处理,膨胀石墨的石墨化度和抗氧化性提高。2)随着埋碳热处理温度从1 550 ℃提高到1 600 ℃,改性膨胀石墨的石墨化度和抗氧化性提高;随着埋碳热处理温度从1 600 ℃提高到1 650 ℃,改性膨胀石墨的石墨化度和抗氧化性降低。3)随着氧氯化锆真空浸渍时间从30 min延长到60 min,改性膨胀石墨的石墨化度和抗氧化性提高;随着氧氯化锆真空浸渍时间从60 min延长到90 min,改性膨胀石墨的石墨化度和抗氧化性降低。4)在-0.08 MPa真空度下浸渍60 min,再在1 600 ℃埋碳热处理3 h制备的改性膨胀石墨的石墨化度和抗氧化性能最高。

关键词: 氧氯化锆, 改性处理, 膨胀石墨, 石墨化度, 抗氧化性

CLC Number:

TQ175

Wang Ziyi, Wei Juncong, Zheng Xiaoyi, Wang Ziqi, Tu Junbo, Yu Baisong, Su Yuqing, Wang Yilong. Preparation and properties of expanded graphite modified by zirconium oxychloride[J]. Refractories, 2021, 55(2): 126-130.

王梓祎, 魏军从, 郑晓艺, 王子琦, 涂军波, 郁柏松, 苏玉庆, 王义龙. 氧氯化锆改性膨胀石墨的制备及性能研究[J]. 耐火材料, 2021, 55(2): 126-130.

Figures/Tables 8

Fig.1 XRD patterns of modified EG prepared by carbon embedded heat treatment at different temperatures and before modification

Fig.2 Raman spectra of modified EG prepared by carbon embedded heat treatment at different temperatures and before modification

Fig.3 SEM photos of EG before modification

Fig.4 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 550 ℃

Fig.5 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 600 ℃

Fig.6 SEM photos of modified EG prepared by carbon embedded heat treatment at 1 650 ℃

Fig.7 TG-DSC curves of modified EG prepared before and after carbon embedded heat treatment at different temperatures

Fig.8 Raman spectra of modified EG prepared before and after vacuum impregnation in zirconium oxychloride impregnation solution for different periods

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