微波干燥自发凝固成型氧化铝湿坯

doi:10.15541/jim20220469

无机材料学报 ›› 2023, Vol. 38 ›› Issue (4): 461-468.DOI: 10.15541/jim20220469

微波干燥自发凝固成型氧化铝湿坯

刘文龙¹^,²(), 赵瑾¹^,²(), 刘娟¹^,², 毛小建¹^,², 章健¹^,², 王士维¹^,²()

1.中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海200050
2.中国科学院大学材料科学与光电研究中心, 北京 100049

收稿日期:2022-08-09 修回日期:2022-11-25 出版日期:2023-04-20 网络出版日期:2022-12-09
通讯作者: 赵瑾, 助理研究员. E-mail: zhaojin@mail.sic.ac.cn;
王士维, 研究员. E-mail: swwang51@mail.sic.ac.cn
作者简介:刘文龙(1997-), 男, 硕士研究生. E-mail: liuwenlong20@mails.ucas.ac.cn

Microwave Drying of Spontaneous-Coagulation-Cast Wet Alumina Green Body

LIU Wenlong¹^,²(), ZHAO Jin¹^,²(), LIU Juan¹^,², MAO Xiaojian¹^,², ZHANG Jian¹^,², WANG Shiwei¹^,²()

1. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2022-08-09 Revised:2022-11-25 Published:2023-04-20 Online:2022-12-09
Contact: ZHAO Jin, lecturer. E-mail: zhaojin@mail.sic.ac.cn;
WANG Shiwei, professor. E-mail: swwang51@mail.sic.ac.cn
About author:LIU Wenlong (1997-), male, Master candidate. E-mail: liuwenlong20@mails.ucas.ac.cn
Supported by:
National Natural Science Foundation of China(52130207)

摘要/Abstract

摘要：

为了解决常规干燥(控温控湿)过程中坯体出现水分梯度问题, 利用微波干燥法来干燥湿坯。通过对比常规干燥(温度: 40 ℃; 湿度: 60%)和微波干燥的方式, 研究了湿坯的重量损失、线性收缩、表面温度和水分分布。与常规干燥相比, 采用微波干燥(功率250 W)时, 干燥结束时间和停止收缩时间分别缩短至1/6.8和1/6。在微波干燥过程中, 样品表面温度随时间延长先升高后降低, 与体内水分密切相关。而在常规干燥过程中, 温度保持恒定在40 ℃。采用低场核磁共振（NMR）成像技术表征湿坯内部的水分分布情况发现: 在微波干燥过程中, 水分分布更均匀, 表明微波干燥时湿坯的干燥应力更低。在1550 ℃下烧结6 h后, 微波干燥制备得到的氧化铝陶瓷具有更高的抗弯强度, 且标准差更小。

关键词: 微波干燥, 低场核磁共振成像, 水分分布, 氧化铝, 凝胶

Abstract:

To solve moisture gradients in the conventional drying with controlled temperature and relative humidity, microwave heating was employed to dry wet alumina green bodies shaped by spontaneous coagulation casting. The weight loss, linear shrinkage, surface temperature, and moisture distribution of the green bodies by conventional drying (temperature: 40 ℃; humidity: 60%) and microwave drying were investigated. The time for no further weight loss and shrinkage of the body by microwave drying (power: 250 W) were respectively shortened to 1/6.8 and 1/6 of those by conventional drying. Surface temperature of the green body during the microwave drying increased firstly and then decreased with time, which was strongly correlated with the internal moisture, while the temperature in the conventional drying keeping at 40 ℃. Low-field nuclear-magnetic-resonance (NMR) imaging revealed that the moisture distribution in the green bodies dried by microwave drying was more uniform than that by conventional drying, indicating that drying stress in the former was lower than that in the latter. After sintering at 1550 ℃ for 6 h, alumina ceramics from microwave drying had a higher flexural strength with a smaller deviation than that from conventional drying.

Key words: microwave drying, low-field nuclear-magnetic-resonance imaging, moisture distribution, alumina, coagulation

中图分类号:

TQ174

刘文龙, 赵瑾, 刘娟, 毛小建, 章健, 王士维. 微波干燥自发凝固成型氧化铝湿坯[J]. 无机材料学报, 2023, 38(4): 461-468.

LIU Wenlong, ZHAO Jin, LIU Juan, MAO Xiaojian, ZHANG Jian, WANG Shiwei. Microwave Drying of Spontaneous-Coagulation-Cast Wet Alumina Green Body[J]. Journal of Inorganic Materials, 2023, 38(4): 461-468.

图/表 10

Fig. 1 Effects of (a) drying methods and (b) microwave power on the volume fraction of residual water in wet alumina green bodies

Table 1 CRP and residual water (after CRP and drying) of samples

Drying method	Microwave power/W	CRP/ h	Residual water after CRP/% (in vol.)	Residual water after drying/% (in vol.)
Conventional	—	10	(20.4±1.5)	0.8
Microwave	250	1.8	(11.2±1.4)	0.6
	400	1.3	(9.4±1.4)	0.5
	550	1.0	(7.7±0.7)	0.4

Fig. 2 Effects of (a) drying methods and (b) microwave power on shrinkage behavior of wet alumina green bodies

Table 2 Shrinkage stop time and shrinkage of samples

Drying method	Microwave power/W	Shrinkage stop time/h	Shrinkage/%
Conventional	—	6.0	(4.9±0.1)
Microwave	250	1.0	(5.2±0.1)
	400	0.7	(5.1±0.1)
	550	0.5	(4.8±0.1)

Fig. 3 Effect of microwave power on the surface temperature of wet alumina green bodies

Fig. 4 Photos of alumina green bodies dried by (a, e) conventional drying and microwave drying ((b, f) 250 W, (c, g) 400 W, and (d, h) 550 W)

Fig. 5 Effects of (a) drying methods and (b) microwave power on pore-size distribution of alumina green bodies

Fig. 6 Fracture surfaces of alumina green bodies (a) Microwave drying (250 W); (b) Conventional drying

Fig. 7 Moisture distributions of wet alumina green bodies in the drying process (a) Conventional drying for 0, 2, 4, 8, and 15 h; (b) 250-W microwave drying for 0, 0.3, 0.6, 1.2, and 2 h

Fig. 8 Effect of drying methods on flexural strength of alumina green bodies and ceramics

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微波干燥自发凝固成型氧化铝湿坯

Microwave Drying of Spontaneous-Coagulation-Cast Wet Alumina Green Body

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