莫来石晶须/堇青石表面层的制备及准超疏水性能

doi:10.7503/cjcu20190090

摘要/Abstract

摘要：

采用溶胶-凝胶法制备了硅铝混合凝胶粉体, 再通过熔盐反应在堇青石陶瓷基体上生长莫来石晶须, 制得莫来石晶须/堇青石表面层微结构. 表征结果表明, 莫来石晶须紧密生长在堇青石基体上, 晶须直径为100~300 nm, 长度可达几个微米. 莫来石晶须表面含有大量Si—OH和Al—OH极性亲水基团, 采用十二烷基三甲氧基硅烷与活性基团间的偶联反应将非极性基团引入莫来石晶须表面, 获得了静态润湿角为146°的莫来石晶须/堇青石表面层. 动态润湿研究表明, 合成的莫来石晶须增大了堇青石陶瓷的表面粗糙度, 使亲水的莫来石晶须/堇青石表面更加亲水, 而硅烷偶联剂修饰的堇青石/莫来石晶须表面则成为准超疏水表面.

关键词: 堇青石陶瓷, 莫来石晶须, 润湿角, 疏水性, 表面粗糙度

Abstract:

Silicon-aluminum hybrid gel powders were prepared by sol-gel technology, and the microstructure of mullite whiskers/cordierite was obtained through growth of mullite whiskers on the surface of cordierite ceramic substrate by molten salt reaction. X-Ray diffraction, scanning electron microscopy and energy dispersive X-ray spectroscopy were employed to characterized the structural morphology and phase compositions. The results show that the surface of cordierite ceramic was covered by dense mullite whiskers with nanometer-sized(100—300 nm) diameters and micrometer-sized lengths. The surface modification of mullite whiskers was performed by coupling reaction between n-dodecyltrimethoxysilan and numerous active groups(Si—OH, Al—OH) on the surface of mullite whiskers, and static wetting angle of this sample is 146°. Dynamic wetting studies show that mullite whiskers increase the surface roughness of cordierite ceramics, making the hydrophilic mullite whiskers/cordierite surface more hydrophilic and the surface of the mullite whiskers/cordierite modified by the silane coupling agent change into quasi-superhydrophobic surface

Key words: Cordierite ceramics, Mullite whiskers, Wetting angle, Hydrophobicity, Surface roughness

中图分类号:

O647

TrendMD:

杜毅帆, 艾超前, 张瑶瑶, 王伟. 莫来石晶须/堇青石表面层的制备及准超疏水性能. 高等学校化学学报, 2019, 40(9): 1955.

DU Yifan, AI Chaoqian, ZHANG Yaoyao, WANG Wei. Preparation and Quasi-superhydrophobic Properties of the Surface of Mullite Whiskers/Cordierite ^†. Chem. J. Chinese Universities, 2019, 40(9): 1955.

图/表 10

Fig.1 XRD patterns(A) and SEM images of samples obtained at the molten salts reaction temperatures of 950(B), 1000(C) and 1050 ℃(D)

Fig.2 SEM images of cordierite(A) and the samples obtained at the molten salts reaction temperatures of 950(B), 1000(C) and 1050 ℃(D)

Fig.3 SEM image(A), EDS mapping scannings(B—E) and static wetting angle(F) of the sample prepared through molten salt reaction and silane coupling reaction treatment at 1000 ℃ Elemental content(molar fraction): (B) Al, 26.05%; (C) Si, 9.51%; (D) O, 57.24%; (E) C, 7.20%.

Fig.4 TEM(A) and HRTEM(B) images of mullite whiskers after ultrasonic treatment

Fig.5 XPS spectra of the sample prepared through molten salt reaction and silane coupling reaction treatment (A) Survey spectrum; (B) C1s; (C) O1s; (D) Si2p; (E) Al2p.

Fig.6 FTIR spectra of mullite whiskers/cordierite(a) and mullite whiskers/cordierite modifed by silane(b)

Fig.7 Schematic illustration of hydrophobic mullite whiskers/cordierite interface preparation

Fig.8 Surface dynamic wettability of different interface layers (A) Cordierite; (B) mullite whiskers/cordierite; (C) cordierite modified by silane; (D) mullite whiskers/cordierite modified by silane.

Fig.9 Wettability of different solvents on the interface of mullite whiskers/cordierite modified by silane coupling agent (A) Carbon tetrachloride; (B) xylene; (C) kerosene; (D) water.

Fig.10 Effect of reaction time of silane coupling agent on surface contact angle

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