Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, PR China.
Langmuir. 2010 Feb 16;26(4):2769-73. doi: 10.1021/la902812g.
Silylated layered double hydroxides (LDHs) were synthesized through a surfactant-free method involving an in situ condensation of silane with the surface hydroxyl group of LDHs during its reconstruction in carbonate solution. X-ray diffraction (XRD) patterns showed the silylation reaction occurred on the external surfaces of LDHs layers. The successful silylation was evidenced by (29)Si cross-polarization magic-angle spinning nuclear magnetic resonance ((29)Si CP/MAS NMR) spectroscopy, attenuated total reflection Fourier transform infrared (ATR FTIR) spectroscopy, and infrared emission spectroscopy (IES). The ribbon shaped crystallites with a "rodlike" aggregation were observed through transmission electron microscopy (TEM) images. The aggregation was explained by the T(2) and T(3) types of linkage between adjacent silane molecules as indicated in the (29)Si NMR spectrum. In addition, the silylated products show high thermal stability by maintained Si related bands even when the temperature was increased to 1000 degrees C as observed in IES spectra.
硅烷化层状双氢氧化物（LDHs）通过一种无表面活性剂的方法合成，该方法涉及在 LDHs 在碳酸盐溶液中重构期间，硅烷与 LDHs 表面羟基的原位缩合。X 射线衍射（XRD）图谱表明硅烷化反应发生在 LDHs 层的外表面上。（29）Si 交叉极化魔角旋转核磁共振（（29）Si CP/MAS NMR）光谱、衰减全反射傅里叶变换红外（ATR FTIR）光谱和红外发射光谱（IES）证明了硅烷化反应的成功。通过透射电子显微镜（TEM）图像观察到具有“棒状”聚集的带状微晶。TEM 图像表明，这种聚集是由相邻硅烷分子之间的 T(2)和 T(3)类型的键合引起的，如（29）Si NMR 谱所示。此外，硅烷化产物在 IES 光谱中观察到即使温度升高到 1000°C 时仍保持 Si 相关带，显示出高的热稳定性。
