Preparation of organic-inorganic hybrid precursors O=P(OSiMe3)x(OH)3-x for low-melting glasses
Preparation of organic-inorganic hybrid precursors O=P(OSiMe3)x(OH)3-x for low-melting glasses
复制标题
低熔点玻璃有机-无机杂化前驱体O=P(OSiMe3)x(OH)3-x的制备
DOI：
10.2109/jcersj.111.171
复制
发表时间：
2003
影响因子：
1.1
通讯作者：
T. Yoko
中科院分区：
文献类型：
--
作者：
H. Niida;Masahide Takahashi;T. Uchino;T. Yoko
提出了一种用于低熔点玻璃的有机-无机杂化前驱体的合成方法。该工艺以磷酸（H_3PO_4）和三甲基氯硅烷（Me_3SiCl）为原料，通过非水酸碱反应P-OH+Si-Cl→P-O-Si+HCl↑，合成了一种新型的硅基氧化物。29 Si和31 P NMR谱证实了P-O-SiMe 3键的形成和P-OH基团的消失。在高Si浓度下观察到的前体的粘度降低是由P-OH的数量减少引起的，这与氢键的减少有关。利用P-O-SiMe_3键，通过非水酸碱反应制备了Me_3SiO_（0.5）-Me_2SiO-SnO-P_2 O_5系统的低熔玻璃。由此获得的混合玻璃表现出较低的玻璃化转变温度，随着-SiMe 3含量的增加，玻璃化转变温度从29 °C变化到−47°C。终止的氧化物框架的有机官能团降低了网络尺寸，从而导致较低的玻璃化转变温度。
The synthesis of organic-inorganic hybrid precursors for low-melting glass has been proposed. In this process, a non-aqueous acid-base reaction of P-OH+Si-Cl→P-O-Si+HCl↑ was employed using orthophosphoric acid (H3PO4) and trimethylchlorosilane (Me3SiCl) as starting materials. The formation of P-O-SiMe3 linkage and the disappearance of P-OH group were confirmed by 29Si and 31P NMR spectra. The viscosity decrease of the precursors observed at high Si concentrations was caused by the decrease in the number of P-OH, which was correlated to the decrease of the hydrogen bond. By the use of P-O-SiMe3 linkage, low-melting glasses in the system of Me3SiO0.5-Me2SiO-SnO-P2O5 have also been prepared through the non-aqueous acid-base reaction. The hybrid glasses thus obtained exhibited low glass transition temperatures, which changed from 29 to −47°C as the -SiMe3 content increased. Termination of the oxide framework by the organic functional groups lowered the network dimension, giving rise to the lower glass transition temperature.
影响因子：
3.5
作者：
Niida, H;Takahashi, M;Yoko, T
通讯作者：
Yoko, T