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Study on the coating of nano-scale SiO_2 film on the surface of nanocrystalline Mg-Al layered double hydroxides

Science china {1. 2005年第2期48卷 107-114页

作者： zhang zejiang1,2,3, mei xiujuan2, xu chenghua1 & qiu fali1 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. Sichuan Fire Research institute of Public Security Ministry, chengdu 611830, china 3. Graduate School of the chinese academy of sciences, Beijing 100039, china Correspondence should be addressed to zhang zejiang (email: zzjzzjzz@***) 1. chengdu {1. of organic chemistry Chinese Academy of Sciences 610041 Chengdu China 2. Sichuan Fire Research institute of Public Security Ministry 611830 Chengdu China 3. Graduate School of the chinese academy of sciences 100039 Beijing China

The coating process of a nano-scale SiO2 film on the nanocrystalline Mg-Al layered double hydroxides via a sol-gel process was investigated. The uniform and dense SiO2film with a thickness of about 5 nm on the nano-LDHs particles was characterized by the solubility test in the dilute HNO3 or HCl acid, TEM and FT-IR, XRD, TG and DSC. The chemical shifts of binding en- ergies of Al 2p, Mg 2p, Si 2s and O 1. on the coated particles indicate that the coating of the SiO2 nano-film on the surface of the nano-LDHs proceeds through the formation of Mg-O-Si and Al-O-Si bonds. The thermal analysis shows that both the SiO2-coated nano-LDHs and the nano-LDHs have a similar mass loss process, in which there are three obvious stages of mass loss in the temperature range of 40—700℃. Furthermore, the more the coatedamount of SiO2on the surface of the nano-LDHs is, the less the mass loss of the samples is at 700℃.The nano- LDHs have two obvious endothermic peaks at 244.67℃ and 430.1.℃, whose corresponding heat absorption capacities are 41..28 J/g and 336.30 J/g, respectively. In contrast, the coated nano-LDHs have only one endothermic peak at 243.60℃ with a heat absorption capacity of 221.25 J/g.

关键词： layered double hydroxides, nanocrystalline, silica, coating.

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Study on fire-retardant nanocrystalline Mg-Al layered double hydroxides synthesized by microwavecrystallization method

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Science china {1. 2004年第6期47卷 488-498页

作者： zhang zejiang1, xu chenghua1, qiu fali1, mei xiujuan2, LAN Bin2 & zhang Shuosheng2 1. chengdu institute of organic chemistry, chinese academy of sciences, chengdu 610041, china 2. Sichuan Fire Research institute of Public Safety Ministry, chengdu 611830, china 1. chengdu {1. of organic chemistry Chinese Academy of Sciences 610041 Chengdu China 2. Sichuan Fire Research institute of Public Safety Ministry 611830 Chengdu China

Nanocrystalline Mg-Al layered double hydroxides with the particle size being 1.—40 nm were firstly prepared by the technology of the microwave-crystallization and the vari- able-speed addition of the alkali. The obtained samples were characterized by TEM and XRD. The roles of the microwave and addition rate of the alkali were also discussed in the present work. The thermal decomposition activation energy of the nano-LDHs was calculated according to their TG, DTG and DSC curves by the Ozawa method. The results showed that the thermal decom- position of the nano-LDHs had four steps. Thereby the decomposition model of the nano-LDHs was supposed according to the analysis of their thermal decomposition. After PS, ABS, HDPE and PVC were filled with the nano-LDHs, their LOI values could be increased up to 28, 27, 26 and 33, respectively. When the fire-retardant coating contained 1.9% of the nano-LDHs that was 0.27 times the dosage of the conventional TiO2, its fire endurance time reached 32.75min that was 7.05 min longer than that of the best coating containing TiO2 according to the model big-panel combustion test method.

关键词： layered double hydroxides, nanocrystal, microwave synthesis, thermal decomposition, fire-retardant performance.

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