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采用共沉淀法合成了Ｎｉ／Ｆｅ摩尔比为１、２、３、６和１０的ＮｉＦｅ水滑石。热重差热结果显示ＮｉＦｅ水滑石的分解有二个过程，分别对应于２００℃和３００℃的吸热峰。经４００℃焙烧后，ＮｉＦｅ水滑石转变为具有较高表面积的ＮｉＦｅＯ混合氧化物（约１００ｍ２／ｇ），其ＸＲＤ结果仅显示ＮｉＯ的衍射峰；经８００℃焙烧后，ＮｉＦｅＯ仍有１５ｍ２／ｇ左右的表面积。穆斯堡尔谱测定表明ＮｉＦｅＯ混合氧化物较Ｆｅ２Ｏ３易还原。
NiFe hydrotalcites with Ni / Fe molar ratios of 1, 2, 3, 6 and 10 were synthesized by coprecipitation method. The thermogravimetric-differential thermal analysis shows that the decomposition of NiFe hydrotalcite has two processes, corresponding to the endothermic peaks of 200 ℃ and 300 ℃ respectively. After calcination at 400 ℃, the NiFe hydrotalcite is transformed into NiFeO mixed oxide with a high surface area (about 100m2 / g). The XRD results show only the diffraction peaks of NiO. After calcination at 800 ℃, NiFeO is still about 15m2 / g Of the surface area. Mossbauer spectroscopy shows that NiFeO mixed oxides are easier to reduce than Fe2O3.