采用共沉淀法制备二元氢氧化铜锌硝酸盐(CZL)和氢氧化镍锌硝酸盐(NZL),考察了p H和Cu/Zn(Ni/Zn)原料摩尔配比对其晶体结构的影响,并通过XRD、FTIR和TG-DTA对其结构和热稳定性进行表征。结果发现,NZL的热稳定性明显高于CZL。在此基础上,分别采用共沉淀法和离子交换法制备阴离子十二烷基硫酸钠(DS)和两性十二烷基二甲基羧基甜菜碱(DCB)表面活性剂插层CZL和NZL插层材料,并采用XRD和FTIR表征其结构,结果表明,采用离子交换和共沉淀法均可合成晶型单一且结构完整的NZL-DS;采用共沉淀法可合成晶型单一的NZL-DCB结构;采用离子交换和共沉淀法均可合成两种晶型的CZL-DS,且离子交换法不能完全取代层间的NO-3;采用离子交换法不能合成NZL-DCB和CZL-DCB,这与DCB的带电性弱有关。 CZL and NZL were prepared by co-precipitation method. The effects of mole ratio of p H and Cu / Zn (Ni / Zn) on its crystal structure were investigated. , And its structure and thermal stability were characterized by XRD, FTIR and TG-DTA. The results showed that, NZL thermal stability was significantly higher than CZL. On this basis, the cationic sodium dodecyl sulfate (DS) and amphipathic dimethylcarboxybetaine (DCB) surfactant intercalation CZL and NZL intercalation were prepared by coprecipitation and ion exchange methods, respectively XRD and FTIR. The results show that NZL-DS with single crystal structure and complete structure can be synthesized by ion exchange and coprecipitation method. NZL-DCB with single crystal structure can be synthesized by coprecipitation method. The CZL-DS of both crystal forms can be synthesized by both ion exchange and coprecipitation methods, and the ion exchange method can not completely replace the inter-layer NO-3. The ion exchange method can not synthesize NZL-DCB and CZL-DCB, The charge is weak.