采用ＥＸＡＦＳ方法研究了负载型Ｎｉ／ＳｉＯ２的区域结构和机械合金化方法扩展ＦｅＣｕ金属固溶范围，并形成纳米尺寸的非平衡亚稳态合金．实验结果表明，利用实验室ＥＸＡＦＳ方法也可以开展较好的结构测量研究，但必须选用合适的靶材、工作电压电流、单色器晶体、狭缝、脉冲高度分析器基线和道宽等．在实验室ＥＸＡＦＳ测量中，分辨能力是获得正确结果的关键． The EXAFS method was used to study the structure of the supported Ni / SiO2 and the mechanical alloying method to broaden the range of FeCu metal solution and to form nano-sized non-equilibrium metastable alloy. Experimental results show that the use of laboratory EXAFS method can also be a good structural measurement studies, but must choose the right target, voltage and current, monochromator crystals, slits, pulse height analyzer baseline and width and so on. In laboratory EXAFS measurements, resolving power is the key to getting the right result.