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A simple and cost-effective method, interlayer in-situ reaction process, has been developed to produce laminated metal-intermetallic materials. Layered NiAl3 and Ni2Al3/Ni composites have been fabricated successfully by using the process. It is shown that volume friction of the intermetallic layers can be well controlled by the thickness of the metals. It is difficult to produce high strength composites if the original metals are directly exposed at high temperature. This is rectified by a pre-treating processing in which a prefect interface is formed to prevent the metals from oxidation at high temperature. The pre-treated composites have an improvement in tensile strength and thermal stability. SEM observations show that the composites exhibit a mixing fracture mode suggesting that the composites would have high toughness.