Mechanical activation has been found to be a very effective method of inducing reaction. In this paper, a mixture of ilmenite and graphite with a molar ratio of 1 to 3similar to4 was ball milled at room temperature and subsequently annealed. The enhanced carbothermic reactions were monitored by thermogravimetric analysis and X-ray diffraction analysis. A series of reduction reactions occurs with a higher reaction rate in a temperature range lower than that without pre-milling. A longer milling time leaded to a lower reaction temperature and less intermediate phases. When the milled powder was heated in a tube furnace to a temperature range between 1300 degreesC and 1400 degreesC for 2similar to6 hours under a cheap mixed gas containing nitrogen, the composite powder of iron and Ti(C,N) without intermediate phases was achieved.