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As a fluid a water was used, because this is a simple, low cost and ecologic substance. As a source of metal we used nitrates of metals (Al(NO3)3, Cu(NO3)2). The condition of one-step synthesis CNT-composites was changed from 370 – 450 oC, 23 – 30MPa, 0.7 – 0.005 m/l. CNT-composite materials obtained have been characterized with SEM and HRTEM. It was found the size, morphology and coating of CNT depends on time of reaction, temperature of the synthesis, pressure. Thus the increasing of time reaction and concentration of metal nitrate led to increasing of size metal oxide particles without CNT coating. It was demonstrated that CNT composites with Al2O3 can be pruduced by one step procedure.