| 摘要 |
PURPOSE: Provided is a massive synthesis method of high purity double-walled carbon nanotubes by sintering catalytic metal particles supported on powder and flowing C-source gas into catalytic metal particles supported powder. CONSTITUTION: The massive synthesis method of double-walled carbon nanotubes(20-40nm size) by vapor phase growth comprises the steps of: (i) supporting catalytic metal particles comprising Fe, Co, Ni, Mo or alloy thereof on nano-sized pores of powder comprising MgO, Al2O3, zeolite or silica; (ii) sintering catalytic metal-supported powder at 700-900deg.C for 6-12hrs in air atmosphere; (iii) putting catalytic metal-supported powder into a quartz(or graphite) boat in the furnace; (iv) keeping the temperature of the furnace at 700-1100deg.C; (v) supplying Ar and C-source gas comprising C2H2, CH3, C2H4 and CO to the sintered catalytic metal-supported powder, wherein the C-source comprising alcohol, benzene, hexane, tetra hydrofuran or propanol is also supplied after vaporization of the solution. The catalytic metal particles(2-5nm size) are supported on powder by the following steps of: (i) preparing catalytic metal particles-contained solution by dissolving catalytic metals such as Fe(NO3)3·9H2O, CoSO4·xH2O, NiSO4·6H2O in water; (ii) mixing the solution with support powders, wherein the mole ratio of Fe, Ni or Co : Mo : MgO is 0.7-1 : 0.1-0.3 :10-13 in case that the resultant mixed solution contains Fe, Ni or Co, Mo and MgO, the mole ratio of Fe : Ni : Mo : MgO is 0.7-1 : 0.1-0.3 : 0.1-0.3 : 10-13 in case that the mixed solution contains Fe or Ni, Mo and MgO, and the mole ratio of Fe : Co : Mo : MgO is 0.7-1 : 0.1-0.3 : 0.1-0.3 : 10-13 in case that the mixed solution contains Fe or Co, Mo and MgO; (iii) drying the mixed solution at 150deg.C for 15hrs in a vacuum oven to remove water contained in the mixed solution; (iv) grinding catalytic metal particles-contained powder. |
