| 摘要 |
A method for preparing a highly pure hafnium amide is provided to easily and safely remove zirconium component from a crude hafnium amide(a hafnium complex), thereby producing a high-purity hafnium amide with high yield. The method comprises the steps of: (a) adding a compound containing a carbonyl group or sulfonyl group and represented by the formula of A(OyXOnRf)m(in which A is H, O or Hf, X is C or S when A is H or O, X is S when A is Hf, each m, n and y is 1 when A and X respectively are H and C, m, n and y respectively are 1, 2 and 1 when A and X respectively are H and S, m, n and y respectively are 2, 1 and 0 when A is O and X is C, m, n and y respectively are 2, 2 and 0 when A is O and X is S, m, n and y respectively are 4, 2 and 1 when A is Hf, Rf is C1-12 alkyl, C1-12 perfluoroalkyl, C6-12 aryl, or C4-12 heteroaryl when A is H or O, and Rf is C1-12 perfluoroalkyl when A is Hf) to a crude hafnium amide represented by the formula of Hf[N(R1)(R2)]4(in which each R1 and R2 is independently methyl group or ethyl) and containing a zirconium component as an impurity; and (b) subjecting a product of the step(a) to a distillation under reduced pressure to remove the zirconium component from the crude hafnium amide. The method further comprises the steps of: (c) adding a lithium alkylamide represented by the formula of Li(NR3R4)(in which each of R3 and R4 is independently methyl or ethyl) to a distillate obtained by the step(b); and (d) subjecting a product of the step(c) to a distillation under reduced pressure.
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