Preparation of metal imino/amino complexes for metal oxide and metal nitride thin films
First Claim
Patent Images
1. In a process for producing a metal imino/amino complex of the formula and selected from the group consisting of R1N═
- M(NR2R3)3 and (R1N═
)2M′
(NR2R3)2 where M and M′
are pentavalent or hexavalent metals respectively;
R1 is C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl, or NR4R5 wherein R4 and R5 are independently alkyl, cycloalkenyl or R4 and R5 groups are joined in a cyclic form; and
, R2 and R3 are individually selected from C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl or R2 and R3 groups are joined in a cyclic form, the improvement which comprises;
(a) forming an intermediate complex selected from the group consisting of R1N═
MX3(DL)2 or ((R1N)2M′
X2(DL))2 by reacting a reaction mixture consisting essentially of a metal halide of the formula and selected from the group consisting of MX5 or M′
X6 with an amine consisting essentially of a primary amine of the formula H2NR1 in the presence of a donating ligand, DL, where M is a pentavalent metal and M′
is a hexavalent metal respectively, X is a halide which is selected from the group consisting of fluoride, chloride, bromide and iodide; and
R1 is as defined and then, (b) reacting the intermediate complex selected from the group consisting of R1N═
MX3(DL)2 and ((R1N)2M′
X2(DL))2 with a lithium amide of the formula LiNR2R3 where R2 and R3 are individually selected from the group consisting C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl or R2 and R3 groups are joined in a cyclic form thereby producing said metal imino/amino complex of the formula selected from the group consisting of R1N═
M(NR2R3)3 and (R1N═
)2M′
(NR2R3)2.
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Abstract
This invention relates to an improved process to produce metal imino/amino complexes having the formula R1N=M(NR2R3)3 where M is a pentavalent metal or (R1N=)2M′(NR2R3)2 where M′ is a hexavalent metal. In the process MX5 and two-equivalents of primary amine R1NH2 or metal hexahalide, M′X6 with seven-equivalents of primary amine H2NR1 are reacted in the presence of excess pyridine. The resulting reaction product R1N═MX3(py)2 or [(R1N)2M′X2(py)]2 then is followed by the addition of LiNR2R3. The process provides the final product in high yield and in high purity as well as representing a simplified procedure for synthesizing R1N═M(NR2 R3)3 or (R1N═)2M′(NR2R3)2type complexes.
413 Citations
21 Claims
-
1. In a process for producing a metal imino/amino complex of the formula and selected from the group consisting of R1N═
- M(NR2R3)3 and (R1N═
)2M′
(NR2R3)2 where M and M′
are pentavalent or hexavalent metals respectively;
R1 is C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl, or NR4R5 wherein R4 and R5 are independently alkyl, cycloalkenyl or R4 and R5 groups are joined in a cyclic form; and
, R2 and R3 are individually selected from C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl or R2 and R3 groups are joined in a cyclic form, the improvement which comprises;(a) forming an intermediate complex selected from the group consisting of R1N═
MX3(DL)2 or ((R1N)2M′
X2(DL))2 by reacting a reaction mixture consisting essentially of a metal halide of the formula and selected from the group consisting of MX5 or M′
X6 with an amine consisting essentially of a primary amine of the formula H2NR1 in the presence of a donating ligand, DL, where M is a pentavalent metal and M′
is a hexavalent metal respectively, X is a halide which is selected from the group consisting of fluoride, chloride, bromide and iodide; and
R1 is as defined and then,(b) reacting the intermediate complex selected from the group consisting of R1N═
MX3(DL)2 and ((R1N)2M′
X2(DL))2 with a lithium amide of the formula LiNR2R3 where R2 and R3 are individually selected from the group consisting C1-8 alkyl, silylalkyl, cycloalkyl, aryl, alkyl substituted aryl or R2 and R3 groups are joined in a cyclic form thereby producing said metal imino/amino complex of the formula selected from the group consisting of R1N═
M(NR2R3)3 and (R1N═
)2M′
(NR2R3)2.- View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21)
- M(NR2R3)3 and (R1N═
Specification
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Current AssigneeVersum Materials US Inc.
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Original AssigneeAir Products and Chemicals Incorporated (Linde Plc)
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InventorsLei, Xinjian, Norman, John Anthony Thomas
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Primary Examiner(s)O SULLIVAN, PETER G
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Application NumberUS10/179,818Time in Patent Office302 DaysField of Search556/42, 556/51US Class Current556/42CPC Class CodesC07F 9/005 Compounds of elements of Gr...
