Patent US5591483A successfully refreshed from Google Patents.
US5591483A
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Process for the preparation of metal nitride coatings from single source precursors
Assignee: Wayne State University
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Filing: 1994-08-31
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Granted: 1997-01-07
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Expires: 2014-08-31
Abstract
Abstract Metal nitride coatings are deposited effectively by the decomposition of single source metal imido-amidoamine precursors perpared by the reaction of a pentavalent metal halide with a primary amine or hydrazine. With hydrazine-derived precursors, TaN coatings may be deposited at temperatures as low as 400 degrees Celcius or lower.
Inventors
- 👤 Charles H. Winter
- 👤 T. Suren Lewkebandara
- 👤 Kumudini C. Jayaratne
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 02:41
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/22; C23C16/30; C23C16/34
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
259 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor i) the reaction product of a primary amine of the formula NH 2 --R with a metal halide of the formula MX 5 where X is fluorine, chlorine, bromine, or iodine, or ii) the reaction product of a primary amine of the formula NH 2 --NR 1 R 2 with a metal halide of the formula MX 4 where X is fluorine, chlorine, bromine, or iodine; where M is a metal; where R is selected from the group consisting of C 1-8 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-8 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; b) subliming said precursor at a pressure of from 0.0001 mm Hg to about 760 mm Hg; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 2
Dependent Claim
259 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor i) the reaction product of a primary amine of the formula NH 2 --R with a metal halide of the formula MX 5 where X is fluorine, chlorine, bromine, or iodine, or ii) the reaction product of a primary amine of the formula NH 2 --NR 1 R 2 with a metal halide of the formula MX 4 where X is fluorine, chlorine, bromine, or iodine; where M is a metal; where R is selected from the group consisting of C 1-8 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-8 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; b) subliming said precursor at a pressure of from 0.0001 mm Hg to about 760 mm Hg; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 3
Dependent Claim
16 words
The process of claim 1 wherein said primary amine is a C 1-4 alkyl primary amine.
Claim 4
Dependent Claim
9 words
The process of claim 1 wherein X is Cl.
Claim 5
Dependent Claim
21 words
The process of claim 1 wherein said substrate is heated to a temperature of about 300° C. to about 1000° C.
Claim 6
Dependent Claim
26 words
The process of claim 1 wherein said primary amine has the formula: NH.sub.2 --NR.sup.1 R.sup.2 where R 1 and R 2 are C 1-4 lower alkyl.
Claim 7
Dependent Claim
9 words
The process of claim 5 wherein X is Cl.
Claim 8
Dependent Claim
20 words
The process of claim 5 wherein said substrate is heated to a temperature of about 400° C. to 500° C.
Claim 9
Dependent Claim
17 words
The process of claim 1 wherein said coating is formed at a rate greater than 10 Å/s.
Claim 10
Dependent Claim
22 words
The process of claim 8 wherein said substrate is maintained at a temperature of from about 400° C. to about 600° C.
Claim 11
Dependent Claim
206 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor a complex of the formula: [MX.sub.2 (NR)(NHR)(NH.sub.2 R)].sub.n where M is Nb or Ta; where X is fluorine, chlorine, bromine, or iodine; where R is selected from the group consisting of C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; and where n is a whole number from 1-3; b) subliming said precursor; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 12
Dependent Claim
206 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor a complex of the formula: [MX.sub.2 (NR)(NHR)(NH.sub.2 R)].sub.n where M is Nb or Ta; where X is fluorine, chlorine, bromine, or iodine; where R is selected from the group consisting of C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; and where n is a whole number from 1-3; b) subliming said precursor; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 13
Dependent Claim
12 words
The process of claim 10 wherein R is C 1-4 lower alkyl.
Claim 14
Dependent Claim
9 words
The process of claim 10 wherein R is t-butyl.
Claim 15
Dependent Claim
21 words
The process of claim 10 where R is --NR.sup.1 R.sup.2 wherein R 1 and R 2 are C 1-4 lower alkyl.
Claim 16
Dependent Claim
20 words
The process of claim 13 wherein said substrate is heated to a temperature of 300° C. to about 600° C.
Claim 17
Dependent Claim
17 words
The process of claim 13 wherein said substrate is heated to a temperature of about 400° C.
Claim 18
Dependent Claim
20 words
The process of claim 13 wherein said complex is [MCl 2 (NNMe 2 )(NHNMe 2 )(NH 2 NMe 2 )].
Claim 19
Dependent Claim
17 words
The process of claim 10 wherein said coating is formed at a rate greater than 10 Å/s.
Claim 20
Dependent Claim
22 words
The process of claim 17 wherein said substrate is maintained at a temperature of from about 400° C. to about 600° C.
Claim 21
Dependent Claim
174 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor a complex of the formula: [M'X.sub.2 (NNR.sup.1 R.sup.2)(NH.sub.2 NR.sup.1 R.sup.2)].sub.n where M' is a metal; where X is fluorine, chlorine, bromine, or iodine; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals, where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; and where n is a whole number from 1-3; b) subliming said precursor; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 22
Dependent Claim
174 words
A process for coating a substrate with a coating of metal nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor a complex of the formula: [M'X.sub.2 (NNR.sup.1 R.sup.2)(NH.sub.2 NR.sup.1 R.sup.2)].sub.n where M' is a metal; where X is fluorine, chlorine, bromine, or iodine; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals, where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; and where n is a whole number from 1-3; b) subliming said precursor; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to metal nitride, whereby said coating of metal nitride is formed on said substrate.
Claim 23
Dependent Claim
18 words
The process of claim 19 wherein M is selected from the group consisting of Ti, Zr, and Hf.
Claim 24
Dependent Claim
17 words
The process of claim 19 wherein said coating is formed at a rate greater than 10 Å/s.
Claim 25
Dependent Claim
22 words
The process of claim 21 wherein said substrate is maintained at a temperature of from about 400° C. to about 600° C.
Claim 26
Dependent Claim
17 words
The process of claim 21 wherein said substrate is maintained at a temperature of about 400° C.
Claim 27
Dependent Claim
254 words
A process for coating a substrate with a coating of tantalum nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor i) the reaction product of a primary amine of the formula NH 2 --R with a tantalum halide of the formula MX 5 where X is fluorine, chlorine, bromine, or iodine, or ii) the reaction product of a primary amine of the formula NH 2 --NR 1 R 2 with a tantalum halide of the formula MX 4 where X is fluorine, chlorine, bromine, or iodine; where R is selected from the group consisting of C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; b) subliming said precursor at a pressure of from 0.0001 mm Hg to about 760 mm Hg; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to tantalum nitride, whereby said coating of tantalum nitride is formed on said substrate.
Claim 28
Dependent Claim
254 words
A process for coating a substrate with a coating of tantalum nitride by chemical vapor deposition from a single source precursor, comprising: a) selecting as said precursor i) the reaction product of a primary amine of the formula NH 2 --R with a tantalum halide of the formula MX 5 where X is fluorine, chlorine, bromine, or iodine, or ii) the reaction product of a primary amine of the formula NH 2 --NR 1 R 2 with a tantalum halide of the formula MX 4 where X is fluorine, chlorine, bromine, or iodine; where R is selected from the group consisting of C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, C 6-10 aryl radicals, --NR 1 R 2 , and mixtures thereof; where R 1 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; where R 2 is selected from the group consisting of hydrogen, C 1-18 alkyl, C 3-8 cycloalkyl, C 2-18 alkenyl, C 3-8 cycloalkenyl, and C 6-10 aryl radicals; or where R 1 and R 2 together with N form a cyclic C 2-8 saturated or C 3-8 unsaturated imine; b) subliming said precursor at a pressure of from 0.0001 mm Hg to about 760 mm Hg; and c) contacting said sublimed precursor with a substrate maintained at a temperature sufficient to effect decomposition of said precursor to tantalum nitride, whereby said coating of tantalum nitride is formed on said substrate.
References Cited (Backward Citations)
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