Synthesis of titanium nitride films

Claim 1

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate, in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution containing hydrolyzed and condensed titanium alkoxide to the surface of a substrate at a substantially ambient temperature to provide a titanium containing gel-film on the surface of the substrate; and heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.

Claim 2

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate, in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution containing hydrolyzed and condensed titanium alkoxide to the surface of a substrate at a substantially ambient temperature to provide a titanium containing gel-film on the surface of the substrate; and heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.

Claim 20

A method according to claim I wherein the step of applying a solution containing titanium alkoxide to the surface of a substrate comprises the step of applying the solution to the surface of a polymer substrate.

Claim 22

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution of hydrolyzed and condensed titanium alkoxide in solvent, in which the titanium alkoxide has the formula Ti(OR) 4 , wherein R is an alkyl group having 1 to 6 carbon atoms, and in which the solvent is selected from the group consisting of aliphatic, cycloaliphatic and aromatic compounds containing from 1 to 20 carbon atoms and at least one functional group consisting of ether and hydroxyl, to the surface of a substrate at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate; and heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.

Claim 23

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution of hydrolyzed and condensed titanium alkoxide in solvent, in which the titanium alkoxide has the formula Ti(OR) 4 , wherein R is an alkyl group having 1 to 6 carbon atoms, and in which the solvent is selected from the group consisting of aliphatic, cycloaliphatic and aromatic compounds containing from 1 to 20 carbon atoms and at least one functional group consisting of ether and hydroxyl, to the surface of a substrate at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate; and heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.

Claim 32

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices on the surface of a substrate, the method comprising: applying a solution containing a hydrolyzed and condensed titanium alkoxide in solvent, in which the titanium alkoxide has the formula Ti(OR) 4 , wherein R is an alkyl having 1 to 6 carbon atoms, and in which the solvent is selected from the group consisting of aliphatic, cycloaliphatic and aromatic compounds containing from 1 to 20 carbon atoms and at least one functional group consisting of ether and hydroxyl, to the surface of a substrate at a substantially ambient temperature to provide a titanium-containing gel-film on the surface of the substrate; predensifying the titanium containing gel-film on the surface of a substrate upon which the titanium containing solution has been applied; cooling the predensified gel-film on the surface of the substrate to substantially ambient temperature; heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C. and at a rate of temperature change of at least about 50° C. per minute; maintaining the heated substrate at the temperature to which it is heated for at least about thirty minutes to about six hours; and cooling the heated substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of temperature change used to heat the substrate.

Claim 33

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices on the surface of a substrate, the method comprising: applying a solution containing a hydrolyzed and condensed titanium alkoxide in solvent, in which the titanium alkoxide has the formula Ti(OR) 4 , wherein R is an alkyl having 1 to 6 carbon atoms, and in which the solvent is selected from the group consisting of aliphatic, cycloaliphatic and aromatic compounds containing from 1 to 20 carbon atoms and at least one functional group consisting of ether and hydroxyl, to the surface of a substrate at a substantially ambient temperature to provide a titanium-containing gel-film on the surface of the substrate; predensifying the titanium containing gel-film on the surface of a substrate upon which the titanium containing solution has been applied; cooling the predensified gel-film on the surface of the substrate to substantially ambient temperature; heating the substrate in an ammonia atmosphere to a temperature of at least about 700° C. and at a rate of temperature change of at least about 50° C. per minute; maintaining the heated substrate at the temperature to which it is heated for at least about thirty minutes to about six hours; and cooling the heated substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of temperature change used to heat the substrate.

Claim 34

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution containing hydrolyzed and condensed titanium (IV) ethoxide and t-butanol to the surface of a substrate at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate; predensifying the titanium containing gel-film on the surface of a substrate upon which the titanium containing solution has been applied by heating the substrate to a temperature of from about 400° C. to about 900° C. by rapid thermal annealing so that the rate of temperature change exceeds about 1000° C. per minute in hydrogen gas; cooling the heated predensified gel-film on the surface of the substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of heating; heating the substrate in an ammonia atmosphere to a temperature of at least about 900° C. and at a rate of temperature change of at least about 70° C. per minute; maintaining the heated substrate at the temperature to which it is heated for between about thirty minutes and one hour; and cooling the heated substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of temperature change used to heat the substrate.

Claim 35

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: applying a solution containing hydrolyzed and condensed titanium (IV) ethoxide and t-butanol to the surface of a substrate at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate; predensifying the titanium containing gel-film on the surface of a substrate upon which the titanium containing solution has been applied by heating the substrate to a temperature of from about 400° C. to about 900° C. by rapid thermal annealing so that the rate of temperature change exceeds about 1000° C. per minute in hydrogen gas; cooling the heated predensified gel-film on the surface of the substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of heating; heating the substrate in an ammonia atmosphere to a temperature of at least about 900° C. and at a rate of temperature change of at least about 70° C. per minute; maintaining the heated substrate at the temperature to which it is heated for between about thirty minutes and one hour; and cooling the heated substrate to substantially ambient temperature at a rate of temperature change substantially equal to the rate of temperature change used to heat the substrate.

Claim 36

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: heating a substrate upon which a hydrolyzed and condensed solution containing titanium has been applied at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate, and in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.

Claim 37

A method of producing a substantially stoichiometric film of titanium nitride on the surface of a substrate in which the film is particularly suitable for diffusion barriers and planarization and interconnect materials in electronic devices, the method comprising: heating a substrate upon which a hydrolyzed and condensed solution containing titanium has been applied at a substantially ambient temperature to provide a gel-film containing titanium on the surface of the substrate, and in an ammonia atmosphere to a temperature of at least about 700° C., and at a rate of temperature change of at least about 50° C. per minute for a time sufficient to form a substantially stoichimetric film of titanium nitride.