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1. WO2013006242 - ATOMIC LAYER DEPOSITION OF TRANSITION METAL THIN FILMS

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[ EN ]

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WHAT IS CLAIMED IS:

1. A method of forming a metal film on a substrate, the method comprising a deposition cycle including:

a) contacting a substrate with a vapor of a metal-containing compound described by formula 1 for a first predetermined pulse time to form a first modified surface:

M Ln (1)

wherein:

n is 1 to 8;

M is a transition metal;

L is a ligand;

b) contacting the first modified surface with an acid for a second predetermined pulse time to form a second modified surface; and

c) contacting the second modified surface with a reducing agent for a third predetermined pulse time to form a metal layer.

2. The method of claim 1 wherein M is a transition metal in the +2 oxidation state.

3. The method of claim 1 wherein M is silver, palladium, platinum, rhodium, iridium, cobalt, ruthenium, manganese, nickel, or copper.

4. The method of claim 1 wherein M is copper.

5. The method of claim 1 wherein the acid is formic acid.

6. The method of claim 1 wherein the acid comprises a component selected from the group consisting of:

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hydrogen,

7. The method of claim 1 wherein the pKa of the conjugate acid to L is larger than the pKa of the acid used in step b).

8. The method of claim 1 wherein the acid comprises a component selected from the group consisting of: HX, H3PO4, and H3PO2; and X is N3", NO3", and halide.

9. The method of claim 1 wherein the reducing agent is selected from the group consisting of hydrazine, hydrazine hydrate, alkyl hydrazines, 1,1 -dialkylhydrazines, 1,2-dialkylhydrazines, ¾, ¾ plasma, ammonia, ammonia plasma, silanes, disilanes, trisilanes, germanes, diborane, formalin, amine borane, dialkyl zinc, alkyl aluminum, alkyl gallium, alkyl indium complexes, and other plasma-based gases, and combinations thereof.

10 The method of claim 1 wherein each L independently comprises a component selected from the group consisting of a two electron ligand, a multidentate ligand, charged ligand (e.g., -1 charged), a neutral ligand, and combinations thereof.

11. The method of claim 1 wherein two L ligands are combined together as part of a bidentate ligand.

12 . The method of claim 11 wherein the bidentate ligand is dimethylamino-2-propoxide.

13. The method of claim 1 wherein L is selected from the group consisting of:

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, Si(R3)3, or vinyl; and R is Ci_8 alkyl.

14. The method of claim 1 wherein L is selected from the group consisting of:



independently hydrogen, Ci_4 alkyl, C6-12 aryl, Si(R3)3, or vinyl; and R3 is Ci_s alkyl.

15. The method of claim 1 wherein L is selected from the group consisting of: 11-1051


independently hydrogen, Ci_4 alkyl, C6-i2 aryl, Si(R3)3, or vinyl; and R3 is Ci_8 alkyl.

1 wherein L is:


; R is hydrogen, Ci_4 alkyl, C6-i2 aryl, Si(R )3, or vinyl; and

R3 is Ci_8 alkyl.

17. The method of claim 1 wherein the deposition cycle is repeated a plurality of times to form a predetermined thickness of the metal film.

18. The method of claim 1 wherein the deposition cycle is repeated a plurality of times to form a metal film having a thickness from about 5 nanometers to about 300 nanometers.

19. A method of forming a metal film on a substrate, the method comprising a deposition cycle including:

a) contacting a substrate with a vapor of a metal-containing compound described by formula 1 for a first predetermined pulse time to form a first modified surface:

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M Ln (1)

wherein:

n is 1 to 8;

M is a transition metal;

L is a ligand;

b) contacting the first modified surface with an acid for a second predetermined pulse time to form a second modified surface, the pKa of the conjugate acid to L is larger than the pKa of the acid used in this step; and

c) contacting the second modified surface with a reducing agent for a third predetermined pulse time to form a metal layer, the deposition cycle being repeated a plurality of times to form a metal film having a thickness from about 5 nanometers to about 300 nanometers.

20 . The method of claim 19 wherein L is selected from the group consisting of:

dimethylamino-2-propoxide,

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hydride, and


R, R1, R2 are each independently hydrogen, Ci_4 alkyl, C6-i2 aryl, Si(R3)3, or vinyl; and R3 is Ci_ alkyl;

the acid in step b) is selected from the group consisting of: formic acid,

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H3P02 ;

X is N3~, N03", and halide; R is hydrogen, Ci alkyl, C6-i2 aryl, Si(R )3, or vinyl; R is Ci alkyl. and n is an integer from 1 to 6; and

the reducing agent is selected from the group consisting of hydrazine, hydrazine hydrate, alkyl hydrazines, 1 ,1-dialkylhydrazines, 1 ,2-dialkylhydrazines, H2, H2 plasma, ammonia, ammonia plasma, silanes, disilanes, trisilanes, germanes, diborane, formalin, amine borane, dialkyl zinc, alkyl aluminum, alkyl gallium, alkyl indium complexes, and other plasma-based gases, and combinations thereof.