IP Library Granted Patent US 6,972,239
Granted Patent B1
US 6,972,239 · App. 10/923,529 · Granted Dec 6, 2005

Low temperature MOCVD processes for fabrication of Pr

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Quick Facts
Patent No.
US 6,972,239
App. No.
10/923,529
Granted
Dec 6, 2005
Kind
B1
Abstract

A method of fabricating a PCMO thin film at low temperature for use in a RRAM device includes preparing a PCMO precursor; preparing a substrate; placing the substrate into a MOCVD chamber; introducing the PCMO precursor into the MOCVD chamber to deposit a PCMO thin film on the substrate; maintaining a MOCVD vaporizer at between about 240° C. to 280° C. and maintaining the MOCVD chamber at a temperature of between about 300° C. to 400° C.; removing the PCMO thin-film bearing substrate from the MOCVD chamber; and completing the RRAM device.

Claims (33)

1. A method of fabricating a PCMO thin film at low temperature for use in a RRAM device, comprising:

preparing a PCMO precursor;

preparing a substrate;

placing the substrate into a MOCVD chamber;

introducing the PCMO precursor into the MOCVD chamber to deposit a PCMO thin film on the substrate;

maintaining a MOCVD vaporizer at between about 240° C. to 280° C. and maintaining the MOCVD chamber at a temperature of between about 300° C. to 400° C.;

removing the PCMO thin-film bearing substrate from the MOCVD chamber; and

completing the RRAM device.

2. The method of claim 1 wherein said preparing a PCMO precursor includes dissolving solid organometallic compounds including Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 , where thd is C 11 H 19 O 2 , in organic solvents butylether and tetraglyme, wherein a 1N metal of each Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 has a ratio of between about 0.9:0.6:1, and are separately dissolved in a mixed solvent of butyl ether and tetraglyme in the volume ratio of 3:1, resulting in a precursor solution having a concentration of 0.1 M/L of metals for each of the Pr, Ca and Mn precursors.

3. The method of claim 1 wherein said preparing a substrate includes preparing a substrate taken from the group of substrates consisting of Pt/Ti/SiO 2 /Si and Ir/Ti/SiO 2 /Si, and dip etching the selected substrate in HF having a 50:1 dilution with water for about 20 seconds.

4. The method of claim 1 wherein the MOCVD chamber is maintained with an oxygen partial pressure of between about 20% to 30%, the temperature of the feed line is set between about 240° C. to 280° C., the pressure in the deposition chamber is maintained at between about 1 torr. to 5 torr, and wherein the precursor solution has a delivery rate, into the MOCVD chamber of between about 0.1 ml/min to 0.5 ml/min, for a deposition process time of between about 20 minutes to 60 minutes.

5. The method of claim 1 which includes annealing the PCMO thin film at a temperature of between about 500° C. to 600° C. for about five minutes.

6. A method of fabricating a nucleated PCMO thin film at low temperature for use in a RRAM device, comprising:

preparing a PCMO precursor, including dissolving solid organometallic compounds including Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 , where thd is C 11 H 19 O 2 , in organic solvents butylether and tetraglyme, wherein a 1N metal of each Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 has a ratio of between about 0.9:0.6:1, and are separately dissolved in a mixed solvent of butyl ether and tetraglyme in the volume ratio of 3:1, resulting in a precursor solution having a concentration of 0.1 M/L of metals for each of the Pr, Ca and Mn precursors;

preparing a substrate;

placing the substrate into a MOCVD chamber;

introducing the PCMO precursor into the MOCVD chamber to deposit a PCMO thin film on the substrate;

maintaining a MOCVD vaporizer at between about 240° C. to 280° C. and maintaining the MOCVD chamber at a temperature of between about 300° C. to 400° C.;

annealing the PCMO thin film at a temperature of between about 500° C. to 600° C. for about five minutes;

removing the nucleated PCMO thin-film bearing substrate from the MOCVD chamber; and

completing the RRAM device.

7. The method of claim 6 wherein said preparing a substrate includes preparing a substrate taken from the group of substrates consisting of Pt/Ti/SiO 2 /Si and Ir/Ti/SiO 2 /Si, and dip etching the selected substrate in HF having a 50:1 dilution with water for about 20 seconds.

8. The method of claim 6 wherein the MOCVD chamber is maintained with an oxygen partial pressure of between about 20% to 30%, the temperature of the feed line is set between about 240° C. to 280° C., the pressure in the deposition chamber is maintained at between about 1 torr. to 5 torr, and wherein the precursor solution has a delivery rate, into the MOCVD chamber of between about 0.1 ml/min to 0.5 ml/min, for a deposition process time of between about 20 minutes to 60 minutes.

9. A method of fabricating a PCMO thin film at low temperature for use in a RRAM device, comprising:

preparing a PCMO precursor;

preparing a substrate, including preparing a substrate taken from the group of substrates consisting of Pt/Ti/SiO 2 /Si and Ir/Ti/SiO 2 /Si, and dip etching the selected substrate in HF having a 50:1 dilution with water for about 20 seconds;

placing the substrate into a MOCVD chamber;

introducing the PCMO precursor into the MOCVD chamber to deposit a PCMO thin film on the substrate;

maintaining a MOCVD vaporizer at between about 240° C. to 280° C. and maintaining the MOCVD chamber at a temperature of between about 300° C. to 400° C., wherein the MOCVD chamber is maintained with an oxygen partial pressure of between about 20% to 30%, the temperature of the feed line is set between about 240° C. to 280° C., the pressure in the deposition chamber is maintained at between about 1 torr. to 5 torr, and wherein the precursor solution has a delivery rate, into the MOCVD chamber of between about 0.1 ml/min to 0.5 ml/min, for a deposition process time of between about 20 minutes to 60 minutes;

annealing the PCMO thin film at a temperature of between about 500° C. to 600° C. for about five minutes;

removing the PCMO thin-film bearing substrate from the MOCVD chamber; and

completing the RRAM device.

10. The method of claim 9 wherein said preparing a PCMO precursor includes dissolving solid organometallic compounds including Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 , where thd is C 11 H 19 O 2 , in organic solvents butylether and tetraglyme, wherein a 1N metal of each Pr(thd) 3 Ca(thd) 2 , Mn(thd) 3 has a ratio of between about 0.9:0.6:1, and are separately dissolved in a mixed solvent of butyl ether and tetraglyme in the volume ratio of 3:1, resulting in a precursor solution having a concentration of 0.1 M/L of metals for each of the Pr, Ca and Mn precursors.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 15, 2013
From: INTELLECTUAL PROPERTIES I KFT.
To: XENOGENIC DEVELOPMENT LIMITED LIABILITY COMPANY
Reel/Frame 029632/0534 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 7, 2013
From: SHARP KABUSHIKI KAISHA
To: INTELLECTUAL PROPERTIES I KFT.
Reel/Frame 029574/0933 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 26, 2012
From: SHARP LABORATORIES OF AMERICA INC.
To: SHARP KABUSHIKI KAISHA
Reel/Frame 028443/0637 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 20, 2004
From: LI, TINGKAI; ZHUANG, WEI-WEI; CHARNESKI, LAWRENCE J.; EVANS, DAVID R.; HSU, SHENG TENG
To: SHARP LABORATORIES OF AMERICA, INC.
Reel/Frame 015716/0435 →