METHOD AND APPARATUS FOR CHARACTERIZING METAL OXIDE REDUCTION

• US 20160111344A1
• Filed: 03/13/2015
• Published: 04/21/2016
• Est. Priority Date: 10/17/2014
• Status: Active Grant

• Current Assignee: Lam Research Corporation
• Original Assignee: Lam Research Corporation
• Inventors: Opocensky, Edward C., Spurlin, Tighe A., Reid, Jonathan D.
• Granted Patent: US 9,472,377 B2
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: C23C 8/12 using elemental oxygen or ozone
• CPC Class Codes: C23C 8/80 After-treatment
• CPC Class Codes: H01J 37/32 Gas-filled discharge tubes heating by discharge H05B
• CPC Class Codes: H01J 37/32357 Generation remote from the workpiece, e.g. down-stream
• CPC Class Codes: H01L 21/02068 during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
• CPC Class Codes: H01L 21/02244 of a metallic layer
• CPC Class Codes: H01L 21/02255 formation by thermal treatment H01L21/02252 takes precedence; after treatment of an insulating film H01L21/3105 and subgroups
• CPC Class Codes: H01L 21/324 Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering H01L21/20 - H01L21/288 and H01L21/302 - H01L21/322 take precedence
• CPC Class Codes: H01L 21/6719 characterized by the construction of the processing chambers, e.g. modular processing chambers
• CPC Class Codes: H01L 21/6723 comprising at least one plating chamber electroless plating apparatuses C23C, electroplating apparatuses C25D
• CPC Class Codes: H01L 21/76855 After-treatment introducing at least one additional element into the layer
• CPC Class Codes: H01L 21/76862 Bombardment with particles, e.g. treatment in noble gas plasmas; UV irradiation
• CPC Class Codes: H01L 21/76871 Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
• CPC Class Codes: H01L 21/76873 for electroplating
• CPC Class Codes: H01L 21/76876 for deposition from the gas phase, e.g. CVD
• CPC Class Codes: H01L 22/14 for electrical parameters, e.g. resistance, deep-levels, CV, diffusions by electrical means
• CPC Class Codes: H01L 22/20 Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
• CPC Class Codes: H01L 22/26 Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement endpoint detection arrangements in CMP apparatus B24B37/013, in discharge apparatus H01J37/32

Abstract

Method and apparatus for characterizing metal oxide reduction using metal oxide films formed in an anneal chamber are disclosed. Oxygen is provided into an anneal chamber. A substrate including a metal seed layer is exposed to the oxygen and exposed to a heated substrate support in the anneal chamber to form a metal oxide of the metal seed layer. The oxidized substrate can be stored for later use or transferred to a processing chamber for reducing the metal oxide to metal. The oxidized substrates formed in this manner provide metal oxides that are repeatable, uniform, and stable. The oxidized substrate is exposed to a reducing treatment under conditions that reduce the metal oxide to metal in the form of a film integrated with the metal seed layer.

Claims

1. A method of characterizing metal oxide reduction, the method comprising:

(a) providing oxygen into an anneal chamber;

(b) providing a substrate with a metal seed layer formed thereon in the anneal chamber;

(c) exposing the substrate to conditions for forming a metal oxide of the metal seed layer in the anneal chamber;

(d) providing the substrate in a processing chamber; and

(e) exposing the substrate to a reducing treatment under conditions that reduce the metal oxide to metal in the form of a film integrated with the metal seed layer.

2. The method of claim 1, wherein providing oxygen into the anneal chamber comprises exposing the anneal chamber to atmospheric conditions.

3. The method of claim 1, wherein providing oxygen into the anneal chamber comprises:

closing the anneal chamber from atmospheric conditions; and

flowing oxygen into the anneal chamber.

4. The method of claim 1, wherein exposing the substrate to conditions for forming the metal oxide comprises converting greater than 90% of the metal of the metal seed layer to metal oxide.

5. The method of claim 1, further comprising:

heating a substrate support in the anneal chamber, wherein the substrate is provided on the heated substrate support.

6. The method of claim 5, wherein exposing the substrate to conditions for forming the metal oxide comprises exposing the substrate to the oxygen in the anneal chamber simultaneous with exposing the substrate to the heated substrate support.

7. The method of claim 5, wherein the temperature of the heated substrate support is between about 100°

C. and about 400°

C.

8. The method of claim 1, wherein the metal seed layer has a thickness between about 100 Å

and about 400 Å

.

9. The method of claim 1, further comprising:

measuring a first sheet resistance of the substrate prior to exposing the substrate to the reducing treatment; and

measuring a second sheet resistance of the substrate after exposing the substrate to the reducing treatment.

10. The method of claim 9, further comprising:

measuring a third sheet resistance of the substrate prior to exposing the substrate to conditions for forming the metal oxide.

11. The method of claim 1, further comprising:

repeating operations (a)-(c) for each of a plurality of additional substrates prior to providing the substrate in the processing chamber.

12. The method of claim 11, further comprising:

repeating operations (d)-(e) for each of the plurality of additional substrates after exposing the substrate to the reducing treatment.

13. The method of claim 1, wherein exposing the substrate to the reducing treatment comprises:

forming a remote plasma of a reducing gas species in a remote plasma source, wherein the remote plasma comprises one or more of;

radicals, ions, and ultraviolet (UV) radiation from the reducing gas species; and

exposing the substrate to the remote plasma.

14. The method of claim 1, further comprising:

cooling the substrate prior to providing the substrate in the processing chamber but after exposing the substrate to conditions for forming the metal oxide.

15. An apparatus for characterizing metal oxide reduction, the apparatus comprising:

an anneal chamber;

a substrate support for holding a substrate in the anneal chamber, wherein the substrate includes a metal seed layer;

a processing chamber separate from the anneal chamber; and

a controller configured with instructions for performing the following operations;

(a) providing oxygen into the anneal chamber;

(b) heating the substrate support in the anneal chamber;

(c) exposing the substrate to the heated substrate support and to the oxygen to form a metal oxide of the metal seed layer in the anneal chamber;

(d) transferring the substrate to the processing chamber; and

(e) exposing the substrate to a reducing treatment under conditions that reduce the metal oxide to metal in the form of a film integrated with the metal seed layer.

16. The apparatus of claim 15, wherein providing oxygen into the anneal chamber comprises exposing to the anneal chamber to atmospheric conditions.

17. The apparatus of claim 15, further comprising:

a door configured to open and close the anneal chamber; and

a gas inlet for delivering oxygen into the anneal chamber, wherein providing oxygen into the anneal chamber comprises flowing oxygen into the anneal chamber when anneal chamber is closed.

18. The apparatus of claim 15, wherein greater than about 90% of the metal of the metal seed layer is converted to the metal oxide after exposing the substrate to the heated substrate support and to the oxygen.

19. The apparatus of claim 15, wherein the controller further comprises instructions for:

measuring a first sheet resistance of the substrate prior to exposing the substrate to the reducing treatment; and

measuring a second sheet resistance of the substrate after exposing the substrate to the reducing treatment.

20. The apparatus of claim 15, wherein the controller further comprises instructions for:

repeating operations (a)-(c) for each of a plurality of additional substrates prior to transferring the substrate to the processing chamber; and

repeating operations (d)-(e) for each of the plurality of additional substrates after exposing the substrate to the reducing treatment.

21. The apparatus of claim 15, further comprising:

a remote plasma source coupled to the processing chamber, wherein exposing the substrate to the reducing treatment comprises;

forming a remote plasma of a reducing gas species in the remote plasma source, wherein the remote plasma comprises one or more of;

radicals, ions, and ultraviolet (UV) radiation from the reducing gas species; and

exposing the substrate to the remote plasma.