Method of manufacturing silicided silicon microtips for scanning probe microscopy

• US 6,139,759 A
• Filed: 02/23/1999
• Issued: 10/31/2000
• Est. Priority Date: 07/08/1997
• Status: Expired due to Fees

• Current Assignee: International Business Machines Corporation
• Original Assignee: International Business Machines Corporation
• Inventors: Slinkman, James A., Moszkowicz, Leon, Kaszuba, Philip V., Never, James M., Doezema, Lambert A.
• Primary Examiner(s): Gulakowski, Randy
• Assistant Examiner(s): OLSEN, ALLAN W
• Application Number:
  US09/256,261
• Time in Patent Office: 616 Days
• Field of Search: 216/11, 216/13, 257/10
• US Class Current: 216/11
• CPC Class Codes: B82Y 35/00 Methods or apparatus for measurement or analysis of nanostructures
• CPC Class Codes: G01Q 60/30 Scanning potential microscopy
• CPC Class Codes: G01Q 60/40 Conductive probes
• CPC Class Codes: Y10S 977/879 Material

Abstract

A micromechanical sensor probe for a scanned-probe tool comprising a silicon probe and a coating of a refractory metal silicide formed at least on the tip of the probe. Titanium silicide is preferred. A method for manufacturing such a probe includes the steps of, first, providing a silicon cantilever and tip combination and, second, forming a refractory metal silicide on at least the tip of the cantilever and tip combination. This second step of the method includes removing any remnant oxide from the tip, stabilizing the cantilever and tip combination on a carrier, depositing a refractory metal on the silicon tip, heating the cantilever and tip combination in an ambient free of oxygen to react chemically the refractory metal on and the silicon of the tip, selectively etching any unreacted refractory metal from the tip, and annealing the cantilever and tip combination in an ambient free of oxygen. The method may also include, as a final step, removing any unreacted refractory metal from the tip.

Claims

1. A method for manufacturing a micromechanical sensor probe for a scanned-probe tool comprising the steps of:

(a) providing a silicon cantilever and tip combination; and

(b) forming a refractory metal silicide on at least the tip of the cantilever and tip combination by;

(b1) removing any remnant oxide from the tip;

(b2) stabilizing the cantilever and tip combination on a carrier;

(b3) depositing a refractory metal on the silicon tip;

(b4) heating the cantilever and tip combination in an ambient free of oxygen to react chemically the refractory metal on and the silicon of the tip;

(b5) selectively etching and removing any unreacted refractory metal from the tip; and

(b6) annealing the cantilever and tip combination in an ambient free of oxygen.

2. The method of claim 1 wherein the step (b1) of removing any remnant oxide from the tip includes cleaning the tip with a 10:

1, buffered hydrofluoric acid solution.

3. The method of claim 1 wherein the step (b2) of stabilizing the cantilever and tip combination on a carrier involves using a non-volatile one of a glue and a tape affixing the cantilever and tip combination to the carrier.

4. The method of claim 1 wherein, in the step (b2), a plurality of cantilever and tip combinations are stabilized on the carrier for simultaneous processing.

5. The method of claim 1 further comprising, during the step (b3) of depositing a refractory metal on the silicon tip, introducing a partial pressure of oxygen to form a microcapacitor on the tip.

6. The method of claim 1 wherein the refractory metal deposited in the step (b3) is titanium.

7. The method of claim 6 wherein at least about 20 nm of titanium are deposited.

8. The method of claim 6 wherein the titanium is deposited in a vacuum of at least 10^-6 torr.

9. The method of claim 1 wherein the step (b4) of heating the cantilever and tip combination involves annealing the titanium-coated tip in argon at one of 650°

C. for at least 5 minutes and 700°

C. for at least 0.5 minutes to form the C49 phase of titanium silicide.

10. The method of claim 6 wherein the step (b4) of heating the cantilever and tip combination involves annealing the titanium-coated tip in nitrogen at one of 650°

C. for at least 5 minutes and 700°

C. for at least 0.5 minutes to form the C49 phase of titanium silicide and an overlayer of TiN.

11. The method of claim 1 wherein the step (b5) of selectively etching and removing any unreacted refractory metal from the tip applies a room temperature mixture of 5 parts distilled water (H₂ O), 1 part hydrogen peroxide (H₂ O₂), and 1 part ammonium hydroxide (NH₄ OH).

12. The method of claim 6 wherein the step (b6) of annealing the cantilever and tip combination in an ambient free of oxygen involves subjecting the cantilever and tip combination to a temperature of about 800°

C. for at least 5 minutes in argon.

13. The method of claim 1 wherein the step (b) of forming a refractory metal silicide on at least the tip of the cantilever and tip combination further includes (b7) removing any unreacted refractory metal from the tip.

14. The method of claim 13 wherein the step (b7) of removing any unreacted refractory metal from the tip applies an etchant of 7 parts distilled water (H₂ O), 2 parts hydrogen peroxide (H₂ O₂), and 1 part ammonium hydroxide (NH₄ OH).

15. The method of claim 1 wherein the step (b) of forming a refractory metal silicide involves forming a refractory metal silicide on both the tip and the cantilever.

16. The method of claim 1 wherein the step (b) of forming a refractory metal silicide on at least the tip of the cantilever and tip combination yields a thicker coating of the refractory metal silicide on the free end of the tip than at the corner of the tip where the tip joins the cantilever.

17. The method of claim 1 wherein, in the step (b) of forming a refractory metal silicide on at least the tip of the cantilever and tip combination, the refractory metal silicide is formed directly on the tip, without any intervening insulating layer, along the entire length of the tip.