Liquid-particle analysis of metal materials

• US 8,030,082 B2
• Filed: 01/13/2006
• Issued: 10/04/2011
• Est. Priority Date: 01/13/2006
• Status: Active Grant

• Current Assignee: Honeywell International Inc.
• Original Assignee: Honeywell International Inc.
• Inventors: Strothers, Susan D., Clark, Brett M., Kardokus, Janine K.
• Primary Examiner(s): Menon; Krishnan S
• Assistant Examiner(s): FRITCHMAN, REBECCA M
• Application Number:
  US11/331,489
• Publication Number:
  US 20070166828A1
• Time in Patent Office: 2,090 Days
• Field of Search: 436/73, 436/75, 356/336, 356/337, 356/338, 356/341, 250/574
• US Class Current: 436/73
• CPC Class Codes: G01N 33/2022 Non-metallic constituents
• CPC Class Codes: G01N 33/205 in liquid state, e.g. molten metals

Abstract

The invention includes a method of detecting impurities in a metal-containing article. A portion of metal material is removed from a metal article and is solubilized in an acid or base-comprising liquid to produce a liquid sample. The liquid sample is subjected to an incident laser beam and light scattered from the sample is detected. The invention includes a method of analyzing a physical vapor deposition target material. A portion of target material is removed from the target and is rinsed with an acid-comprising solution. The portion of target material is dissolved to produce a liquid sample. The sample is subjected to an incident laser beam and scatter of the laser beam is detected to determine the number of particles present in the sample within a particular size range.

Claims

1. A method of detecting impurities in a metal-containing article, comprising:

providing an article comprising a metal material;

solubilizing a portion of metal material in a liquid to produce a liquid sample containing undissolved impurities, the liquid being one of an acid solution or a base solution;

subjecting the liquid sample to at least one of an incident laser beam and a non-coherent broad band beam; and

detecting light scattered from the original impurities in the liquid sample; and

counting the number of particles present in the liquid sample.

2. The method of claim 1 wherein the impurities present in the metal material comprise at least one of non-metallic particles and inclusions present in the metal material.

3. The method of claim 1 wherein the impurities present in the metal material consist essentially of the at least one of non-metallic particles and inclusions.

4. The method of claim 1 wherein impurities present in the liquid sample comprise particles in the size range of less than 100 μ

m.

5. The method of claim 1 wherein impurities present in the liquid sample comprise particles, wherein all particles in the sample have a particle size of less than about 1 μ

m.

6. The method of claim 1 wherein the detecting scattered light comprises obtaining a scatter pattern, and further comprising determining particle sizes of particulate impurities present in the liquid sample based upon the scatter pattern.

7. The method of claim 6 wherein the determined particle sizes are less than 100 μ

m.

8. The method of claim 6 wherein the determined particle sizes are less than 20 μ

m diameter.

9. The method of claim 6 wherein the determined particle sizes are less than 1 μ

m.

10. The method of claim 6 wherein the determined particle sizes are less than 0.5 μ

m.

11. The method of claim 1 wherein the metal-containing article is a sputtering target.

12. The method of claim 11 wherein the portion of the metal material is removed prior to any sputtering from the target.

13. The method of claim 11 wherein the portion of the metal material is removed after sputtering from the target has occurred.

14. The method of claim 1 wherein the metal-containing article comprises a layer of the metal material deposited by sputtering from a sputtering target.

15. The method of claim 1 wherein the incident laser beam is a first laser beam having a first wavelength, and further comprising after subjecting the liquid sample to the first incident laser beam, subjecting the liquid sample to a second incident laser beam having a second wavelength that differs from the first wavelength.

16. The method of claim 15 wherein scatter from the first laser beam provides particle size and count information for a first set of particles within a first size range, and wherein scatter from the second laser beam provides particle size and count information for a second set of particles within a second size range.

17. A method of analyzing a physical vapor deposition target material comprising:

rinsing a portion of material with an acid-comprising solution;

preparing a sample for analysis by dissolving metal comprised by the portion of material in a liquid;

subjecting the liquid sample to an incident beam selected from a laser beam and a non-coherent broad band beam;

detecting scatter of the incident beam to determine the number of particles present in the liquid sample within a particle size range.

18. The method of claim 17 wherein the particles present in the sample comprise at least one of non-metallic compounds and inclusions.

19. The method of claim 17 wherein the particle size range is less than 20 μ

m.

20. The method of claim 17 wherein the target material comprises at least one metal selected from the group consisting of Al, Cu, Ti, Ta, Ru, W, Au, Ag, Mo, Co, Ni, Se, Ni, Se, Te, Ge, Sn and Pb.