IP Library Granted Patent US 8,372,651
Granted Patent B2
US 8,372,651 · App. 11/696,797 · Granted Feb 12, 2013

Method of monitoring a surfactant in a microelectronic process by absorbance

Inventors: Amy M. Tseng (Woodridge, IL); John E. Hoots (Batavia, IL); Brian V. Jenkins (Warrenville, IL)
Assignee: Nalco Company
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Quick Facts
Patent No.
US 8,372,651
App. No.
11/696,797
Granted
Feb 12, 2013
Kind
B2
Abstract

A method of monitoring a surfactant in a microelectronic process is disclosed. Specifically, the monitoring of a surfactant occurs by studying the absorbance of a sample collected from a microelectronic process.

Claims (43)

1. A method of monitoring a surfactant in a process for making a microelectronic component comprising:

a. adding the surfactant to a process for making a microelectronic component, wherein an absorbance of the surfactant is capable of being measured, wherein the absorbance is ultraviolet-visible absorbance;

b. sampling fluid from the process;

c. measuring the absorbance of the surfactant in the sample;

d. correlating the absorbance of the surfactant in the sample with the concentration of the surfactant in the process; and

e. taking action to maintain the concentration of the surfactant in the process at a desired level, wherein the desired level is a dilution ratio of about 200 parts total volume to about one part surfactant volume;

wherein the sampling comprises adding a chromogenic agent into the fluid, the chromogenic agent comprising 4,5,6,7-Tetrachloro-2′,4′,5′,7′-tetraiodofluorescein disodium salt.

2. The method of claim 1 wherein the process is a photolithography process.

3. The method of claim 1 wherein the process is a wet-etching process.

4. The method of claim 1 wherein the process is monitored on-line.

5. The method of claim 1 wherein the sampling involves an SIA analysis of the sample or an SFA analysis of the sample.

6. The method of claim 1 wherein sampling uses a LOV module for a sample analysis.

7. The method of claim 1 wherein sampling includes dilution of the sample and/or removal of contaminants from the sample.

8. The method of claim 1 wherein the surfactant is a cationic surfactant.

9. The method of claim 8 wherein the surfactant is a fluorinated surfactant.

10. The method of claim 1 wherein the surfactant is a non-ionic surfactant.

11. The method of claim 10 wherein the surfactant is a fluorinated surfactant.

12. The method on claim 1 wherein the monitoring is continuous, sequential, or at a programmed interval.

13. The method of claim 1 wherein sampling includes measuring an additional process variable, optionally wherein the process variable includes at least one of the following process variables: pH of the process; conductivity of the process stream; and viscosity of the process stream.

14. The method of claim 1 wherein the process is monitored on-line.

15. A method of monitoring a surfactant in a process for making a microelectronic component comprising:

a. adding the surfactant to a process for making a microelectronic component;

b. sampling fluid from the process, the sampling performed subsequent to the addition of the surfactant to the process and also before application of the surfactant to the microelectronic component, the sampling accomplished by drawing the sample into a side stream comprising a flow cell, wherein the sampling includes comprises adding a chromogenic agent to the sample and forming a reacted surfactant;

c. measuring an absorbance of the reacted surfactant in the sample, wherein the absorbance is ultraviolet-visible absorbance;

d. correlating the absorbance of the reacted surfactant with the concentration of the surfactant in the process;

e. taking action to maintain the concentration of the surfactant in the process at a desired level; wherein the desired level is a dilution ratio of about 200 parts total volume to about one part surfactant volume; and

wherein the chromogenic agent is 4,5,6,7-Tetrachloro-2′,4′,5′,7′-tetraiodofluorescein disodium salt.

16. The method of claim 15 further comprising adding at least one modifying agent to the sample, which modifies the absorbance signal of the surfactant positively or negatively.

17. The method of claim 16 wherein said modifying agent positively affects the signal and is a cationic agent selected from the group consisting of: tertiary amines; quaternary amines; tetramethylammonium hydroxide; tetrabutylammonium chloride; cetyltrimethylammonium bromide; and a combination thereof.

18. The method of claim 16 wherein the modifying agent positively affects the signal and is an anionic agent that contains at least one of the following functional groups: sulfonate, carboxylate, and phosphonate.

19. The method of claim 16 wherein said surfactant is a non-ionic surfactant.

20. The method of claim 15 wherein said surfactant is a cationic surfactant.

21. The method of claim 20 wherein the surfactant is a fluorinated surfactant.

22. The method of claim 15 wherein said surfactant is a non-ionic surfactant.

23. The method of claim 22 wherein the surfactant is a fluorinated surfactant.

24. The method of claim 15 wherein the process is a photolithography process.

25. The method of claim 15 wherein the process is a wet-etching process.

26. The method of claim 15 wherein the process is monitored on-line.

27. The method of claim 15 wherein the sampling involves an SIA analysis of the sample or an SFA analysis of the sample.

28. The method of claim 15 wherein sampling uses a LOV module for a sample analysis.

29. The method of claim 15 wherein sampling includes dilution of the sample and/or removal of contaminants from the sample.

30. The method on claim 15 wherein the monitoring is continuous, sequential, or at a programmed interval.

31. The method of claim 15 wherein sampling includes measuring an additional process variable, optionally wherein the process variable includes at least one of the following process variables: pH of the process; conductivity of the process stream; and viscosity of the process stream.

Assignments (7)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 4, 2017
From: NALCO COMPANY
To: ECOLAB USA INC.
Reel/Frame 042147/0420 →
CHANGE OF NAME Recorded Feb 28, 2017
From: NALCO COMPANY
To: NALCO COMPANY LLC
Reel/Frame 041835/0903 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 28, 2017
From: NALCO COMPANY LLC; CALGON CORPORATION; CALGON LLC; ONDEO NALCO ENERGY SERVICES, L.P.
To: ECOLAB USA INC.
Reel/Frame 041836/0437 →
RELEASE OF SECURITY INTEREST Recorded Feb 24, 2017
From: BANK OF AMERICA, N.A.
To: NALCO COMPANY
Reel/Frame 041808/0713 →
RELEASE OF SECURITY INTEREST Recorded May 26, 2015
From: BANK OF AMERICA, N.A.
To: NALCO COMPANY
Reel/Frame 035771/0668 →
SECURITY AGREEMENT Recorded May 18, 2009
From: NALCO COMPANY; CALGON LLC; NALCO ONE SOURCE LLC; NALCO CROSSBOW WATER LLC
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 022703/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 5, 2007
From: TSENG, AMY M.; HOOTS, JOHN E.; JENKINS, BRIAN V.
To: NALCO COMPANY
Reel/Frame 019119/0728 →
Continuity (1)
Related Publication 20080245134A1 · Oct 9, 2008