IP Library Granted Patent US 8,753,896
Granted Patent B2
US 8,753,896 · App. 11/696,760 · Granted Jun 17, 2014

Method of monitoring a surfactant in a microelectronic process by fluorescence

Inventors: Brian V. Jenkins (Warrenville, IL); John E. Hoots (Batavia, IL); Amy M. Tseng (Woodridge, IL)
Assignee: Nalco Company
H01L22/00H01L22/20H01L22/30G01N21/00
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Quick Facts
Patent No.
US 8,753,896
App. No.
11/696,760
Granted
Jun 17, 2014
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 fluorescence or electromagnetic emission of a sample collected from a microelectronic process.

Claims (70)

1. A method of controlling concentration of a diluted surfactant fluid within a desired dilution ratio prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant and a carrier fluid prior to application of the diluted surfactant fluid to the microelectronic component, wherein the surfactant is capable of fluorescence;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creating a conditioned sample b further diluting the sampled diluted surfactant fluid;

measuring the fluorescence of the surfactant in the conditioned sample;

correlating the measured fluorescence of the surfactant in the conditioned sample with the concentration of the surfactant in the sampled diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is not within the desired dilution ratio, taking action to adjust the concentration of the surfactant in the diluted surfactant fluid so the fluid is within the desired dilution ratio prior to application of the diluted surfactant fluid to the microelectronic component; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is within the desired dilution ratio, applying the diluted surfactant fluid onto the microelectronic component.

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 controlled 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 the sampling utilizes a LOV module for a sample analysis.

7. The method of claim 1 , wherein the sampling further comprises removal of contaminants from the sampled diluted surfactant fluid.

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 controlling 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. A method of controlling concentration of a diluted surfactant fluid within a desired dilution ratio prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant and a carrier fluid prior to application of the diluted surfactant fluid to the microelectronic component;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creating a conditioned sample by further diluting the sampled diluted surfactant fluid and adding a fluorogenic agent capable of reacting with the surfactant;

measuring at least the fluorescence of the reacted surfactant in the conditioned sample;

correlating the measured fluorescence of the reacted surfactant in the conditioned sample with the concentration of the surfactant in the sampled diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is not within the desired dilution ratio, taking action to adjust the concentration of the surfactant at a desired dilution ratio in the diluted surfactant fluid so the fluid is within the desired dilution ratio prior to application of the diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is within the desired dilution ratio, applying the diluted surfactant fluid onto the microelectronic component.

15. The method of claim 14 , wherein the fluorogenic agent is 4,5,6,7-Tetrachloro-2′,4′,5′,7′-tetraiodofluorescein disodium salt.

16. The method of claim 14 , further comprising adding at least one modifying agent to the sampled diluted surfactant fluid and/or the conditioned sample, which modifies the fluorescence of the reacted surfactant positively.

17. The method of claim 16 , wherein said modifying agent is a cationic agent selected from the group consisting of: a tertiary amine; a quaternary amine; tetramethylammonium hydroxide; tetrabutylammonium chloride; cetyltrimethylammonium bromide; and combinations thereof.

18. The method of claim 16 , wherein the modifying agent is an anionic agent comprising at least one of the following functional groups: a sulfonate, a carboxylate, and a phosphonate.

19. The method of claim 14 wherein said surfactant is a cationic surfactant.

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

21. The method of claim 14 , wherein said surfactant is a non-ionic surfactant.

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

23. A method of controlling concentration of a diluted surfactant fluid within a desired consumption factor prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant, a fluorescent tracer, and a carrier fluid prior to application of the diluted surfactant fluid to the microelectronic component, wherein the surfactant is capable of fluorescence;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creatine a conditioned sample b further diluting the sampled diluted surfactant fluid;

measuring the fluorescence of the surfactant and the fluorescence of the fluorescent tracer in the conditioned sample;

determining a consumption factor of the surfactant by comparing the fluorescence of the fluorescent tracer and the fluorescence of the surfactant in the conditioned sample; and

if the consumption factor in the previous step indicates that the sampled diluted surfactant fluid is being consumed at an undesired rate, taking action to adjust the concentration of the surfactant in the diluted surfactant fluid so the fluid is within the desired consumption factor prior to application of the diluted surfactant fluid to the microelectronic component; and

if the consumption factor in the previous step indicates that the sampled diluted surfactant fluid is within the desired consumption factor, applying the diluted surfactant fluid onto the microelectronic component.

24. The method of claim 23 , wherein the fluorescent tracer is an inert fluorescent tracer.

25. A method of controlling concentration of a diluted surfactant fluid within a desired dilution ratio prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant a fluorescent tracer and a carrier fluid prior to application of the diluted surfactant fluid to the microelectronic component;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creating a conditioned sample b further diluting the sampled diluted surfactant fluid;

measuring in the conditioned sample at least the fluorescence of the fluorescent tracer alone or in combination with the surfactant if the surfactant is capable of fluorescence;

correlating the measured fluorescence of the fluorescent tracer alone or in combination with the surfactant with the concentration of the surfactant in the sampled diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is not within the desired dilution ratio taking action to adjust the concentration of the surfactant in the diluted surfactant fluid so the fluid is within the desired dilution ratio prior to application of the diluted surfactant fluid to the microelectronic component and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is within the desired dilution ratio, applying the diluted surfactant fluid onto the microelectronic component.

26. The method of claim 25 , wherein said fluorescent tracer is an inert fluorescent tracer.

27. A method of controlling concentration of a diluted surfactant fluid within a desired dilution ratio prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant and a carrier fluid prior to the application of the diluted surfactant fluid to the microelectronic component, wherein the surfactant is capable of emitting electromagnetic radiation;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creatine a conditioned sample b further diluting the sampled diluted surfactant fluid;

measuring the emission of electromagnetic radiation of the surfactant in the conditioned sample;

correlating the measured emission of electromagnetic radiation of the surfactant in the conditioned sample with the concentration of the surfactant in the sampled diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is not within the desired dilution ratio, taking action to adjust the concentration of the surfactant in the diluted surfactant fluid so the fluid is within the desired dilution ratio prior to application of the diluted surfactant fluid to the microelectronic component; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is within the desired dilution ratio, applying the diluted surfactant fluid onto the microelectronic component.

28. A method of controlling concentration of a diluted surfactant fluid within a desired dilution ratio prior to application of the diluted surfactant fluid to a microelectronic component during manufacture of the microelectronic component comprising:

creating a diluted surfactant fluid by combining a surfactant and a carrier fluid prior to application of the diluted surfactant fluid to the microelectronic component;

sampling the diluted surfactant fluid prior to application of the diluted surfactant fluid to the microelectronic component;

creating a conditioned sample by further diluting the sampled diluted surfactant fluid and adding an emission a eg capable of reacting with the surfactant and emitting electromagnetic radiation as a result of the reaction;

measuring at least the emission of electromagnetic radiation of the reacted surfactant in the conditioned sample;

correlating the measured emission of electromagnetic radiation of the reacted surfactant with the concentration of the surfactant in the sampled diluted surfactant fluid; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is not within the desired dilution ratio, taking action to adjust the concentration of the surfactant in the diluted surfactant fluid so the fluid is within the desired dilution ratio prior to application of the diluted surfactant fluid to the microelectronic component; and

if the correlation in the previous step indicates that the sampled diluted surfactant fluid is within the desired dilution ratio, applying the diluted surfactant fluid onto the microelectronic component.

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: JENKINS, BRIAN V.; HOOTS, JOHN E.; TSENG, AMY M.
To: NALCO COMPANY
Reel/Frame 019119/0159 →
Continuity (1)
Related Publication 20080248577A1 · Oct 9, 2008