Two-stage chemical mixing system

• US 5,874,049 A
• Filed: 01/23/1997
• Issued: 02/23/1999
• Est. Priority Date: 11/07/1995
• Status: Expired due to Fees

• Current Assignee: Air Liquide Electronics US LP (Air Liquide SA)
• Original Assignee: Applied Chemical Solutions, Inc. (Tokyo Electron Limited)
• Inventors: Geatz, J. Tobin, Green, Randall L., Ferri, Edward T. Jr.
• Primary Examiner(s): MCMAHON, TIMOTHY M
• Application Number:
  US08/789,335
• Time in Patent Office: 761 Days
• Field of Search: 422/106, 422/110, 422/111, 422/256, 366/132, 366/152.1, 366/152.2, 366/153.1, 366/162.1
• US Class Current: 422/106
• CPC Class Codes: G05D 11/133 with discontinuous action
• CPC Class Codes: G05D 11/138 by sensing the concentration of the mixture, e.g. measuring pH value

Abstract

A chemical mixing system for mixing ingredients at desired concentrations concentration within a qualification range. Batches of the mixed chemical are mixed in a relatively small mix vessel and transferred to a relatively large mix drum. The concentration of the chemical within the mix drum is measured by a concentration monitor. If the measured concentration of the chemical in the mix drum is within the qualification range, the batches of chemical in the mix vessel are mixed to the desired concentration. If the measured concentration of the chemical in the mix drum is below the qualification range, the batches of chemical in the mix vessel are mixed to a high concentration which is greater than the desired concentration. If the measured concentration of the chemical in the mix drum is above the qualification range, the batches of chemical in the mix vessel are mixed to a low concentration which is less than the desired concentration. Batch averaging is thereby performed to maintain the concentration of chemical in the mix drum within the desired qualification range.

Claims

1. A chemical mixing system for controlling a concentration of a chemical species in an admixture such that the concentration of the chemical species is maintained within a defined qualification range, said chemical mixing system comprising:

(a) a mix vessel having an internal volume suitable for preparing a batch from ingredients comprising a diluent and a concentrated solution containing a relatively high concentration of the chemical species relative to the qualification range, wherein the mix vessel is adapted to receive the concentrated solution and the diluent from first and second supply sources, respectively;

(b) a mix drum having an internal volume for holding a supply of the admixture, wherein the internal volume of the mix drum is of a size sufficient for holding a plurality of batches prepared in the mix vessel, and wherein the mix drum is coupled to the mix vessel so that one or more batches prepared in the mix vessel can be transported to the internal volume of the mix drum in order to replenish the supply of, and controllably adjust the concentration of the chemical species in, the admixture; and

(c) a control system responsive to information comprising a measured concentration of the chemical species in the admixture, wherein said control system is capable of generating control signals for controlling the amounts of the concentrated solution and the diluent which are combined in the mix vessel when a batch is prepared so that the prepared batch comprises a corrective concentration of the chemical species relative to the measured concentration of the chemical species in the admixture.

2. The chemical mixing system of claim 1, wherein the control signals are valve control signals and the system further comprises a plurality of control valves disposed in the chemical mixing system at positions effective for regulating the amount of the concentrated solution and the diluent added to the mix vessel from the first and second supply sources, respectively, wherein the control valves are actuated in response to information comprising the valve control signals generated by the control system.

3. The chemical mixing system of claim 1, wherein the control system further comprises a plurality of sensors disposed on the system at positions effective to generate sensor signals representative of the respective amounts of the concentrated solution and diluent which are added to the internal volume of the mix vessel, and wherein the control system is responsive to information comprising both the measured concentration and the sensor signals.

4. The chemical mixing system of claim 3, wherein the plurality of sensors comprises:

(a) a first sensor disposed on the system at a position effective for detecting when a defined amount of one of the concentrated solution and the diluent is added to the mix vessel;

(b) a second sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is within the qualification range;

(c) a third sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is less than the qualification range; and

a fourth sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is greater than the qualification range.

5. The chemical mixing system of claim 3, wherein the sensors are disposed on the mix vessel.

6. The chemical mixing system of claim 1, wherein the ratio of the mix vessel internal volume to the mix drum internal volume is about 1:

10.

7. The chemical mixing system of claim 1, wherein the mix vessel and the mix drum each comprise a corrosion resistant material selected from the group consisting of an ultra high molecular weight polyethylene and a perfluoroalkoxy material.

8. The chemical mixing system of claim 1, wherein the concentrated solution is a concentrated aqueous HF solution and the diluent is ultra pure water.

9. The chemical mixing system of claim 1, wherein the mix drum further comprises:

(a) a low level sensor disposed at a low volume level, said low level sensor capable of generating a low level sensor signal indicative of when the supply of admixture in the drum corresponds to the low volume level; and

(b) a high level sensor disposed at a high volume level, said high level sensor capable of generating high level sensor signals indicative of when the supply of the admixture in the drum corresponds to the high volume level; and

wherein the control system is responsive to such low and high level sensor signals such that the control system causes batchwise replenishment and chemical species concentration control of the admixture supply when the low level sensor generates a signal indicating that the volume level of the supply admixture in the mix drum corresponds to the low volume level and such that the control system stops such batchwise replenishment and chemical species concentration control when the high level sensor generates a signal indicating that the volume of the admixture supply in the mix drum corresponds to the high volume level.

10. The chemical mixing system of claim 1, wherein the chemical mixing system further comprises a plurality of pressure vacuum vessels for motivating the concentrated solution and the diluent through at least a portion of the system.

11. The chemical mixing system of claim 1 further comprising:

(a) an exit line for transmitting the admixture from the mix drum to a point of use; and

(b) a conductivity probe disposed on said exit line for measuring said measured concentration of the chemical species in the admixture.

12. The chemical mixing system of claim 3, wherein said plurality of sensors comprises:

(a) a first sensor disposed on the mix vessel at a level corresponding to a predefined amount of diluent;

(b) a second sensor disposed on the mix vessel at a level higher than the first sensor by an amount which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration within the qualification range;

(c) a third sensor disposed on the mix vessel at a level higher than the first sensor, but lower than the second sensor, to approximately correspond to a concentrated solution volume that will provide a batch having a chemical species concentration which is less than the qualification range; and

(d) a fourth sensor disposed on the mix vessel at a level higher than the second sensor at a position which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration which is greater than the qualification range.

32. The chemical mixing system of claim 3, wherein said plurality of sensors comprises:

(a) a first sensor disposed on the mix vessel at a level corresponding to a predefined amount of diluent;

(b) a second sensor disposed on the mix vessel at a level higher than the first sensor by an amount which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration within the qualification range;

(c) a third sensor disposed on the mix vessel at a level higher than the first sensor, but lower than the second sensor, to approximately correspond to a concentrated solution volume that will provide a batch having a chemical species concentration which is less than the qualification range; and

(d) a fourth sensor disposed on the mix vessel at a level higher than the second sensor at a position which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration which is greater than the qualification range.

13. A process for controlling an amount of a chemical species in an admixture, comprising the steps of:

(a) providing a supply of the admixture, wherein the admixture comprises a concentration of the chemical species;

(b) measuring the concentration of the chemical species in the admixture;

(c) determining if the measured concentration is within a defined qualification range;

(d) preparing a batch comprising a corrective concentration of the chemical species relative to the measured concentration of the chemical species in the admixture, wherein the step of preparing the batch comprises the steps of;

(i) providing ingredients comprising a concentrated solution and a diluent, wherein the concentrated solution contains a relatively high concentration of the chemical species relative to the qualification range;

(ii) providing a mix vessel having an internal volume suitable for preparing the batch, wherein the mix vessel is adapted to receive the concentrated solution and the diluent from first and second supply sources, respectively, and wherein the system is provided with a plurality of sensors capable of generating sensor signals representative of the respective amounts of the concentrated solution and the diluent which are added to the internal volume of the mix vessel; and

(iii) adding amounts of said ingredients to the mix vessel effective to provide the batch with the corrective concentration of the chemical species, wherein the amount of said ingredients added to the mix vessel is controlled in response to information comprising the sensor signals and to the measured concentration of the chemical species in the admixture; and

(e) combining the batch with the admixture supply in order to controllably adjust the concentration of the chemical species in the admixture.

14. The process of claim 13, wherein at least a portion of the admixture supply is provided in a mix drum having an internal volume for holding said portion of the admixture, and wherein a mix drum conduit assembly is coupled to the mix drum, said mix drum conduit assembly including (i) a line for transporting the admixture from the mix drum to a point of use and (ii) a recirculation line for transporting the admixture to and from the mix drum.

15. The process of claim 14, wherein the step of measuring the concentration of the chemical species in the admixture comprises measuring said concentration from a portion of the admixture which is being transported through said mix drum conduit assembly.

16. The process of claim 14, wherein the internal volume of the mix vessel is less than the internal volume of the mix drum, and wherein the mix vessel is coupled to the mix drum by a conduit for transmitting batches from the mix vessel to the mix drum.

17. The process of claim 16, wherein the ratio of the internal volume of the mix vessel to the internal volume of the mix drum is about 1:

10.

18. The process of claim 13, wherein the plurality of sensors comprises:

(a) a first sensor disposed on the system at a position effective for detecting when a defined amount of one of the concentrated solution and the diluent is added to the mix vessel;

(b) a second sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is within the qualification range;

(c) a third sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is less than the qualification range; and

(d) a fourth sensor disposed on the system at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is greater than the qualification range.

19. The process of claim 16, wherein the chemical constituent sensors are disposed on the mix vessel.

20. The process of claim 13, wherein said plurality of sensors comprises:

(a) a first sensor disposed on the mix vessel at a level corresponding to a predefined amount of diluent;

(b) a second sensor disposed on the mix vessel at a level higher than the first sensor by an amount which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration within the qualification range;

(c) a third sensor disposed on the mix vessel at a level higher than the first sensor, but lower than the second sensor, to approximately correspond to a concentrated solution volume that will provide a batch having a chemical species concentration which is less than the qualification range; and

(d) a fourth sensor disposed on the mix vessel at a level higher than the second sensor at a position which corresponds approximately to a concentrated solution volume that will yield a batch having a chemical species concentration which is greater than the qualification range.

21. The process of claim 16, wherein the mix vessel and the mix drum each comprise a corrosion resistant material selected from the group consisting of an ultra high molecular weight polyethylene and a perfluoroalkoxy material.

22. The process of claim 13, wherein the concentrated solution is a concentrated aqueous HF solution and the diluent is ultra pure water.

23. The process of claim 13, wherein the mix drum further comprises:

(a) a low level sensor disposed at a low volume level, said low level sensor capable of generating a low level sensor signal indicative of when the supply of admixture in the mix drum corresponds to the low volume level; and

(b) a high level sensor disposed at a high volume level, said high level sensor capable of generating high level sensor signals indicative of when the supply of the admixture in the mix drum corresponds to the high volume level; and

wherein the method further comprises providing a control system responsive to such low and high level sensor signals such that the control system causes batchwise replenishment and chemical species concentration control of the admixture supply when the low level sensor generates a signal indicating that the volume level of the supply admixture in the mix drum corresponds to the low volume level and stops such batchwise replenishment and chemical species concentration control when the high level sensor generates a signal indicating that the volume of the admixture in the mix drum corresponds to the high volume level.

24. The process of claim 16, further comprising the steps of:

(a) transporting respective volumes of the concentrated solution and the diluent into the mix vessel in order to prepare the batch having a corrective concentration of the chemical species;

(b) transporting the batch from the mix vessel to the mix drum; and

(c) transporting the admixture from the mix drum to a point of use;

wherein said transporting steps are caused by a plurality of pressure vacuum vessels.

25. A process for controlling an amount of a chemical species in an admixture, comprising the steps of:

(a) providing a supply of the admixture, wherein the admixture comprises a concentration of the chemical species;

(b) measuring the concentration of the chemical species in the admixture;

(c) determining if the measured concentration is within a defined qualification range; and

(d) batchwise adjusting the concentration of the chemical species in the admixture in response to the measured concentration of the chemical species in the admixture, said batchwise adjusting step comprising the steps of;

(i) providing a concentrated solution having a high concentration of the chemical species relative to the qualification range;

(ii) providing a diluent;

(iii) providing a control system responsive to information comprising the measured concentration of the chemical species in the admixture, wherein said control system is capable of generating control signals for controlling respective amounts of the concentrated solution and the diluent in order to provide a batch having a corrective concentration of the chemical species relative to the measured concentration of the chemical species in the admixture; and

(iv) using information comprising the control signals to controllably dilute the concentrated solution with an amount of the diluent effective to provide said batch having a corrective concentration of the chemical species relative to the measured concentration of the chemical species in the admixture; and

(v) combining the batch with the supply of the admixture.

26. The process of claim 25, wherein at least a portion of the admixture supply is provided in a mix drum having an internal volume for holding said portion of the admixture, and wherein a mix drum conduit assembly is coupled to the mix drum, said mix drum conduit assembly including (i) a line for transporting the admixture from the mix drum to a point of use and (ii) a recirculation line.

27. The process of claim 26, wherein the step of measuring the concentration of the chemical species in the admixture comprises measuring said concentration from a portion of the admixture which is being transported through said mix drum conduit assembly.

28. The process of claim 26, wherein the batch is prepared in a mix vessel having an internal volume, wherein the internal volume of mix vessel is less than the internal volume of the mix drum, and wherein the mix vessel is coupled to the mix drum by a conduit for transmitting batches from the mix vessel to the mix drum.

29. The process of claim 26, wherein the ratio of the internal volume of the mix vessel to the internal volume of the mix drum is about 1:

10.

30. The process of claim 28, further comprising the step of providing a plurality of sensors disposed on the mix vessel at positions effective to generate sensor signals representative of the respective amounts of the concentrated solution and diluent which are added to the internal volume of the mix vessel, and wherein the control system is responsive to information comprising both the measured concentration and the sensor signals for controlling the amounts of the concentrated solution and diluent which are combined to form the batch.

31. The process of claim 30, wherein the plurality of sensors comprises:

(a) a first sensor disposed on the mix vessel at a position effective for detecting when a defined amount of one of the concentrated solution and the diluent is added to the mix vessel;

(b) a second sensor disposed on the mix vessel at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is within the qualification range;

(c) a third sensor disposed on the mix vessel at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is less than the qualification range; and

(d) a fourth sensor disposed on the mix vessel at a position effective for detecting when a combined amount of the concentrated solution and the diluent in the mix vessel is effective to provide a batch having a corrective concentration of the chemical species which is greater than the qualification range.

33. The process of claim 28, wherein the mix vessel and the mix drum each comprise a corrosion resistant material selected from the group consisting of an ultra high molecular weight polyethylene and a perfluoroalkoxy material.

34. The process of claim 25, wherein the concentrated solution is a concentrated aqueous HF solution and the diluent is ultra pure water.

35. The process of claim 26, wherein the mix drum further comprises:

(a) a low level sensor disposed at a low volume level, said low level sensor capable of generating a low level sensor signal indicative of when the supply of admixture in the drum corresponds to the low volume level; and

(b) a high level sensor disposed at a high volume level, said high level sensor capable of generating high level sensor signals indicative of when the supply of the admixture in the drum corresponds to the high volume level; and

wherein the control system is responsive to such low and high level sensor signals such that the control system causes batchwise replenishment and chemical species concentration control of the admixture supply when the low level sensor generates a signal indicating that the volume level of the supply admixture in the mix drum corresponds to the low volume level and stops such batchwise replenishment and chemical species concentration control when the high level sensor generates a signal indicating that the volume of the admixture in the mix drum corresponds to the high volume level.