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Process for precise volumetrio diluting/mixing of chemicals    
United States Patent5490611   
Link to this pagehttp://www.wikipatents.com/5490611.html
Inventor(s)Bernosky; Eugene W. (Hollister, CA); Geatz; J. Tobin (Durham, NC); Ferrie, Jr.; Edward T. (Gilroy, CA); Roberson, Jr.; Glenn A. (Hollister, CA)
AbstractApparatus and method for accurate measuring and mixing of chemicals is disclosed. The apparatus includes one or more metered vessels having a container of predetermined volume and at least one constricted vent tube therein. By mounting a sensor on the constricted vent tube, a greatly amplified measurement of the precise chemical volume in the metered vessel is provided. The apparatus and method of the present invention readily lends itself to a variety of applications and can be adapted to handle virtually any form of chemical mixing, diluting, or generating process.
   














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Drawing from US Patent 5490611
Process for precise volumetrio diluting/mixing of chemicals - US Patent 5490611 Drawing
Process for precise volumetrio diluting/mixing of chemicals
Inventor     Bernosky; Eugene W. (Hollister, CA); Geatz; J. Tobin (Durham, NC); Ferrie, Jr.; Edward T. (Gilroy, CA); Roberson, Jr.; Glenn A. (Hollister, CA)
Owner/Assignee     Applied Chemical Solutions, Inc. (Hollister, CA)
Patent assignment
All assignments
Publication Date     February 13, 1996
Application Number     08/349,429
PAIR File History     Application Data   Transaction History
Image File Wrapper   Patent Term   Fees
Litigation
Filing Date     December 5, 1994
US Classification     222/1 222/56 222/61 222/64 222/145.5 222/145.6 222/152
Int'l Classification     B67D 005/08
Examiner     Oberleitner; Robert J.
Assistant Examiner     Bomberg; Kenneth
Attorney/Law Firm     Faegre & Benson
Address
Parent Case     The present application is a division of U.S. patent application Ser. No. 035,252 filed Mar. 22, 1993 now U.S. Pat. No. 5,370,269 , which was a continuation-in-part of U.S. patent application Ser. No. 948,392, filed Sep. 21, 1992 now Pat. No. 5,330,072, which was a continuation-in-part of U.S. patent application Ser. No. 583,826, filed Sep. 17, 1990, and issued as U.S. Pat. No. 5,148,945 on Sep. 22, 1992.
Priority Data    
USPTO Field of Search     222/1 222/43 222/56 222/59 222/61 222/64 222/66 222/71 222/135 222/136 222/145.5 222/145.6 222/152 222/309 222/318 222/399 137/205 137/208 137/209 137/545
Patent Tags     precise volumetrio diluting/mixing chemicals
   
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Ferri, Jr.
222/61
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Bernosky
222/61
Dec,1994

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Ferri, Jr.

Jul,1994

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Clark
29/25.01
Sep,1993

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Geatz
222/1
Sep,1992

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Shannon
222/61
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Shannon
222/61
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diVincenzo
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Buschmann
222/23
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What is claimed:

1. A process for precision mixing of chemicals from multiple bulk sources which comprises:

providing a metered vessel, such vessel comprising a container of predetermined volume;

providing a first intake conduit for the flow of chemical between a first bulk source and the metered vessel;

providing a first constricted fill tube in the container, the first fill tube extending to a first height;

providing a second intake conduit for the flow of chemical between a second bulk source and the metered vessel;

providing a second constricted fill tube in the container, the second fill tube extending to a second height which is higher than the first height;

providing at least first and second sensors associated with each fill tube, the first sensor detecting when the chemical level is approaching a desired volume and the second sensor positioned to detect the presence of chemical in the associated fill tube when chemical has reached the desired volume in the metered vessel;

providing a first valve on the first intake conduit responsive to the second sensor associated with the first fill tube, for ceasing fluid flow to the metered vessel through the first intake conduit;

providing a second valve on the second intake conduit responsive to the second sensor associated with the second fill tube, for ceasing fluid flow to the metered vessel through the second intake conduit;

providing a conduit from the metered vessel to at least one down-stream facility;

providing means to transfer chemical from the bulk sources to the metered vessel;

providing means to motivate chemical from the metered vessel to the down-stream facility; and

wherein precision mixing is accomplished by the following steps: motivating chemical from the first bulk source into the metered vessel until chemical reaches the second sensor associated with the first fill tube, at which point the first valve on the first intake conduit is regulated to cease chemical flow to the metered vessel; motivating chemical from the second bulk source into the metered vessel until chemical reaches the second sensor associated with the second fill tube, at which point the second valve on the second intake conduit is regulated to cease chemical flow into the metered vessel; mixing together the chemicals from the first bulk source and the second bulk source in measured proportions provided from the metered vessel; and transferring mixed chemical to the down-stream facility.

2. The process of claim 1 wherein mixing of the chemicals occurs in the metered vessel.

3. The process of claim 1 further comprising

providing a mixing vessel downstream of the metered vessel; and

wherein mixing of the chemicals occurs in the mixing vessel.

4. The process of claim 3 further comprising

proving multiple metered vessels, each corresponding to one of the bulk sources; and

transferring chemical from each of the metered vessels into the mixing vessel where mixing occurs.

5. The process of claim 3 which further comprises

providing means to regulate temperature in the mixing vessel; and

wherein the temperature of the chemical is maintained at a pre-determined level during the mixing step in the mixing vessel.

6. The process of claim 1 further comprising

providing adjustable valve means on each of the first and second intake conduits to permit constriction of the rate of fluid flow; and

regulating the adjustable valve means to reduce chemical flow rate once the first sensor associated with the first and second fill tubes detests the fluid level approaching the desired volume, and regulating the valve means to cease chemical flow once chemical has reached the desired volume.

7. The process of claim 1 which further comprises

providing a vacuum system in communication with the metered vessel;

providing a pressure system in communication with the metered vessel;

wherein chemical is drawn into the metered vessel by establishing a negative pressure in the vessel through use of the vacuum system, and chemical is dispensed from the metered vessel by applying pressure to the vessel through use of the pressure system.

8. Apparatus for accurately mixing chemicals from at least two bulk sources which comprises:

a metered vessel comprising a container of predetermined volume.

at 1easer first and second constricted fill tubes in the container, the first fill tube extending to a first height, and the second fill tube extending to a second height which is higher than the first height;

a first intake line providing fluid communication between a first bulk source and the metered vessel;

a second bulk intake line providing fluid communication between a second bulk source and the metered vessel;

a dispense line providing fluid communication between the metered vessel and at least one down-stream facility;

at least first and second sensors associated with each fill tube, the first sensor detecting when chemical level is approaching a desired volume and the second sensor positioned to detect the presence of chemical in the associated fill tube when chemical has reached the desired volume in the metered vessel so as to assure precise cessation of chemical flow at the desired volume;

a first value on the first intake line responsive to the second sensor associated with the first fill tube, for ceasing fluid flow to the metered vessel through the first intake line;

a second valve on the second intake line responsive to the second sensor associated with the second fill tube, for ceasing fluid flow to the metered vessel through the second intake line;

wherein the metered vessel is first filled with chemical from the first bulk source until the second sensor associated with the first fill tube detects the presence of chemical in the first fill tube and the valve on the first intake line is closed to cease fluid flow from the first bulk source; and the metered vessel is next filled with chemical from the second bulk source until the second sensor associated with the second fill tube detects the presence of chemical in the second fill tube and the valve on the second intake line is closed to cease fluid flow from the second bulk source.

9. The apparatus of claim 8 wherein each of the intake lines includes an adjustable valve means responsive to the first sensor associated with the first and second fill tubes, to constrict flow into the metered vessel, and assuring precise cessation of chemical flow into the metered vessel at the desired volume.

10. The apparatus of claim 8 wherein precision volume adjustment apparatus is provided on the metered vessel to assist in calibrating the exact volume of the vessel.

11. The apparatus of claim 10 wherein the precision volume adjustment apparatus comprises means for mounting the first and second fill tubes in sliding relationship with the container to control the level at which chemical begins to enter the fill tube so as to provide precision volume adjustment of the vessel.

12. The apparatus of claim 8 wherein the first and second fill tubes include a valve thereon to control the flow of fluid from the container.

13. The apparatus of claim 12 wherein the valves on the first and second fill tubes are opened only at an appropriate stage to permit chemical to fill each of the fill tubes in order of height.
 Description Submit all comments and votes
 


BACKGROUND OF THE INVENTION

1. Field of the Invention

The present invention relates to apparatus and method for mixing/diluting, generating, and/or transferring of process chemicals. More particularly, the present invention provides improved process and apparatus for the precise mixing/diluting all forms of chemicals and, especially, ultra-high purity chemicals for use in a variety of industries, such as in the manufacture of semiconductor wafers and similar products.

2. Description of the Prior Art

The inventions of the parent applications are directed to process and apparatus for the transfer and delivery of high-purity chemicals from a bulk source to one or more end-use stations. As is explained therein, in many applications in industry today it is extremely important to maintain process chemicals free of virtually all contaminants. For instance, in the semiccnductor industry the purity of chemicals, such as sulfuric acid, hydrogen peroxide, and ammonium hydroxide, used in semiconductor wafer production must be pure on level of approximately 25 (or fewer) particles per milliliter with a particle size of less than a fraction of a micron. As a result of these purity standards, many conventional methods of chemical transfer and delivery, such as paddled pumps and similar devices, have proven completely unsatisfactory.

Of further concern in these industries is that many of the chemicals employed are toxic, chemically aggressive, and/or require special conduit material, and must be carefully handled. In order to assure adequate purity and worker safety, it is extremely important that such chemicals be transferred, stored, and dispensed in a closed system, with minimal contact with the environment or workers.

Prior to the inventions of the parent applications, generally one of two methods were employed to effectuate high-purity chemical transfer. The first method is a "pumped delivery." In this method a positive displacement pump, usually an air powered double diaphragm type, is employed to provide both lift at a suction inlet from a bulk source of the chemicals and simultaneous pressure at the output to the end-user. The chemical is lifted from a chemical drum, driven through a pump, and pushed out to the point of use.

Although the pumped delivery system is widely employed, it is far from satisfactory. This system is capable of producing only minimal lift from the chemical bulk source--usually on the order of only a few pounds per square inch. Moreover, the system is replete with contamination problems: the rapidly expanding and contracting of the pump diaphragm material (e.g. TEFLON.RTM.) causes mechanical degradation, with the degradation by-products (many of which being too small to filter with state-of-the-art filtration equipment) entering the chemical process stream; further, the rapid action of the pump (usually greater than 60 cycles per minute) creates massive impulses in the system with a resulting pulsed flow which forces particles through filters--thus rendering the filters far less effective. Finally, the mechanical shock and vibration inherent in this system creates constant maintenance problems, such as leaks.

The other system which is generally used addressed only some of these problems. In a "pump/pressure delivery" system, a positive displacement pump is again employed to provide lift from the bulk source of chemicals. However, the chemicals are delivered to an intermediate vessel from which inert gas pressure is used to motivate chemical to the use areas.

Although the pump/pressure system is better controlled and is more conducive to use of filters to assure chemical purity, it still has serious drawbacks in a sub-micron chemical environment. Again, lift provided by a double diaphragm pump is restricted. Further, such pumps are prone to degradation--with the by-products entering the chemical stream. Finally, the use of a single pressure vessel for delivery results in non-continuous delivery--constraining the volume of each delivery to "batch" sizes based on the size of the pressure vessel. If demand exceeds the volume of the pressure vessel, further delivery must be "queued" while the pump refills the pressure vessel. Alternatively, pressure from the pump that is equal to or greater than the pressure of the delivery vessel must be applied to the delivery vessel to supplement or refill it during demand; this further compounds filtration and maintenance problems.

The inventions disclosed in the parent applications solve all these problems. In those inventions, a combination of vacuum and pressure is used to transfer chemical smoothly from a bulk source, through one or more intermediate pressure/vacuum vessels ("PVV"), and to one or more end-use stations. First, a vacuum pump is used to establish a vacuum in one of the PVVs to draw chemicals into the PVV. Once a PVV is filled, the vessel is then pressurized to motivate chemical to an end-use station, to another PW, or for recirculation back to the bulk source. The elimination of pumps from all chemical conduits in the system avoids the problems of degradation and contamination.

As is explained in the parent applications, the advantages of this improved transfer and delivery apparatus include: even (i.e. non-pulsed) flow through the system, reducing maintenance problems and allowing far more efficient use of filters; built-in redundancy to assure constant chemical supply and fail-safe operation; and electronic controls to monitor and maintain all aspects of system operation automatically.

In light of these substantial advantages of a vacuum/pressure transfer and delivery system, applicants believe that similar advantages can be achieved in a vacuum/pressure system for taking chemicals from multiple bulk sources and automatically mixing them (e.g. combining two or more process chemicals or diluting one or more process chemicals with water or other chemical) prior to delivery to the end-user.

Although liquid mixing systems are known, none addresses the contamination concerns of a high-purity environment. Most existing systems employ conventional fluid transfer means (e.g. pumps or water line pressure) to fill two or more metered vessels. From these vessels, the liquids to be mixed are then transferred, usually by pumps, to a mixing vessel and then to a storage facility or user. Examples of such existing systems are illustrated in U.S. Pat. Nos. 3,960,295, issued Jun. 1, 1976, to Horak, 4,019,528, issued Apr. 26, 1977, to Tyrrell, 4,215,719, issued Aug. 5, 1980, to Laar et al., and 4,823,987, issued Apr. 25, 1989, to Switall. None of these teaches means to assure that high purity chemicals will not be contaminated on a sub-micron level by the mixing apparatus itself.

Additionally, none of the existing mixing systems provides a simple yet effective method of accurately mixing chemicals in precise volumes. Although it is common to employ multiple metered vessels to measure the amount of each chemical to be mixed, with sensors typically used to cease the flow of liquid to the metered vessel once it is filled, none of these systems provides means to amplify the sensors' accuracy in order to assure very precise measurement of the volume of each vessel. The use of other metering methods, such as highly accurate flow meters or similar devices, may address some of these concerns, but are generally undesirable due to their expense, fragile nature, and/or possible contamination risks. As a result, none of the existing diluting/mixing systems is considered fully satisfactory in providing accurate mixing of high purity chemicals required by many industries.

Accordingly, it is a primary object of the present invention to provide improved apparatus and method for accurate mixing of chemicals from two or more bulk sources. It is a further object of the present invention to provide an apparatus and method that includes, or readily interfaces with, means to transfer and deliver chemical from the bulk sources to end-use stations.

It is another object of the present invention to provide an apparatus and method that includes means to transfer and mix high-purity process chemicals from bulk sources and deliver them reliably and without contamination to end-use stations.

It is yet another object of the present invention to provide an apparatus and method that includes a simple and relatively inexpensive means to yield extremely precise volumetric measurement of chemicals.

It is an additional object of the present invention to provide an apparatus and method that employs a vacuum-pressure transfer and delivery system so as to generate even flow and negligible mechanical shock in the system.

These and other objects of the present invention will become evident from review of the following specification.

SUMMARY OF THE INVENTION

The present invention provides an improved apparatus and method for extremely accurate mixing of chemicals from two or more chemical bulk sources.

In operation the invention employs one or more metered vessels of predetermined volume in communication with the bulk source of chemical via an intake line and in communication with a downstream facility via a dispense line. Each of the metered vessels includes one or more constricted vent tubes therein. Chemical is transferred from each of the bulk sources to the metered vessel until a set capacity is attained. At that point, chemical flow proceeds up the vent tube until a sensor is reached. A valve is provided on the intake line to cease fluid flow to the metered vessel in response to a signal from the sensor. By employing a constricted vent tube, the signal from the sensor can be greatly amplified to provide for more accurate filling of the metered vessel and more accurate mixing of chemicals. By including adjustable valve means on the intake lines and multiple sensors on the vent tubes, the rate of flow into the metered vessel can be carefully adjusted to provide extremely accurate chemical mixing proportions.

For improved motivation of chemicals through the apparatus of the present invention, a vacuum system and a pressure system are provided. Chemical can be smoothly drawn from the bulk source by decompressing (i.e. to a negative pressure) the metered vessel via the vacuum system. Once the metered vessel is filled, the metered vessel can then be pressurized using compressed gas in the pressure system to drive chemical through the dispense line to an intermediate or end-use station. The pressure system may also be used to perform other functions in the apparatus of the present invention, such as activating pneumatic valves or pressurizing sealed bulk sources and/or intermediate storage vessels to assist in motivation of chemical.

For many applications it is desirable to provide a separate mix tank where the measured proportions of chemicals can be thoroughly combined. As is disclosed, the mix tank may include a variety of means to improve the mixing process, such as heat exchange apparatus to adjust temperature of the chemicals or a gas sparger system or similar apparatus for producing turbulence to aid in the mixing process. This apparatus may also be included on the metered vessels themselves, which is particularly beneficial in instances where mixing of chemicals occurs in the metered vessels.

In addition to chemical mixing/diluting of virtually any form of chemical solution, the present invention encompasses other useful applications, such as serving as a chemical generator, or as a low-volume chemical transfer/dispense apparatus.

DESCRIPTION OF THE DRAWINGS

The operation of the present invention should become apparent from the following description when considered in conjunction with the accompanying drawings, in which:

FIG. 1 is a schematic representation of the diluter/mixer apparatus of the present invention.

FIG. 2 is an enlarged schematic representation of one embodiment of a metered vessel of the present invention.

FIG. 3 is an enlarged schematic diagram illustrating the theory of operation of the constricted vent tubes of the present invention.

FIG. 4 is a schematic representation of another embodiment of the diluter/mixer apparatus of the present invention.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides an improved apparatus and method for precisely mixing chemicals from two or more bulk sources and delivering the mixture to a variety of possible downstream destinations, including end use stations, intermediate storage vessels, and/or independent chemical transfer or dispense apparatus.

Illustrated in FIG. 1 is one embodiment of a diluter/mixer 10 of the present invention. The diluter/mixer 10 includes two metered vessels 12a, 12b. The first metered vessel 12a receives chemical from a bulk source 16 through a first chemical inlet 18 and a first intake line 20. The second metered vessel 12b receives chemical from a bulk source 22 through a second chemical inlet 24 and a second intake line 26.

In the embodiment shown, chemical exits each of the metered vessels 12a, 12b through a dispense line 28, 30 to a mix tank 32 where the chemicals are combined in the manner described below. Once mixing is completed, chemical can then be transferred through a continuation of the dispense line 31 to variety of destinations, such as: intermediate storage vessels 34, 36; chemical transfer/delivery apparatus 38, such as the apparatus disclosed in applicant's U.S. Pat. No. 5,148,945; or one or more point-of-use stations 40.

It should be understood that under certain conditions the mix tank 32 may be eliminated without diminishing the utility of the present invention. Examples of such circumstances are: where intermediate storage vessels or similar receptacles are employed and complete mixing of chemical can occur in the intermediate tanks themselves; and a single vessel diluter/mixer apparatus, such as that shown in FIG. 4 and described below, wherein mixing occurs in the metered vessel.

To accomplish extremely accurate mixing of chemicals, the metered vessels 12 of the present invention are provided with means to amplify the precise fluid level within the vessels as they approach filled capacity. As is shown in FIGS. 1 and 2, each of the metered vessels 12a, 12b, 12c of the present invention comprises a sealed main container 42a, 42b, 42c and a constricted vent tube 44a, 44b, 44c. Once the chemical content of the container 42 reaches the vent tube 44, the pressure of the trapped air in the top of the sealed container 42 will cause chemical to cease filling the container 42 and to begin filling only the tube 44. As is explained below, the greatly constricted capacity of the tube 44 provides a significantly amplified accuracy of measurement of chemical in the metered vessel and permits more accurate cessation of chemical flow into the vessel 12.

The theory of operation of the constricted vent tubes of the present invention can be better understood with reference to FIG. 3. As is illustrated, a reliable yet relatively low cost sensor 46a, 46b might have an effective "bandwidth" of about 1/2 inch. Mounting such a sensor on a container 48 having a volume of V.sub.v, the range of error of the sensor 46a would comprise the volume V.sub.w (i.e. the volume occupied by a 1/2" of chemical across the entire diameter of container 48).

In contrast, by employing the same type of sensor 46b, with the exact same 1/2" bandwidth, on a vent tube 50, the range of error is greatly reduced. In this instance, the range of error is only the volume V.sub.n (i.e. the volume occupied by a 1/2" of chemical across the much smaller diameter of the vent tube 50). Since the volume V.sub.n is insignificant relative to the volume V.sub.v, this simple modification of the metered vessel provides vastly improved accuracy to the process of filling the vessel without the need of introducing more expensive (and generally less reliable) sensors having narrower bandwidths.

To improve the accuracy of filling the metered vessels 12 further, in the preferred embodiments shown in FIGS. 1 and 2, two sensors 52, 54 are provided to monitor the presence of chemical in the metered vessels 42 and vent tubes 44. The first sensor 52a, 52b, 52c (shown in FIG. 2 mounted on the container 42c near the level of the base of the vent tube 44c, and shown in FIG. 1 mounted on the vent tube 44a, 44b itself) provides a signal when chemical approaches or initially enters the vent tube 44a, 44b, 44c. The second sensor 54a, 54b, 54c is mounted on the vent tube 44a, 44b, 44c and provides a signal when chemical reaches the desired predetermined capacity of each vessel 12a, 12b, 12c. As is explained below, t