WO1999057340A2 - Chemical mixing, replenishment, and waste management system - Google Patents
Chemical mixing, replenishment, and waste management system Download PDFInfo
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- WO1999057340A2 WO1999057340A2 PCT/US1999/009541 US9909541W WO9957340A2 WO 1999057340 A2 WO1999057340 A2 WO 1999057340A2 US 9909541 W US9909541 W US 9909541W WO 9957340 A2 WO9957340 A2 WO 9957340A2
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- control system
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- mix
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
Definitions
- This invention relates generally to systems for controlling chemical processes, and more particularly, to a chemical analyzer system that performs several basic functions, specifically sampling, analysis, mixing, replenishment, and cleanup, and further including the functions of performing diagnostics, auto-calibration, and calculations.
- the invention relates to a system of humidifying nitrogen gas to a predetermined relative humidity level, and to calibration of an on-line pH sensor using an off-line pH sensor.
- a chemical management system such as a system that controls a plating process is required to perform a number of functions, not all of which have been successfully implemented in the prior art.
- a chemical system that employs a NiFe plating bath there is a need that the NiFe plating bath be ready for use on demand.
- a system that manages the plating bath preferably should prepare and hold a new plating bath, and measure and control the bath chemistry. The temperature of the bath should be controlled and adjustments to the quantity of fluid in the bath should be effected by replenishment as evaporation occurs. In addition, it is preferred that the bath be aged by performing dummy plating.
- each set of mixing and holding tanks has a respectively associated chemistry.
- a holding tank and a mixing tank At each such site there may provided a holding tank and a mixing tank.
- the holding tank stores plating solution that is in a condition ready to be used.
- the mixing tank on the other hand, is used to make up plating solution and for dummy plating.
- each such tank is constructed to be chemically inert with respect to the chemistry of the plating solution. Materials that are known to be suitable for this purpose are Teflon® materials and equivalents.
- properly humidified nitrogen blanket reduces dehydration of the plating solution, which would result in elevated concentration thereof.
- a number of system parameters must be monitored and controlled. These included, specifically in a NiFe plating environment, the respective concentrations of Ni and Fe. In addition, the pH of the solution, as well as its density and temperature need to be controlled to within predetermined ranges. Moreover, the dummy plating system, including the plating schedule and the current used therein, must be controlled as must the Fe concentrate during dummy plating.
- an object of this invention to provide a sensor system that simply and economically provides an accurate indication of the quantity of fluid in a tank. It is another object of this invention to provide a simple approach to humidifying nitrogen gas precisely to preclude either evaporation or enlargement of a plating solution in a mix or hold tank.
- this invention provides, in one aspect thereof, a NiFe blend, analyzer, and distribution system.
- This specific illustrative embodiment of the invention is designed to achieve the following principal objectives:
- the following first portion of the system of the invention relates to the Chemical Support Mix and Distribution System. All operational functions are accessible from the
- Precision blending is achieved through the use of high accuracy, low maintenance delivery systems and level sensors for wet chemistry and water additions. Manual, dry chemical additions are assisted by means of operator prompts and instructions and easy access delivery panels.
- the system is designed to accommodate future expansion and retrofit with respect to automated dry chemical delivery systems for chemicals such as sodium saccharin, boric acid, and the like.
- Efficient solution amalgamation is achieved through a combination of variable speed mixing, temperature control (primarily to assist in the dissolution of boric acid), and recirculation.
- Continuous level monitoring provides fault-high, process, and fault- low level control and alarm functions.
- Level monitoring and solution metrology is used together as port of system diagnostics to alert the operator to possible subsystem failures or necessary component calibration(s).
- Solution preparation includes continuous filtration via recirculation through an external heat exchanger.
- the mix tank is equipped with the necessary hardware to allow electroplating to occur inside the vessel.
- the anode and cathode are placed in a separate container from which the solution in the mix tank is reticulated during the dummy plating cycle. Keeping the electrodes separate from the solution in the mix tank avoids further dissolution of the anode, which could affect solution composition and contamination. In addition, this design accommodates easy removal of the anode and cathode assemblies when necessary.
- the system transfers the solution to a holding/distribution tank.
- the solution continues to be monitored for composition assay and temperature. Adjustments are automatically carried out by the metrology control system with respect to composition.
- the temperature is controlled locally at the holding tank, and the metrology control system monitors the temperature and provides operator alerts and alarms should the temperature deviate beyond the user-definable range.
- the holding tank is equipped with continuous level monitoring and control. The primary functions of the level monitoring at the holding tank are (1) fault-high and fault-low monitoring alarming and functional interlocks, (2) automatic adjustment of replenishment calculation based on actual level, and (3) transfer signals in order to request the transfer of solution from the mix tank to the holding tank.
- the system includes connections that allow the solution in the holding tank to be distributed to a "global loop," (the global loop feeds the actual plating reservoirs) and then recirculated back to the holding tank.
- the point of return also includes filtration that is used to filter any particulate that may have been introduced from the global loop.
- the blending and preparation of a new batch of NiFe solution begins.
- the mix tank and the holding tank function together in such manner as to ensure that the holding tank does not run empty or ever be overfilled.
- the solution in the mix tank will not be transferred to the holding tank until it has completed all of its preprogrammed routines for proper solution preparation Solution Maintenance
- Critical parameters of the solution are monitored and controlled using a combination of automated titration technology as well as the incorporation of other subsystem components for monitoring other items, such as direct pH and specific gravity. Continuous filtration is accommodated by recirculating the solution through an external heat exchanger that is designed for heating and cooling requirements. Filter pressures and temperatures are monitored from the System Manager, which will be described below.
- the System Manager additionally provides operator alert and alarms indicating component failures or required maintenance.
- Each filter location is equipped with dual filtration for automatic switching.
- the system senses that one of the filters is building up differential pressure, it will automatically activate the necessary valves in order to switch to a backup filter and alert the operator that the primary filter needs to be changed. Once the automatic switch-over is made, the backup filter will become the primary filter and the newly replaced filler will become the backup.
- This design permits filter maintenance without shutting down the tool or interrupting the supply of solution to the distribution loop System Manager
- the System Manager in a practical embodiment of the invention, is Semi S2-93 and 03 certified and, in a practical embodiment of the invention, provides host communication protocol in either standard ASCII, DDE, or 513C5/GBM (serial or Ethernet). All functions for the blend station and metrology control system including data export, history, maintenance, and reporting, are available from the System Manager
- the System Manager is a computerized control center designed to be very user-friendly. Its use of graphics and data display screens allows the operator to interface with the system effectively and with minimal training.
- the System Manager displays and stores process conditions and analytical results and uses the information to initiate alerts, alarms and other automated control functions such as chemical dispensing, replenishment, cleanup, calibration routines, and the like.
- the chemical control system of the present invention includes in certain embodiments up to four (4) modules: • An automatic chemical analyzer;
- a variable I/O interface for communications and control of remote electro-mechanical devices and computer-based systems; and A PC System Manager for tying all of the modules together into a complete process control and MIS system as well as providing a graphical operator interface with operator alert and alarm reporting.
- LCU variable I/O interface
- PC System Manager for tying all of the modules together into a complete process control and MIS system as well as providing a graphical operator interface with operator alert and alarm reporting.
- the Analyzer is at the heart of the system and provides high accuracy with respect to on-line automatic chemical analysis.
- This analyzer is designed to draw samples automatically from multiple process baths, perform chemical analyses of the process chemistries, and send the results of the analysis to a computerized manager, which will be described below.
- the self calibration and diagnostic routines programmed within the analyzer ensure consistent performance and high accuracy with respect to analytical measurements and chemical monitoring.
- the Replenisher receives chemical addition instructions from the System Manager based either on programmed conditions (actual analytical results versus desired operating ranges) or in response to manually entered operator commands.
- the system is designed to maintain inventories of chemical stocks and deliver reports on chemical usage by the process bath.
- a keypad for remote operational control there is provided a keypad for remote operational control.
- the Local Control Unit monitors physical process parameters such as temperature level, conductivity, pH voltage, etc.
- the LCU Is designed to receive digital or analog signals from local control devices. This information is communicated to the System Manager via a serial link, compared to operator-defined set-points, and is logged into history files. The information is used to provide alert and alarm conditions and to initiate control functions that are serially communicated back to the LCU.
- the LCU then electronically activates the particular hardware that has been predetermined to be required for effecting the required adjustment, e.g., heating and cooling devices, water solenoids, drain valves, etc.
- Primary Automated Routine e.g., Primary Automated Routine
- the primary automated routine of the system of the present invention includes the following steps of operation:
- Solution Maintenance Solution is analyzed for Ni, Fe and/or pH.
- Dummy Plating (Chemical analysis and replenishment can be individually activated or suspended during dummy plating cycle.) Solution is brought to operating temperature electrodes are lowered into solution and current is applied at user-defined settings and for user-defined amp-minutes
- amp-minute replenishment is automatically adjusted based on an analysis result.
- Distribution On Solution is continuously monitored, controlled and aged 17.
- Distribution Off - Level Low System either goes into standby mode, or starts the cleanup routine and then into standby
- Cleanup This routine is user-definable. Spray headers and water fill valves, as well as pumps and mixers, are sequentially assigned to operate as part of the cleanup routine.
- the IBM-compatible PC-based System Manager of the present invention is a standalone unit that coordinates the operation of the other components into a fully integrated network.
- the system provides total control over any chemical process.
- the System Manager records the information it receives into a database and maintains historical records on each process parameter.
- the current parameter values are compared to established set-point limits to provide alert and alarm indications as well as initiate automated control functions.
- the module responsible for controlling each parameter activates the necessary control equipment to return that parameter to its optimum value.
- the System Manager provides the operator with a full-color, menu-driven display of all process information being accumulated by the other modules. The operator is then enabled to access desired information by selecting the appropriate display screen on the system terminal.
- each screen is set with tiered password protection.
- Graphic display screens provide selection and examination of, inter alia:
- Sampling retrieves liquid from a tank, sample loop, or grab sample receptacle and delivers it to the analysis cell.
- the sample syringe is cycled to pump in the sample and purge any other liquid.
- Several cycles of sample are delivered to the beaker to ensure a representative sample.
- both a timer and a sample arrival detector are used to verify that sample arrived in adequate time for the analysis to proceed.
- the beaker is thoroughly cleaned before the final sample dose is dispensed.
- the liquid is either pushed into the analysis beaker by the pressure in the sample loop or drawn in by an eductor. Analysis
- a titration analysis is performed after the sample has been delivered to the cell.
- a titration analysis may be performed with an optional conditioning reagent delivered by gravity through a solenoid valve. Titrant is conveyed by a syringe controlled by a stepper motor. Titrant is continuously added while analog readings are taken in intervals in order to find the endpoint. Once the endpoint is found, the beaker is cleaned and the test is repeated until the results agree within a user-specified tolerance. A minimum of three replicates is required with a maximum of nine is allowed. As soon as the results are satisfactory for noncontiguous analyses, the analyzer performs a thorough cleanup to avoid cross contamination
- the cleanup procedure rinses out all the analyzer components that came in contact with the sample solution. This starts with an air purge through the rotary valve(s) and filters. If the sample fails to clear through the line, an error condition is generated for subsequent analyses warning that the air pressure is low. Once cleared by air, the rinse water, in the form of bursts to maximize the rinsing effect, is turned on and, if used, the sample syringe is cycled until it is cleaned (depending on the process for which the analyzer is being used, there may not be a water rinse of the sampling lines). Following this, the direct fill line to the beaker is cleared. Grab Sample
- Bottled samples may be presented to the Analyzer for analysis at the grab sample sipper port. For optimum results the sample concentration should be within the specification range (alarm limits) of the parameter being tested. Various methods may be used to analyze a grab sample. pH Electrode Calibration
- the pH calibration is performed before an analysis using the pH electrode if a user specified time has elapsed since the last pH calibration.
- the calibration uses two pH buffers to determine the slope and the offset of the pH electrode. A stable reading is obtained on one buffer, then the beaker is cleaned and a reading is taken on the other.
- the slope value in transmitted to the System Manager to enable the operator to know the condition of the electrode.
- the slope and offset values are retained by the analyzer to convert voltage readings to pH values.
- the frequency of calibration is set through the analysis configuration table register titled, in this embodiment, "Hours Calibration Valid. " ORP Electrode Calibration Because the ORP electrode is used for differential, rather than absolute, titrations, calibration is unnecessary. However, determining the sensitivity of the electrode is desirable since can vary with use. Electrode sensitivity, calculated as a ratio of actual response to ideal response, is reported after each analysis and can be viewed at the System Manager with the other Analyzer parameters. Chemical Replenisher
- the replenisher is capable of executing instructions entered at the System Manager.
- the Replenisher simultaneously controls delivery of multiple feedstocks to multiple processes. Flow rates are monitored and when chemical delivery reaches to requested quantity, feed is automatically shut off. The total chemical delivered is recorded by the Replenisher for each feedstock. These values are used to activate low level warnings. The totals and other information are available to the operator and remote computer.
- the chemical blend and distribution system includes a HC1 chemical feedstock cabinet designed to hold two (2) 10L containers of HC1. This system delivers acid to two locations, alert the operator when the acid level is low, and provide an alarm to the operator when empty.
- Some of the hardware and collateral equipment that is employed with this system includes: Pump cart and shelves for containers • Pneumatic valves ( ⁇ 2), pumps ( ⁇ 2) and filters ( ⁇ 2)
- This System is designed to sample and analyze solutions from the two mix tanks and make chemical replenishment adjustments based on the analysis result.
- the metrology system is programmed to execute to following tasks based on a user-defined schedule:
- the System Manager is implemented in an IBM-compatible PC and is designed to provide operator control of all routines and electro-mechanical and computerized components and subsystems.
- This System Manager also provides operator alert and alarms as well as complete history, charts and graphs on all parameters monitored and, or controlled by the System.
- the parameters include:
- Process control parameters include:
- Feedstock filter pressures Recirculation flow rate Mix tank temperatures Mix tank levels Density Nickel Iron pH
- the control system employs a mix container for containing a plating solution and a hold container for containing a plating solution that has been delivered thereto from the mix container. Delivery of a precise predetermined quantum of a predetermined constituent of the plating solution is effected by a precision delivery arrangement. The quantum of predetermined constituent is delivered to the mix and hold containers by a precision delivery arrangement. Plating solution is transferred between the mix and hold containers by a transfer pump.
- a nitrogen gas source provides a nitrogen gas that is humidified to a predetermined relative humidity with respect to the temperature of the solution in the respective mix or hold container to which it is delivered. This humidified nitrogen prevents evaporation of the plating solution and also prevents the plating solution from acquiring or releasing water.
- the nitrogen gas is humidified by bubbling same through a column of deionized water that is in thermal communication with the tank of chemical solution.
- the humidified nitrogen gas is then released to the tank where it forms a layer over the plating solution, as described.
- the extent to which the nitrogen gas is humidified is to an extent a function of the depth in the column at which the nitrogen source gas is placed to release the nitrogen source gas in the deionized water.
- Each of the mix and hold tanks is provided with a associated column of deionized water for effecting the control of the relative humidity of the nitrogen gas.
- a pneumatic pump having a pump inlet for receiving a chemical to be delivered and an outlet for issuing the pumped chemical is coupled to an orifice of predetermined internal dimension.
- the orifice is then coupled to a flow meter for providing an indication of the rate of flow of the chemical through the orifice.
- the pneumatic pump is a positive displacement, double diaphragm pump.
- the pneumatic pump is configured to pump a chemical at a chemical flow rate of approximately 50 ml per minute to approximately 2 liters per minute.
- the chemical is caused to flow at a rate of approximately
- the pneumatic pump has a rated flow rate of approximately between 2 and 10 times the chemical flow rate, and preferably at least approximately four times the chemical flow rate.
- the orifice has an internal diameter of approximately 0.010" and 0.090". In a practical embodiment of the invention, the internal diameter is approximately between 0.030" and
- FIG. 1 is a partially schematic plan illustration of an analyzer manager system that analyzes and controls the chemistry in a chemical processing system, particularly Ni (nickel), Fe (iron), and pH, in this specific illustrative embodiment of the invention;
- Fig. 2 is a partially schematic plan illustration of a chemical replenisher system that, in this specific illustrative embodiment of the invention, replenishes HCl and Fe feedstocks, as well as deionized (DI) water;
- DI deionized
- Figs. 3-5 are top, end, and front plan representations, respectively, of a NiFe blend and distribution system constructed in accordance with the invention
- Fig. 6 is a schematic illustration of a system that controls the chemistry in hold and mix tanks of a NiFe plating system
- Fig. 7 is a representation of a graphical user interface (GUI) screen of a status condition of the system as represented in the logic controller
- Fig. 8 is a representation of a graphical user interface (GUI) screen of an analyzer condition of the system as represented in the logic controller.
- GUI graphical user interface
- Fig. 1 is a partially schematic plan illustration of an analyzer manager system that analyzes and controls the chemistry in a chemical processing system.
- an analyzer 100 analyzes the nickel (Ni) iron (Fe) and pH components and characteristics of a chemical bath (not shown in this figure), which in this embodiment of the invention is a plating solution.
- All control software embodied in analyzer 100 is written in a flow chart language tool designed by Opto 22. The use of this software greatly reduces startup, maintenance, and upgrade, as well as revision costs.
- This flow chart language tool allows the entire program to be viewed, executed, monitored, and modified in flow chart form. In a diagnostic mode, the flow chart symbols are highlighted as they are executed, and such execution can be stopped, single-stepped, or interrogated at will.
- the subject flow chart language tool is commercially available and has associated therewith a broad array of digital and analog I/O hardware that is readily integrated with the software to provide a complete package.
- Fig. 2 is a partially schematic plan illustration of a chemical replenisher system that, in this specific illustrative embodiment of the invention, replenishes HCl and Fe feed stocks.
- the replenisher supplies deionized water.
- Replenisher 200 is shown to be provided with certain stores of the feed stocks and the deionized water to be dispensed. Deionized water is maintained in region 201 of replenisher 200. HCl is stored in region 202, and Fe is contained in region 203. The substances stored in this replenisher are provided to hold and mix tanks, as will be described below with respect to Fig. 3.
- replenisher 200 is provided with a local water gun 205 that provides a source of deionized water for the rinsing of components and for emergency washing.
- Figs. 3-5 are top, end, and front plan representations, respectively, of a NiFe blend and distribution system 300.
- Distribution system 300 is shown to have a mix tank 302, a hold tank 303, a heater/chiller 304, a compartment 305 for pumps, filters, and valves, as well as a secondary containment region 307.
- Mix tank 302 is provided with a mixer 310 that functions to create a vortex pattern (not shown) beginning along the side of mix tank 302 near the top, and extending at the center of the tank at the bottom. The vortex pattern, therefore, sweeps all areas of the tank.
- the mixer is placed off- center and at an angle to maximize the shearing action and the mixing effect.
- mix tank 302 and hold tank 303 are lined with Teflon® material (not specifically designated). It is desired to eliminate most tank seams (not shown) while maintaining the Teflon® material in contact with the solutions (not shown in this figure).
- Teflon® material not specifically designated. It is desired to eliminate most tank seams (not shown) while maintaining the Teflon® material in contact with the solutions (not shown in this figure).
- seamless tanks are provided formed of high purity grade PVDF.
- secondary containment region 307 is configured to be about half of the height of mix tank 302 and hold tank 303.
- secondary containment region 307 has a capacity of approximately 1500 gals, which corresponds to approximately 1 10% of the combined volumes of the hold and mix tanks.
- the containment region has sufficient volume to accommodate all pumps and plumbing.
- Fig. 6 is a schematic illustration of a chemical processing system 400 that controls the chemistry in hold and mix tanks, 302 and 303, respectively, of a NiFe plating system. Elements of structure that have previously been described are similarly designated.
- Mix tank 302 is shown to contain a plating solution 402 that is at a level lower than a high alarm level 403.
- mix tank 302 has a 200 gallon capacity and is operated at 106 gallons (400 liters)
- hold tank 303 has a capacity of 250 gallons, and is operated at 220 gallons (1000 liters). All liquid delivery to the mix tank is monitored with the use of flow sensors, thereby achieving a reproducibility, in this embodiment, of ⁇ 2%.
- level of accuracy can be made to approach the level of reproducibility with proper calibration.
- the flows of all liquids into mix tank 302 are confirmed with an in-tank level sensor 405 that provides a means of cross-checking between the flow sensor and the liquid level sensor.
- level sensor 405 is configured to operate within its most linear and repeatable range. This enables the fluid to be delivered in a stable manner over a long period of time, without requiring recalibration after short periods of time.
- level sensor 405 is a pneumatic device that facilitates continuous level sensing. This form of sensor is precise and trouble-free, and unlike external proximity sensors, will not falsely be activated by a light crystalline tank wall build-up or other changes in environmental conditions, such as humidity.
- the present pneumatic sensors are not affected by tank wall build-up, foam, stirring, temperature, humidity, RF interference, or electrical noise. The present pneumatic sensors usually will not require adjustments after installation.
- level sensor 405 provides a continuous measurement along the full depth of mixing tank 302. This significant feature allows an immediate inventory of contents of the tank that is used by the control software (not shown) for continuous monitoring of pump performance and for confirmation of flow sensor accuracy.
- the gas flow rate in the level sensor is very low, on the order of 10 cc/min, so as to minimize dehydration of the plating solution.
- the inventor herein has discovered through testing that the low gas flow rate level sensor has essentially no detectible effect on the process resulting from dehydration.
- Nitrogen 407 is delivered to mix tank 302 in a particularly advantageous manner.
- the tank nitrogen ventilation gas is humidified to prevent dehydration/concentration of the solutions.
- a vertical column 408 of deionized water is provided in communication with mix tank 302, and receives aerated nitrogen in the form of fine bubbles whereby the nitrogen gas becomes humidified.
- Deionized water is slowly supplied to column 408 through a needle valve 409, and overflows through an inverted U-tube 410 that maintains a predetermined level and prevents nitrogen gas from escaping.
- the relative humidity can be controlled by the extent of immersion of the nitrogen gas outlet within column 408.
- liquid column 408 is attached to the side of the mix tank and is insulated so that the temperature in the water column is identical to that of the plating solution, thereby assuring the correct humidity relative to the solution tank in air space conditions.
- the humidified nitrogen gas is then delivered to mix tank 302 so as to form a gas blanket over plating solution 402. This method prevents over humidifying of the nitrogen gas, which would cause solution growth, such as can occur with conventional fog humidifiers when they are imbalanced.
- Hold tank 303 is supplied with a level monitoring arrangement 415 that is similar to that described hereinabove with respect to mix tank 302.
- a nitrogen gas 417 is delivered into a column 418 to create bubbles of nitrogen gas therein.
- Deionized water is conducted to the column via a needle valve 419, the excess deionized water being permitted to drain out of U-shaped outlet 420.
- the nitrogen gas is humidified in a manner similar to that discussed hereinabove with respect to liquid column 408.
- Deionized water is provided to the mix and hold tanks.
- a source of deionized water 430 is conducted via respective pressure regulators 431 and 432 and pneumatic valves 435 and 436 to the mix and hold tanks.
- the deionized water enters the tanks as a spray so that as each tank is rinsed or filled, all areas are reached.
- the pressure regulators ensure that a full cone and consistent rate of flow are achieved out of each spray head. In a practical embodiment of the invention, it is important to maintain adequate constant pressure, as fluctuating pressures will compromise cleaning effectiveness and will generate unnecessary control system flow rate warnings.
- the solution that is transferred from mix tank 302 to hold tank 303 is motivated by a bellows pump 450 that operates pneumatically in response to air supplied from a regulated and filtered air supply 451 and an electric valve 452. It is preferred that the solution thus transferred be temperature adjusted prior to entering hold tank 302. Otherwise, it would be difficult to maintain the hold tank temperature within a specified ⁇ 0.1 °C during the transfer.
- Fluid from hold tank 303 is conducted to a plating process 460 (not shown) by operation of a bellows pump 465.
- This pump operates in response to air supplied from source 451 and controlled via an electric valve 467.
- a back-up recirculation pump 469 that serves to minimize system down time when pump maintenance is required.
- pump switch-over is performed automatically upon operator request, which controls pneumatic valves 470.
- Bellows pumps 465 and 469 are ultrapure Teflon® bellows-type manufactured by White Knight. The model AT300 bellows pump delivers 10 to 20 gpm, depending upon the pressure head. These pumps are suitable for the hold/distribution tank recirculation loop.
- a model ATI 00 bellows pump delivers 5 to 8 gpm and is suitable for mix tank recirculation, filtration, and transfer to the hold tank (bellows pump 450). Since these pumps are characterized by low pulsations, a pulse dampener is not commonly used therewith.
- bellows pumps 465 and 469 these pumps are associated with respective ones of pneumatic valves 470 and filters 477.
- Control over valves 470 permit automatic switching of the bellows pumps and the filters, facilitating pump maintenance and filter replacement.
- the automatic switch is responsive to a differential pressure that is developed across the filters, and which is monitored by differential pressure sensor 478.
- each level is of a sequentially finer size to prevent early loading of the filters and provide finer filtration where it is needed most.
- the first stage of filtering is in the form of strainers 473 having a 10 micron size locate at the feed stock outlets.
- the second level of filtration corresponds to filters 475 at the outlet of mix tank 302. Filters 475 are 1 micron filters.
- the third level of filtration corresponds to 0.2 micron filters 477 at the outlet of hold tank 303.
- Ball valves 480 which may be manually operated, are provided to permit equipment to be isolated for shut down and maintenance purposes.
- pumps 510 and 51 1 are pneumatic, positive displacement, double diaphragm pumps that by virtue of their being pneumatically operated, achieve a limited maximum closed flow pressure, but nevertheless achieve a reasonably high dynamic range.
- Commercially available pumps that are suitable for the practice of this aspect of the invention are available from ARO.
- WILDEN Model P.025 pumps are used. These pumps are relatively inexpensive and require minimal maintenance, yet, as will be described herein, they achieve high accuracy and precise delivery of chemical.
- pump 510 is arranged to pump HCl from an HCl source in region 202, and pump 51 1 is arranged to pump Fe from a Fe source also in region 202.
- the HCl source is a 10 liter bottle
- the Fe source is a 40 liter tank.
- Each of pumps 510 and 51 1 is coupled at its output to a respectively associated one of orifices 513 and 514.
- the orifices have an internal diameter of approximately between 0.010" and 0.090".
- the orifices have an internal diameter of approximately between 0.030" and 0.060".
- the internal diameter is between 0.040" and 0.050".
- the orifices are coupled to respective ones of flow meters 516 and 517 which in this embodiment of the invention are conventional paddle wheel style flow meters.
- pH sensors In order to provide continuous and accurate pH readings, two pH sensors are used.
- One pH sensor (not shown) is located in analyzer 100 which is auto-calibrated daily, or at some other specified interval.
- this off-line pH sensor provides better than ⁇ 0.02 pH accuracy and ⁇ 0.01 pH repeatability.
- the off-line pH sensor which is off-line (i.e., not subjected continuously to the sample of the chemical solution being used in the plating system) is subjected to a calibrating solution of known pH value, and a reading is taken.
- the off-line pH sensor is subjected to a sample of the same batch to which the on-line pH sensor is being subjected (i.e., the on-line sample), and a second reading is taken.
- This second reading is compared to the reading of the on-line pH sensor, which is pH sensor 485 located in hold tank 303.
- the difference between the readings of the on-line and offline pH sensors on the sample solution constitutes a correction that is added to achieve an accurate value of the pH of the sample solution.
- the on-line sensor is immersed and provides continuous process readings. The sensor is corrected to read the same as the calibrated (off-line) sensor whenever a pH reading is read in the calibrated system. Deviations exceeding a user-defined amount are reported as warnings.
- a high quality research grade pH sensor drifts on the order of 0.002 pH per day, and a typical offset value used to effect the present correction is ⁇ 0.01 pH.
- Specific gravity is monitored by a specific gravity unit 487.
- This specific gravity monitor is an Anton Paar Model DPR407NYB transducer that is located in the recirculation loop. This commercially available specific gravity sensor has a published repeatability of ⁇ 0.00001 g/ml.
- specific gravity sensor 487 may be provided with an associated partial by-pass valve (not shown) to prevent it from causing too much flow restriction.
- mixing time is minimized in mix tank 302 by a liquid ejector (not shown) on the inlet line to the tank.
- a liquid ejector (not shown) on the inlet line to the tank.
- the liquid ejector is a passive device that requires no power or special maintenance, as opposed to a mixer, or high speed pump.
- Fig. 6 additionally shows anodes 490 that are electrically coupled to a rectifier 491 for effecting the dummy plating.
- a small plating cell (not shown) located above mix tank 302 is provided to allow dummy plating to occur in a separate, more accessible area. This would allow the anodes and cathodes to be isolated from the mix solution and rinsed at any time, independent of mix tank activity.
- recirculating NiFe solution may be routed through the plating cell and overflowed to mix tank 302 or by-passed and routed directly to the mix tank.
- the figure shows a heat exchanger 495 at the exit of hold tank 303. This enables supplying solution to the recirculation loop at the most consistent and stable temperature.
- Heat exchanger 495 is a water-jacketed device located just prior to the recirculation loop. Thus, accuracy is maintained and offsets are prevented that would result from varying demand or flow rates.
- the temperature of the heating water is regulated according to the desired NiFe solution exit temperature, and not the internal water temperature. Other forms of heaters may be used in the practice of the invention.
- Fig. 7 is a representation of a graphical user interface (GUI) screen of a status condition of the system as represented by the logic controller (not shown).
- GUI graphical user interface
- a screen 500 which may be in the form of a conventional cathode ray tube, illustrates a variety of status conditions for system 400.
- Screen 500 is but one of a number of arrangements that can be provided to illustrate the status conditions of the system.
- selection of appropriate buttons yields other screens that provide information relating to system history, indication of whether a particular tank is on-line, replenishment status, error conditions, etc.
- Fig. 8 is a representation of a graphical user interface (GUI) screen 501 of an analyzer condition of the system, as represented by the logic controller (not shown).
- this screen depicts a schematic sample process and provides indication of the parameters in the ongoing analysis. Again, this is but one of several display formats that can be employed in the practice of the invention.
- the invention has been described in terms of specific embodiments and applications, persons skilled in the art can, in light of this teaching, generate additional embodiments without exceeding the scope or departing from the spirit of the claimed invention. Accordingly, it is to be understood that the drawing and description in this disclosure are proffered to facilitate comprehension of the invention, and should not be construed to limit the scope thereof.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Automation & Control Theory (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000547288A JP2002513861A (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment and waste management systems |
US09/674,635 US7147827B1 (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment, and waste management system |
AU37789/99A AU3778999A (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment, and waste management system |
EP99920246A EP1080253A2 (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment, and waste management system |
KR1020007012130A KR20010052287A (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment, and waste management system |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US8381198P | 1998-05-01 | 1998-05-01 | |
US60/083,811 | 1998-05-01 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO1999057340A2 true WO1999057340A2 (en) | 1999-11-11 |
WO1999057340A3 WO1999057340A3 (en) | 2000-02-03 |
Family
ID=22180863
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1999/009541 WO1999057340A2 (en) | 1998-05-01 | 1999-04-30 | Chemical mixing, replenishment, and waste management system |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP1080253A2 (en) |
JP (1) | JP2002513861A (en) |
KR (1) | KR20010052287A (en) |
AU (1) | AU3778999A (en) |
WO (1) | WO1999057340A2 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003085173A2 (en) * | 2002-04-03 | 2003-10-16 | Gene Chalyt | Reference electrode calibration for voltammetric plating bath analysis |
US7913644B2 (en) * | 2005-09-30 | 2011-03-29 | Lam Research Corporation | Electroless deposition system |
US7972652B2 (en) * | 2005-10-14 | 2011-07-05 | Lam Research Corporation | Electroless plating system |
AT13262U1 (en) * | 2012-05-16 | 2013-09-15 | Koerner Chemieanlagen | analyzer |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4303484B2 (en) | 2003-01-21 | 2009-07-29 | 大日本スクリーン製造株式会社 | Plating equipment |
KR101679351B1 (en) | 2015-06-11 | 2016-11-24 | 와이엠티 주식회사 | Mixed solution analysis sensor and mixed solution management system using the sensor |
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JPS6230898A (en) * | 1985-07-31 | 1987-02-09 | Sumitomo Metal Ind Ltd | Method and apparatus for replenishing metallic component to plating bath |
JPH04314883A (en) * | 1991-04-15 | 1992-11-06 | Nippon Steel Corp | Tin electroplating method |
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1999
- 1999-04-30 AU AU37789/99A patent/AU3778999A/en not_active Abandoned
- 1999-04-30 KR KR1020007012130A patent/KR20010052287A/en not_active Application Discontinuation
- 1999-04-30 EP EP99920246A patent/EP1080253A2/en not_active Withdrawn
- 1999-04-30 JP JP2000547288A patent/JP2002513861A/en active Pending
- 1999-04-30 WO PCT/US1999/009541 patent/WO1999057340A2/en not_active Application Discontinuation
Patent Citations (5)
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US3602033A (en) * | 1969-06-30 | 1971-08-31 | Exxon Production Research Co | Calibration method for percent oil detector |
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US5352350A (en) * | 1992-02-14 | 1994-10-04 | International Business Machines Corporation | Method for controlling chemical species concentration |
US5342527A (en) * | 1992-06-30 | 1994-08-30 | Hospal Industrie | Method for the calibration of a pair of sensors placed in a dialysis circuit |
US5510018A (en) * | 1993-11-30 | 1996-04-23 | Danieli & C. Officine Meccaniche Spa | System to re-circulate treatment material in processes of surface treatment and finishing |
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Title |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003085173A2 (en) * | 2002-04-03 | 2003-10-16 | Gene Chalyt | Reference electrode calibration for voltammetric plating bath analysis |
WO2003085173A3 (en) * | 2002-04-03 | 2004-04-15 | Gene Chalyt | Reference electrode calibration for voltammetric plating bath analysis |
US6733656B2 (en) * | 2002-04-03 | 2004-05-11 | Eci Technology Inc. | Voltammetric reference electrode calibration |
CN100412541C (en) * | 2002-04-03 | 2008-08-20 | 吉恩·查雷特 | Reference electrode calibration for voltammetric plating bath analysis |
US7913644B2 (en) * | 2005-09-30 | 2011-03-29 | Lam Research Corporation | Electroless deposition system |
US20110135824A1 (en) * | 2005-09-30 | 2011-06-09 | Ron Rulkens | Electroless Deposition System |
US7972652B2 (en) * | 2005-10-14 | 2011-07-05 | Lam Research Corporation | Electroless plating system |
US20110214608A1 (en) * | 2005-10-14 | 2011-09-08 | Igor Ivanov | Electroless Plating System |
US8622017B2 (en) * | 2005-10-14 | 2014-01-07 | Lam Research Corporation | Electroless plating system |
AT13262U1 (en) * | 2012-05-16 | 2013-09-15 | Koerner Chemieanlagen | analyzer |
Also Published As
Publication number | Publication date |
---|---|
AU3778999A (en) | 1999-11-23 |
WO1999057340A3 (en) | 2000-02-03 |
KR20010052287A (en) | 2001-06-25 |
EP1080253A2 (en) | 2001-03-07 |
JP2002513861A (en) | 2002-05-14 |
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