WO2021245000A1 - Installation et procédé de distribution d'un mélange de gaz - Google Patents
Installation et procédé de distribution d'un mélange de gaz Download PDFInfo
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- WO2021245000A1 WO2021245000A1 PCT/EP2021/064478 EP2021064478W WO2021245000A1 WO 2021245000 A1 WO2021245000 A1 WO 2021245000A1 EP 2021064478 W EP2021064478 W EP 2021064478W WO 2021245000 A1 WO2021245000 A1 WO 2021245000A1
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- Prior art keywords
- gas
- flow
- flow rate
- setpoint
- gas mixture
- Prior art date
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/2201—Control or regulation characterised by the type of control technique used
- B01F35/2202—Controlling the mixing process by feed-back, i.e. a measured parameter of the mixture is measured, compared with the set-value and the feed values are corrected
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D11/00—Control of flow ratio
- G05D11/02—Controlling ratio of two or more flows of fluid or fluent material
- G05D11/13—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/10—Mixing gases with gases
- B01F23/19—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2111—Flow rate
- B01F35/21112—Volumetric flow rate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2113—Pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2211—Amount of delivered fluid during a period
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05B—CONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
- G05B11/00—Automatic controllers
- G05B11/01—Automatic controllers electric
- G05B11/36—Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential
- G05B11/42—Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential for obtaining a characteristic which is both proportional and time-dependent, e.g. P. I., P. I. D.
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D11/00—Control of flow ratio
- G05D11/02—Controlling ratio of two or more flows of fluid or fluent material
- G05D11/13—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means
- G05D11/131—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means by measuring the values related to the quantity of the individual components
- G05D11/132—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means by measuring the values related to the quantity of the individual components by controlling the flow of the individual components
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D11/00—Control of flow ratio
- G05D11/02—Controlling ratio of two or more flows of fluid or fluent material
- G05D11/13—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means
- G05D11/135—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means by sensing at least one property of the mixture
- G05D11/138—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means by sensing at least one property of the mixture by sensing the concentration of the mixture, e.g. measuring pH value
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D7/00—Control of flow
- G05D7/06—Control of flow characterised by the use of electric means
- G05D7/0617—Control of flow characterised by the use of electric means specially adapted for fluid materials
- G05D7/0623—Control of flow characterised by the use of electric means specially adapted for fluid materials characterised by the set value given to the control element
Definitions
- the present invention relates to an installation for distributing a gas mixture intended for use by a gas consuming unit.
- the installation allows distribution of the mixture directly to the site of use as well as an adjustment of the mixture flow rate produced by the installation according to the flow rate consumed by the consumer unit.
- the invention also relates to a method for distributing a mixture using such an installation.
- an installation and a method according to the invention are intended to distribute mixtures of pure gases or of premixes of gases, in particular to distribute mixtures of gases extracted from air, such as nitrogen, argon. , oxygen, helium, hydrogen, hydrocarbons such as propane.
- air such as nitrogen, argon. , oxygen, helium, hydrogen, hydrocarbons such as propane.
- gas consuming unit can mean both a single consuming entity and several entities supplied in parallel by the gas mixture, in particular several entities arranged downstream of a junction box.
- gas mixtures are packaged in compressed or liquefied form in gas cylinders.
- the filling of a gas cylinder is carried out in sequential mode, the constituents of the mixture being introduced one after the other into the cylinder.
- the quantity of gas introduced into the bottle is checked, either by monitoring the pressure in the bottle during and after the introduction of the constituent, or by weighing the bottle during the introduction of the constituent.
- Such an installation for conditioning gas mixtures is described in particular in document WO2010 / 031940A1.
- the maximum tolerance for variation of the effective values of the concentrations from the target values may be 10% (% relative), or even 5% or even less. Such tolerances are all the more difficult to comply with as the number of constituents is large and / or as their contents are low.
- current conditioning methods may prove insufficient.
- the manometric conditioning by pressure control offers a precision which is intrinsically limited by the precision of the pressure sensor and by the variations in temperature which influence the calculation of the quantity of gas. Added to the uncertainty in the concentration values of the gas mixture produced are the differences in concentrations between the mixtures packaged in different bottles. Such deviations can significantly vary the results produced by the consuming unit at each bottle change.
- Gravimetric conditioning by weighing the constituents offers greater precision on the composition of the mixture but still requires a step-by-step process with filling of bottles.
- the blends are bottled in packaging centers specially designed for this type of operation.
- the bottles must then be transported to their site of use, which requires dedicated logistics. Constraints related to the transport of dangerous goods can also arise, in particular when it comes to transporting gas mixtures with flammable, pyrophoric, toxic and / or anoxic components.
- the object of the invention is to overcome all or part of the drawbacks mentioned above, in particular by proposing an installation for distributing a gas mixture making it possible to precisely control the composition of the mixture, while offering continuity and flexibility of distribution. , depending in particular on the needs at the point of consumption of the mixture.
- the solution of the invention is an installation for distributing a gas mixture comprising:
- a mixing device fluidly connected to the source of first gas and to the source of second gas, said mixing device being configured to produce at an outlet a gas mixture comprising the first gas and the second gas,
- a first flow regulator member and a second flow regulator member configured to regulate respectively the flow rate of the first gas and the flow rate of the second gas flowing to the mixing device according to a first flow rate setpoint and a second flow rate setpoint defining in operation, a production flow rate of the gas mixture at the outlet of the mixing device,
- control unit configured to control the first and second flow regulator members so as to adjust the first flow setpoint and the second flow setpoint according to respective proportions with respect to the production flow, said respective proportions being determined as a function of 'at least a target content of the gas mixture of the first gas and / or the second gas,
- a buffer tank fluidly connected to the outlet of the mixing device on the one hand and to a distribution line on the other hand, the distribution line being configured to distribute the gas mixture to a consumer unit with a consumption rate representative of '' variable consumption of the gas mixture,
- the control unit being connected to the measurement sensor and configured to generate a first control signal from the first measurement signal, the flow regulating members being configured to adjust the first flow setpoint and the second flow setpoint in response to said first control signal.
- the invention may include one or more of the characteristics set out below.
- the installation comprises a first loop for controlling the first and second flow setpoints on the first measurement signal supplied by the measurement sensor, said first loop comprising:
- a first comparator arranged within the control unit (5) and configured to generate at least a first error signal from the first measurement signal
- a first corrector arranged within the control unit, in particular of the proportional, integral and derivative type, and configured to generate the first control signal from the first error signal,
- the measuring sensor includes a flow sensor or flow meter configured to measure the consumption flow rate.
- the first comparator is configured to generate at least a first error signal representative of a variation in the consumption flow rate and the first corrector is configured to generate a first control signal controlling a movement of the first and second flow regulating members so that the first and second flow rate setpoints vary in the same direction as that of the flow rate variation.
- the measurement sensor includes a pressure sensor configured to measure the pressure prevailing in the buffer tank.
- the first comparator is configured to generate a first error signal representative of a variation in the pressure in the buffer tank and the first corrector is configured to generate at least a first control signal controlling a movement of the first and second flow regulating members so that the first and second flow setpoints vary in a direction opposite to that of the pressure variation.
- the first comparator is configured to generate at least a first error signal from a comparison of the first measurement signal with at least one parameter chosen from: a low pressure threshold, a high pressure threshold.
- Each of the first and second flow rate regulating members can move between a closed position in which the first flow setpoint or the second flow setpoint is zero and a fully open position in which the first flow setpoint or the second flow setpoint have respectively a first maximum flow rate value or a second maximum flow rate value, the first and second flow regulating members being able to occupy at least one intermediate position between the closed position and the open position with said intermediate position preferably corresponding to a first setpoint of flow rate or a second flow rate setpoint equal to at least 25%, more preferably at least 35%, of its respective first or second maximum value.
- the buffer tank has an internal volume equal to at least half of the maximum production rate of the installation.
- the installation comprises a first analysis unit arranged downstream of the buffer tank and configured to analyze at least one content of the first gas and / or the second gas of the mixture distributed by the supply line.
- the installation comprises a second analysis unit configured to measure at least one content of the first gas and / or the second gas of the gas mixture produced at the first outlet of the mixing device and to supply consequently at least a second signal of measurement, the control unit being connected to the second analysis unit and configured to generate a second control signal from the second measurement signal and to modify the proportion of the first flow setpoint and / or the proportion of the second flow setpoint relative to the production flow rate in response to said second control signal.
- the installation includes a second control loop of the respective proportions of the first flow setpoint and / or of the second flow setpoint with respect to the production flow rate on the second measurement signal supplied by the second analysis unit, the second loop comprising:
- a second comparator arranged within the control unit and configured to generate at least a second error signal from a comparison of the second measurement signal with at least one parameter chosen from: a target content in the first gas, a target content of the second gas,
- a second corrector arranged within the control unit, in particular of the proportional, integral and derivative type, and configured to generate the second control signal from the second error signal,
- the actuators of the first and / or second flow regulator members being connected to the second corrector and configured to move the first and / or second flow regulator members in respective positions in which the proportions of the first flow setpoint and / or second flow setpoint relative to the production flow rate comply with the second control signal.
- the control unit includes a man-machine interface comprising:
- an input interface in particular a touch screen, configured for input by a user of at least one target content of the first gas and / or of the second gas in the gas mixture
- At least one calculation rule for calculating, from said target content, the predetermined proportions of the first flow rate instruction and / or of the second flow rate instruction relative to the production flow rate.
- the installation is located at the place of use of the gas mixture by the consuming unit.
- the invention relates to a method of distributing a gas mixture comprising the following steps: a. passage of the first gas through a first flow regulator member so as to distribute the first gas with a first flow rate setpoint to a mixing device, b. passage of a second gas through a second flow regulator member so as to distribute the second gas with a second flow rate setpoint to the mixing device, c. production by an outlet of the mixing device of a gas mixture comprising the first gas and the second gas with a production flow rate, d.
- Fig. 1 shows schematically the operation of an installation according to one embodiment of the invention
- Fig. 2 schematically shows a first servo loop according to one embodiment of the invention
- Fig. 3 shows an example of the change over time of the pressure in the buffer tank and the production flow rate of the installation
- Fig. 4 shows an example of the change over time of the gas mixture flow rate distributed by an installation according to one embodiment of the invention with the content of a constituent of the mixture measured during this change
- Fig. 5 represents an enlargement of the curve relating to the measured content of FIG. 3.
- Figure 1 shows an installation according to the invention comprising a source of first gas 1 and a source of second gas 2.
- the first gas 1 and the second gas 2 are of different nature. They can be pure, simple or compound substances, or premixes of several pure substances, in particular one pure substance diluted with another.
- Each of the gas sources can be a gas bottle, typically a bottle that can have a water volume of up to 50 L, a set of bottles connected together to form a frame of bottles or a larger capacity tank, in particular a capacity up to 1000 L, such as a cryogenic storage tank or a tank fitted on a truck-trailer.
- the sources dispense fluids in the gaseous state. Before distribution, fluids can be stored in the gaseous state, in the liquid state, i. e. liquefied gas or two-phase liquid / gas.
- Figure 1 illustrates the case where the installation is configured to produce a binary gas mixture, i. e. two-component, from two gas sources.
- a binary gas mixture i. e. two-component
- an installation according to the invention could include more than two gas sources and produce mixtures with more than two constituents, in particular mixtures of ternary or quaternary gases.
- Each of the sources of the first gas and of the second gas is connected by a first pipe 21 and a second pipe 22 to respective first and second flow regulating members 41, 42. These are provided to regulate the flows of the first gas and of the second gas.
- the pipes 21, 22 meet at a connection point 31 located upstream of the mixing device 3 to form a common portion of pipe connected to an inlet 32 of the device mixer. A mixture of the first and second gases thus enters the device 3 to be further mixed and homogenized therein. Note that it is also possible for the pipes 21, 22 to each open into two separate inlets 32a, 32b of the mixing device 3.
- each of the pipes 21, 22 is provided with a pressure reducer and a pressure sensor in order to measure and control the pressure prevailing in these. pipelines.
- the pressures of the first and second gases can each be kept constant, typically at a value between 1 and 10 bar.
- Each flow rate regulator member 41, 42 can be any means configured to regulate, regulate, adjust the flow rate of a fluid to bring it to a flow rate value closest to the desired value.
- the flow rate regulating members 41, 42 each comprise a flow rate sensor, or flow meter, associated with an expansion member, such as a valve, for example a valve with proportional adjustment.
- the valve can be pneumatic or piezoelectric, analog or digital.
- the valve comprises a movable part, typically at least one shutter, which is placed in the fluid flow and whose movement makes it possible to vary the passage section, and thus to vary the flow to bring it to the set value.
- the flow regulator members 41, 42 can be mass flow regulators comprising a mass flow sensor and a proportional control valve. Note that even if the regulation is based on a measurement of the mass of fluid, the set and measured flow rate values are not necessarily expressed in mass.
- a volume flow setpoint can be expressed as a percentage of opening of the proportional control valve, to which corresponds a voltage value to be applied to the control valve of the regulator.
- the conversion between percentage opening in mass or volume flow value is done by knowing the nominal value of the regulated flow for 100% opening.
- the valve is piezoelectric.
- This type of valve offers high precision, good reproducibility, allowing the voltage applied to the valve to be monitored.
- Such valves are also insensitive to magnetic fields and radiofrequency noise. Their energy consumption is low with minimal heat generation.
- the metal-to-metal control surface reduces or even eliminates reactions with the gas.
- the first and second flow regulating members 41, 42 make it possible to regulate respectively the flow of the first gas and the flow of the second gas entering the mixer 3 according to a first flow setpoint D1 and a second flow setpoint D2.
- the gas mixture leaves with a production flow rate DP which corresponds, in the case of an installation with two gas sources, to the sum of the two flow rates D1 and D2 of first and second gas.
- the installation comprises for example a source of a third gas
- the flow rate DP will be the sum of the flow rates D1, D2, D3 regulated by the corresponding flow rate regulating members 41, 42, 43 towards the mixing device 3.
- the installation according to the invention further comprises a control unit 5 which is connected to the first and second flow regulator members 41, 42 so as to control their operation, in particular so as to adjust the setpoint values D1, D2 for bring them to values which are determined and adapted according to the operating conditions of the installation.
- the flow regulating members 41, 42 each advantageously comprise a closed loop system which is given flow setpoints by the control unit 5. These setpoints are then compared by the closed loop system with the values. measured by the flow rate regulating members 41, 42 and their positions are adjusted by said system accordingly to send the flow rates as close as possible to D1, D2 to the mixing device 3.
- control unit 5 comprises a programmable logic controller, also called a “PLC” system for “Programmable Logic Controller” in English, that is to say a control system for an industrial process comprising a man-machine interface. for supervision and a digital communication network.
- PLC programmable logic controller
- the PLC system can include several modular controllers which control the subsystems or control equipment of the installation. These devices are each configured to ensure at least one operation among: the acquisition of data from at least one measurement sensor, the control of at least one actuator connected to at least one flow controller unit, the regulation and the slaving of parameters, data transmission between the different equipment of the system.
- the control unit 5 can thus comprise at least one of: a microcontroller, a microprocessor, a computer.
- the control unit 5 can be connected to the various control equipment of the installation, in particular to the components flow regulators 41, 42, to the sensor 8, and communicate with said equipment by electrical links, Ethernet, Modbus, etc.
- Other modes of connection and / or transmission of information are possible for all or part of the equipment of installation, for example by radio frequency links, WIFI, Bluetooth ...
- the electronic logic 5 calculates a predetermined proportion of the flow rate D1 relative to a production flow rate DP and / or a predetermined proportion of the flow rate D2 relative to DP, i. e. predetermined D1 / DP and / or D2 / DP ratios, as a function of a target C1 content of the gas mixture in the first gas and / or a target C2 content of the gas mixture in the second gas.
- the electronic logic 5 does not calculate the flow rate of the second gas D2 from a target content C2 in the second gas but regulates D2 by deduction from D1. D2 then corresponds to DP from which D1 is subtracted. Preferably, the electronic logic 5 calculates a predetermined proportion of the flow rate D1 relative to DP from a target content C1 which is that of the minority gas in the mixture.
- the adjustment of D1 and D2 can be done from respective target contents C1, C2, the third flow rate D3 setpoint in the third gas being deduced from the values of D1 and D2.
- control unit 5 comprises a man-machine interface 300 comprising an input interface, for example a touch screen, allowing a user to input said at least one target content of the first gas and / or the second gas in the gas mixture.
- the contents can be expressed as a volume percentage of the first or second gas present in the gas mixture.
- man-machine interface 300 can allow the user to give instructions to the control unit 5.
- the flow rate regulators 41, 42 are instructed by the control unit 5 to regulate the flow of the first and second gas to the respective setpoints D1, D2 determined from the target composition for the gas mixture. It is with these flow rates that the first gas and the second gas enter the mixing device 3.
- the mixing device 3 comprises a common mixing volume into which the inlet (s) and the outlet 33 open and into which the mixture is homogenized. It is possible for example to use a mixer 3 of the static mixer type allowing continuous mixing of the fluids entering the mixer.
- This type of mixer generally comprises at least one disturbing element, such as a plate, a portion of pipe, an insert, capable of disturbing the flow of fluids, generating pressure drops and / or turbulence to promote the mixing of fluids and its homogenization.
- a mixture of the first and second gases is therefore produced at the outlet 33 of the mixing device 3 with a production flow rate DP.
- the flow rates D1 and D2 are conditioned by the flow rate DP and by the desired contents C1, C2 of first and second gas.
- a problem which arises relates to the distribution of a gas mixture to a consumer unit 10 whose demand for the gas mixture is fluctuating. As a result, the rate of delivery of the gas mixture to point 10 will vary.
- the present invention proposes to connect the outlet 33 of the mixer 3 to the inlet of a buffer tank 7 via a pipe 23.
- a distribution line 6 is fluidly connected to an outlet of the buffer tank 7 and makes it possible, in operation, to distribute the gas mixture to the consuming unit 10.
- the installation can include a vent line 25 fluidly connected to the buffer tank 7 with a vent 15 associated with a valve, useful in the event of overpressure, and to a valve controlling the passage of the mixture to a control unit. gas reprocessing.
- the valve makes it possible, during the start-up phases of distribution to the consumer unit, to purge the pipes of the installation and the buffer tank 7.
- the distribution of the gas mixture to the consumer unit 10 therefore takes place from the buffer tank 7 with a DC consumption flow rate corresponding to the mixed consumption of the consumer unit 10.
- the production flow rate DP upstream of the buffer tank 7 may no longer correspond to the demand for mixing.
- the buffer tank 7, thanks to the additional volume that it provides on the fluid circuit, makes it possible to ensure distribution at the DC flow rate even if it does not correspond to the DP flow rate.
- DP is greater than DC
- the reservoir 7 prevents the gas mixture from being forced towards the distribution line and thus absorbs the overproduction.
- DP is less than DC, the buffer tank 7 forms a mixture reserve from which the user can draw, for example when consumption starts too quickly with a high consumption rate, which makes it possible to ensure distribution at the DC rate even in a situation of under-production.
- the installation comprises a measurement sensor 8 which measures a physical quantity whose variation is representative of a variation in the DC consumption flow rate flowing in the distribution line 6 and provides a first measurement signal corresponding to the 'control unit 5.
- the first measurement signal can comprise several successive measurements carried out by the sensor 8.
- the unit 5 receives it and generates a first control signal which is transmitted to the flow regulating members 41, 42 of so as to adjust the first flow rate setpoint D1 and the second flow rate setpoint D2 in accordance with the first control signal.
- the present invention thus makes it possible to recalculate the flow setpoints D1, D2 initially configured in order to adapt them to a variation in the DC consumption flow rate and therefore at the request of the user.
- the mixing device 3 produces a mixing flow rate, the control of which is associated with the flow rate consumed.
- control unit 5 continues to control the D1 / DP and D2 / DP ratios so that they comply with the desired first gas and second gas contents for the gas mixture.
- the method according to the invention advantageously implements a so-called start-up phase at the start of consumption of the mixture by the consuming unit, while no consumption was detected before.
- start-up phase we go from a zero production rate DP to a production of a mixture of the first and second gases with a predetermined production rate DP.
- the user can start the production of the gas mixture with a predetermined flow rate DP which can be set at a minimum so-called starting value corresponding to a predetermined percentage of the maximum production flow rate that can be produced.
- This maximum production flow rate corresponds to the sum of a first maximum flow rate value and a second maximum flow rate value that the first and second regulating members 41, 42 are designed to distribute.
- the predetermined percentage is at least 25%, preferably at least 35% and more preferably at least 50% of the maximum production rate. This makes it possible to use the sensor which measures the flow in the flow regulators D1, D2 in its optimum and most precise operating range.
- the product gas mixture can be distributed to the vent 15, in particular in the case where the composition of the mixture does not comply with the target composition.
- the user can optionally initially set a higher production flow rate than the expected DC consumption flow rate in order to fill the buffer tank 7 and constitute a mixture reserve there.
- a production regulation phase follows during which the production flow rate DP is adjusted as a function of the consumption flow rate DC.
- the control unit 5 monitors the DC consumption rate via the measurements received from the measuring sensor 8. If a change in the DC consumption rate is detected, the control unit 5 generates a first control signal for adapting the flow rates D1, D2 distributed upstream of the mixer in order to bring the flow rate DP in line with the modified flow rate DC.
- the measurement sensor 8 performs continuous or quasi-continuous measurements.
- the control unit 5 is configured so that the generation of the first control signal and / or the transmission of the first control signal to the flow rate regulators only takes place at a predetermined time interval, in particular an interval of the order of 1 to 60 seconds. In other words, the flow setpoints are maintained during this time interval, without an adjustment of the setpoints being ordered by the control unit 5. This makes it possible to avoid a reaction of the installation following untimely fluctuations in the temperature. DC flow rate or to avoid generating too rapid variations of the DP flow rate which could give rise to operating errors.
- control unit 5 can be configured to, at least temporarily, maintain the production flow rate DP.
- the control unit 5 can draw from the buffer tank 7 to compensate for the underproduction of the mixer 3. If the consumption rate DC decreases, the buffer tank 7 can be filled to dampen the overproduction of the mixer 3.
- control unit 5 is configured so as to stop the gas flow when the physical quantity measured by the sensor 8 is representative of a zero DC consumption flow.
- the control unit 5 can also be configured to stop the gas flow if the physical quantity measured by the sensor 8 is representative of a DC consumption flow rate is low, i. e. lower than a given low flow threshold, in order to avoid an overpressure in the buffer tank 7.
- the control unit 5 can also be configured to generate an alarm signal when the physical quantity measured by the sensor 8 is representative of 'a DC consumption rate greater than a given high rate threshold.
- control loop is generally meant a control system of a process in which a controlling variable acts on a controlled variable, i. e. a quantity to be controlled, to bring it as quickly as possible to a setpoint value and to maintain it there.
- the basic principle of a servo-control is to measure, permanently, the difference between the real value of the quantity to be controlled and the set-point value that one wishes to reach, and to calculate the appropriate command to be applied to one or more. several actuators so as to reduce this gap as quickly as possible. This is also referred to as a closed-loop controlled system.
- the controlling variable is the physical quantity measured by the measuring sensor 8
- the controlled variable is the production flow rate DP, via the setting of the flow rates D1 and D2 of the first and second gas.
- the setpoint is variable according to the consumption conditions of the mixture.
- the first servo loop comprises a first comparator 11 A arranged within the control unit 5 and configured to generate at least a first error signal from the first measurement signal.
- the first error signal can be representative of a variation in the physical quantity measured. It is advantageously obtained by comparison with at least one measurement of said physical quantity taken at another time.
- the first loop comprises a first corrector 12A arranged within the control unit 5 and configured to generate the first control signal from the first error signal.
- the first corrector 12A sends the control signal to actuators which control a movement, in response to the first control signal, of the first and second flow rate regulating members 41, 42 in respective positions in which the first flow setpoint D1 and the second flow setpoint D2 are adjusted in accordance with the first control signal.
- the actuators control the movement of moving parts within the regulators, which vary the flow rates D1, D2 sent to the mixing device 3 in a direction tending to reduce the difference between the flow rates DP and DC.
- the first corrector 12A is of the proportional, integral and derivative (PID) type, which makes it possible to improve the performance of a servo-control thanks to three combined actions: a proportional action, an integral action, a derivative action.
- PID proportional, integral and derivative
- the corrective action of the first servo loop is only applied to the setpoints D1, D2 at a predetermined time interval, preferably an interval between 1 and 60 s, preferably still of the order of 20 s, in order to avoid excessively rapid variations in the production flow rate which can create errors.
- This time interval can be a parameter of the first corrector 12A.
- the first corrector 12A can include in particular a microprocessor, memory registers, programming instructions for processing the first error signal and for developing by numerical calculation the terms proportional, integral, and derivative of the control loop. These terms, which can be determined by calculation and / or experimentally, are combined to provide the control signal for the regulatory organs 41, 42.
- the term derived from D can optionally be zero.
- FIG. 1 illustrates an embodiment in which the measurement signal is obtained by a flow sensor 8, also called a flowmeter, arranged on the distribution line 6 so as to directly measure the distributed DC consumption flow. to the consumer unit 10.
- a flow sensor 8 also called a flowmeter
- FIG. 1 illustrates an embodiment in which the measurement signal is obtained by a flow sensor 8, also called a flowmeter, arranged on the distribution line 6 so as to directly measure the distributed DC consumption flow. to the consumer unit 10.
- the signals received and sent to the various elements of the installation are shown diagrammatically by the dashed lines referenced "A".
- the control signal orders an increase in the first and second flow rate setpoints D1, D2 and a decrease in the first and second flow rate set points D1, D2 if the DC flow rate decreases.
- each of the first and second flow regulating members 41, 42 can move between a closed position in which the first flow setpoint D1 or the second flow setpoint D2 is zero and a fully position. open in which the first flow rate instruction D1 or the second flow rate instruction D2 respectively have a first maximum flow rate value or a second maximum flow rate value.
- the first and second flow regulating members 41, 42 can optionally occupy at least one intermediate position between the closed position and the open position.
- said intermediate position corresponding to a first flow rate setpoint D1 or a second flow rate setpoint D2 greater than or equal to a first minimum flow rate value or a second minimum flow rate value.
- the first minimum flow rate value and / or the second minimum flow rate value is equal to at least 25%, more preferably at least 35%, or even at least 50%, of the respective first or second maximum value. This makes it possible to work on flow ranges where the precision of the regulating members 41, 42, more precisely the precision of the flow sensors used in the regulating members, is better.
- the installation uses a pressure sensor 8 measuring the pressure prevailing in the buffer tank 7 as a physical quantity representative of the DC consumption rate.
- the DC consumption flow fluctuations are thus determined indirectly, via the determination of pressure fluctuations in the buffer tank 7.
- the representation of FIG. 1 remains applicable except that the measurement signal is produced by the sensor 8 connected to the tank. buffer and not by sensor 8 connected to line 6.
- the installation according to the invention can include two sensors 8, one for flow and the other for pressure. These sensors are as described above and each produce a respective first measurement signal.
- the control unit 5 is configured to generate the first control signal from the measurement signal from one or the other of the sensors 8.
- the control unit 5 chooses to use the first measurement signal coming from that of the two measurement sensors 8 which measures a physical magnitude value representative of the highest flow rate.
- the pressure sensor 8 sends the first measurement signal to the first comparator 11 A which generates a first error signal corresponding to the pressure drop information and transmits it to the first corrector 12A so that it calculates a first control signal applied to the first and second flow rate regulating members 41, 42 so that the first and second flow rate setpoints D1, D2 increase by an appropriate factor, which can be determined by the first regulation loop.
- the first comparator 11A is configured to generate at least a first error signal from a comparison of the first measurement signal with at least one parameter chosen from: a low pressure threshold, a threshold of high pressure. These thresholds can be adjusted according to the operating conditions, the characteristics of the installation, etc.
- the first corrector commands the flow regulating members to regulate the flow. of the first and second gases according to the flow rates D1, D2 given.
- This operating mode can be implemented during the regulation phases as well as during the consumption start-up phases.
- a start-up phase as soon as the pressure in the buffer tank 7 reaches the low pressure threshold, the flow regulating members are commanded to regulate the flow of the first and second gases so as to produce the mixture of gas with the DP flow rate set at the start value.
- the flow rate setpoints D1, D2 can correspond respectively to the first minimum flow rate value and to the second minimum flow rate value.
- the flow rate regulators 41, 42 start to produce each of the minimum flow rates leading to a DP flow rate equal to the starting value until reaching the high pressure threshold in the buffer tank 7.
- the flow setpoints D1, D2 are increased by following a regulation scheme by the first corrector 12A, preferably of the PID type, in which the increase in flow rates is a function of the drop in pressure.
- the flow rate regulating members 41, 42 can be moved to their respective closed positions in which the flow rates D1, D2 are impaired.
- FIG. 2 shows schematically an example of the effect of a first servo loop with a first PID type corrector in which the production rate DP, corresponding to the sum of D1 and D2, is corrected as a function of the variation of the pressure P 7 in the buffer tank 7.
- the maximum production flow DP of the installation corresponding to the sum of the first and second maximum flow values, is set at 100 sL / min (standard liter per minute), ie 6 Nm 3 / h (normal cubic meter per hour).
- the installation's minimum DP production flow rate, corresponding to the sum of the first and second minimum flow rate values, is set at 25 sL / min (standard liter per minute), ie 1.5 Nm 3 / h.
- the high and low pressure thresholds are set at 4 bar and 3.8 bar respectively.
- FIG. 2 schematically represents various scenarios which may be encountered during the operation of the installation.
- DP DC
- the pressure in the buffer tank will drop to 3.8 bar (movement to the left along the gray arrow).
- This pressure is the starting pressure of the flow regulators.
- the DP flow rate is at its minimum start-up value, ie 25 sL / min
- the control unit has commanded the flow regulators to produce a DP flow ⁇ DC, the pressure will drop until a temperature is reached.
- DC flow rate equal to the maximum DP flow rate of the installation, ie 100 sL / min (movement from bottom to top along the gray arrows).
- DP> DC the buffer tank begins to fill and the pressure increases from 3.5 bar to 4 bar (following the arrows with black lines). 4 bar is the stop pressure for filling the buffer tank.
- FIG. 3 An example of what happens in practice is shown in Figure 3 showing the time evolution of the pressure in the buffer tank (dashed curve) and the production flow DP (solid line).
- zone A if there is no drop in pressure, the flow setpoint remains at 0.
- zone B flow setpoints are given to the flow regulators D1 and D2, which are incremented at a regular interval if the pressure does not stabilize.
- zone C filling the buffer tank (zone C) is stopped. If the pressure drops again (zone D), the setpoints of the flow regulators will be adjusted to the desired values in order to allow the DC consumption to be predicted and to keep the pressure of the buffer tank stable.
- the normo cubic meter is a unit of measurement of quantity of gas which corresponds to the content of a volume of one cubic meter, for a gas found in normal conditions of temperature and pressure (0 or 15 or more rarely 20 ° C according to the standards and 1 atm, i.e. 101 325 Pa).
- a normal cubic meter corresponds to approximately 44.6 moles of gas.
- the buffer tank advantageously has an internal volume equal to at least half of the maximum DP production flow rate DP of the installation.
- the buffer tank can have an internal volume of at least 1 L, or even at least 50 L, or even 1000 L or more. Preferably, the internal volume of the buffer tank will be between 50 and 400 L.
- the tank can be formed from a single tank or from several tanks fluidly connected to one another, the internal volume of the buffer tank then being understood as the sum of tank volumes.
- the installation may further include a first analysis unit 13 configured to analyze at least one content of the first gas and / or the second gas of the gas mixture distributed by the line of power supply 6.
- a first analysis unit 13 configured to analyze at least one content of the first gas and / or the second gas of the gas mixture distributed by the line of power supply 6. This makes it possible in particular, during the start-up phase of the installation, to condition the distribution of the gas mixture to the conformity of the measured contents with the target contents.
- a tolerance of the order of 0.1 to 5% (relative%) with respect to the target levels C1, C2 can be set. If the mixture produced does not conform, production may possibly be stopped.
- the first analysis unit 13 is configured to analyze the content of the first gas, which may in particular be the minority gas in the gas mixture.
- the installation according to the invention can comprise a second analysis unit 14 arranged upstream of the buffer tank 7 so as to measure at least one content of the first gas and / or the second gas of the gas mixture produced by the mixing device 3.
- the second analysis unit 14 is configured to supply consequently at least one second measurement signal to the control unit 5, which generates a second control signal from the second measurement signal.
- the second control signal is used to control one and / or the other of the flow rate regulating members 41, 42 so as to adjust one and / or the other of the proportions of the first flow rate set point D1 and of the second flow rate set point D2 relative to the production flow rate DP so that the effective composition of the gas mixture leaving the mixing device 3 approaches the target composition at levels C1, C2 (C2 being preferably deduced from C1 and not measured ).
- the signals received and sent to the various elements of the installation as part of the control of the composition of the mixture are shown diagrammatically by the dashed lines “B”.
- This control of the contents of the mixture produced by the mixing device makes it possible to compensate for any errors between the flow rates actually set by the flow regulating members 41, 42 and the flow setpoints D1, D2 which are applied to them.
- the arrangement of a sampling point located between the outlet of the mixing device and the inlet of the buffer tank 7 makes it possible to detect and react more quickly to any variations in content, thus avoiding the risk of consuming an incorrect mixture. in the buffer tank 7.
- the pipe taking the mixture and leading it into the analysis unit advantageously has the shortest possible length so that the analyzer provides a very precise response in real or quasi-real time.
- the pipe is such that the time lag between the moment when the mixture is taken at its sampling point and the moment when the analysis unit gives its measurement is minimal, typically less than 30 seconds, in particular between 1 and 30 seconds.
- the second control signal is produced from a second error signal containing at least one item of information on the difference between a measured content and a target content, for the first gas or the second gas.
- the first gas being the minor gas of the mixture. This difference can be expressed in particular as: where Mi is the content measured for the first gas.
- the relative difference ACi can be used as a correction factor for the first flow rate setpoint D1.
- the desired gas mixture is a mixture formed of the first gas with a target C1 content of 4% and of the second gas for the remainder, therefore with a C2 content of 96% (% by volume).
- a first flow setpoint D1 of 4 sL / min (0.24 Nm 3 / h), corresponding to a proportion of 4% with respect to DP, and a second setpoint D2 of 96 sL / min (5.76 Nm 3 / h), corresponding to a proportion of 96% with respect to DP, are therefore applied to the respective flow rate regulators 41, 42.
- the members 41, 42 have an accuracy of adjustment of plus or minus 1%.
- a first gas content of 3.92% is measured at the outlet of the mixing device 3, corresponding to a deviation ACi of -2% (relative%) with respect to the target content C1.
- the control unit 5 generates a second control signal commanding the flow rate regulating members 41, 42 to adjust the flow rates D1 and D2 with respect to DP so as to compensate for this difference.
- the first setpoint D1 is therefore adjusted to D1 + 2%, ie 4.08 sL / min.
- the control unit 5 controlling the maintenance of D2.
- D2 also is adjusted in response to the second control signal.
- D2 would be adjusted to 95.04 sL / min.
- the correction can also be made by applying a correction factor to at least one of the target contents previously recorded in the control unit 5, in the above example a correction by a factor equal to 0.03, which has the effect of adjusting D1 to 4.08 accordingly sL / min.
- the installation can include an alarm configured to emit an alarm signal if the first analysis unit and / or the second analysis unit detects levels outside the planned tolerance ranges.
- the first analysis unit 13 and / or the second analysis unit 14 can be chosen in particular from the following types of detectors: a thermal conductivity detector, a paramagnetic alternating pressure detector, a catalytic adsorption detector, a detector with non-dispersive infrared absorption, an infrared spectrometer.
- the type of analysis unit can be adapted according to the nature of the gases to be analyzed.
- the first 13 and second 14 analysis units can be interchanged.
- the first 13 and second 14 analysis units are connected to the vent 15 so as to discharge therein the gas mixture analyzed.
- the installation may include a second control loop of the respective proportions of the first flow rate setpoint D1 and / or of the second flow rate setpoint D2 relative to the production flow rate DP on the second measurement signal. supplied by the second analysis unit 14.
- the controlling quantities are the content (s) measured by the second analysis unit 14, the controlled quantities are one and / or the other of the proportions D1 / DP, D2 / DP.
- the setpoint is variable depending on the actual content (s) measured.
- the second loop comprises a second comparator 11 B arranged within the control unit 5 and configured to generate at least a second error signal from a comparison of the second measurement signal with at least one parameter chosen from: the target content C1 in the first gas, the target content C2 in the second gas.
- a second corrector 12B is arranged within the control unit 5, in particular of the PID type, and configured to generate the second control signal from the second error signal.
- the actuators of the first and second flow regulators 41, 42 control the movement of the first and second flow regulators. flow rate 41, 42 in respective positions in which the proportions of D1 and / or D2 with respect to DP conform to the second control signal.
- the regulation loop ordering D2 Preferably, only the proportion of D1 is adjusted, the regulation loop ordering D2 to remain fixed.
- first comparator and the second comparator can possibly form the same entity configured to receive as input data both the measurements of the sensor 8 and of the second analysis unit 14 and to produce the appropriate error signals as output. . It is the same for the first and second correctors.
- the installation according to the invention can be used for the distribution of gas mixtures used in different industries such as semiconductor, photovoltaic, LED, flat screen industries or any other industry such as mining, pharmaceutical, space industries. or aeronautics.
- the installation comprises at least one gas cabinet (in English "gas cabinet") in which are installed at least the control unit 5, the mixing device 3, the flow regulating members, the measurement sensor 8. , the buffer tank 7.
- the sources of the first and second gas can be located inside or outside the cabinet.
- the sources are located outside the cabinet so that the latter retains a reasonable footprint.
- the control unit 5 is arranged outside the cabinet, either by being fixed to one of the walls of the cabinet, or positioned at a distance from the cabinet.
- the gas cabinet may include a housing with a back wall, sidewalls, a front wall, a bottom, and a ceiling.
- one or more buffer reservoirs are provided which stand up on the bottom and can be fixed in the housing in a manner known in the state of the art.
- a system of gas pipes is arranged in said housing, preferably against the bottom of the cabinet.
- the cabinet may include means for monitoring and / or maintaining the gas pipe system such as valves, pressure reducing valves, pressure measuring devices, etc. allowing operations such as gas distribution to be carried out, the opening or closing of certain pipes or portions of pipes, gas pressure management, carrying out purge cycles, leak tests, etc.
- the housing includes gas inlet openings for supply with the first and second gases and a gas outlet opening for dispensing the gas mixture.
- the distribution line 6 is connected to the outlet opening. In operation, the gas cabinet is connected to the consumption unit by the distribution line 6.
- Other gas inlets can be provided, in particular for a purging gas or a standard gas for calibrating the analyze
- the installation according to the invention can in particular be used to produce gas mixtures having the following compositions:
- H2 - hydrogen (H2) in an inert gas such as nitrogen (N2), argon or helium,
- CO2 carbon dioxide
- inert gas such as nitrogen, argon or helium
- CHU - methane
- the target C1 contents of the first gas in particular the target contents of H2, helium, CO2, CH4, O2, are between 0.0001 and 50%, preferably between 0.1 and 20%, the remainder being the second gas.
- a mixture comprising hydrogen as the first gas in nitrogen as the second gas has been produced and distributed on site.
- the target hydrogen content C1 was 4% (% by volume).
- the installation included a first PID-type servo loop as described above and possibly, depending on the accuracy requirements required by the consuming unit, a second servo loop.
- Figure 4 shows a recording of the DC gas mixture flow rate distributed by the distribution line of an installation comprising a second servo loop with the hydrogen content measured during this recording.
- Figure 5 is an enlarged view of the content recording of Figure 4.
- a variable DC gas mixture flow rate between typically 0 and 150 sL / min could be produced with a stability of the content characterized by a relative standard deviation of the order of 3% without a second servo loop and of the order of 1% with a second servo loop.
- the present description describes a gas mixture with two constituents but that it can be transposed to any mixture having a greater number of constituents.
- three sources each distribute a first gas, a second gas, a third gas.
- Flow regulating members 41, 42, 43 are instructed by the control unit 5 to regulate the flow of the first, second and third gases at respective flow setpoints D1, D2, D3.
- the mixer device is configured to distribute a mixture of flow rate DP equal to the sum of D1, D2, D3.
- the proportions of first, second gas and third gas relative to DP are determined as a function of at least two among three target contents C1, C2, C3 of the gas mixture in the first gas, the second gas and the third gas respectively. All or part of the characteristics already described for a two-gas mixture can be transposed to this three or more gas mixture.
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Abstract
Description
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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EP21729523.7A EP4162521A1 (fr) | 2020-06-05 | 2021-05-31 | Installation et procédé de distribution d'un mélange de gaz |
JP2022574653A JP2023528067A (ja) | 2020-06-05 | 2021-05-31 | ガス混合物を送達するためのプラント及び方法 |
CN202180039659.6A CN115917721A (zh) | 2020-06-05 | 2021-05-31 | 用于分配气体混合物的设备和方法 |
KR1020227045309A KR20230021674A (ko) | 2020-06-05 | 2021-05-31 | 가스 혼합물을 분배하기 위한 시설 및 방법 |
US18/008,365 US20230277993A1 (en) | 2020-06-05 | 2021-05-31 | Installation and method for distributing a gas mixture |
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FRFR2005922 | 2020-06-05 | ||
FR2005922A FR3111085B1 (fr) | 2020-06-05 | 2020-06-05 | Installation et procédé de distribution d’un mélange de gaz |
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EP (1) | EP4162521A1 (fr) |
JP (1) | JP2023528067A (fr) |
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CN (1) | CN115917721A (fr) |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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FR2631856A1 (fr) * | 1988-05-31 | 1989-12-01 | Rhone Poulenc Chimie | Procede de melange et de compression de gaz, a debit controle, stable en debit et en composition, a partir d'au moins deux sources sous pression |
EP0623381A1 (fr) * | 1993-05-07 | 1994-11-09 | Teisan Kabushiki Kaisha | Système d'alimentation de gas mélangés |
KR20090118428A (ko) * | 2008-05-13 | 2009-11-18 | 주식회사 동부하이텍 | 반도체 제조 공정용 희석가스 공급장치 및 그 방법 |
WO2010031940A1 (fr) | 2008-09-16 | 2010-03-25 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Installation miniaturisee de fabrication de melanges de gaz |
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- 2021-05-31 US US18/008,365 patent/US20230277993A1/en active Pending
- 2021-05-31 WO PCT/EP2021/064478 patent/WO2021245000A1/fr active Application Filing
- 2021-06-02 TW TW110120009A patent/TW202206740A/zh unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2631856A1 (fr) * | 1988-05-31 | 1989-12-01 | Rhone Poulenc Chimie | Procede de melange et de compression de gaz, a debit controle, stable en debit et en composition, a partir d'au moins deux sources sous pression |
EP0623381A1 (fr) * | 1993-05-07 | 1994-11-09 | Teisan Kabushiki Kaisha | Système d'alimentation de gas mélangés |
KR20090118428A (ko) * | 2008-05-13 | 2009-11-18 | 주식회사 동부하이텍 | 반도체 제조 공정용 희석가스 공급장치 및 그 방법 |
WO2010031940A1 (fr) | 2008-09-16 | 2010-03-25 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Installation miniaturisee de fabrication de melanges de gaz |
Also Published As
Publication number | Publication date |
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KR20230021674A (ko) | 2023-02-14 |
TW202206740A (zh) | 2022-02-16 |
CN115917721A (zh) | 2023-04-04 |
JP2023528067A (ja) | 2023-07-03 |
FR3111085A1 (fr) | 2021-12-10 |
FR3111085B1 (fr) | 2023-05-12 |
US20230277993A1 (en) | 2023-09-07 |
EP4162521A1 (fr) | 2023-04-12 |
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