WO2019091804A1 - Method and device for producing a vapour by the use of control data obtained in a control mode - Google Patents

Abstract

The invention relates to a method for producing a vapour by evaporating the solid or liquid particles of an aerosol, which are brought in at least one vapour generation step by means of a carrier gas flow to a heated evaporation body (6.1), where they are evaporated by supplying evaporation heat. A measured temperature value is determined in a control mode, which temperature is regulated to a setpoint value by means of an open-loop/closed-loop control unit (9) by varying the heating capacity fed into the evaporation body (6.1). The development of the heating capacity over time is stored in a log file. Control data is obtained with the aid of the log data stored in the log file to control the temperature of the evaporation body in a later process step, without closed-loop control, to evaporate the particles of the aerosol.

Description

 description

Method and apparatus for generating a vapor by the

Use of control data obtained in a control mode

Field of engineering

The invention relates to a method for generating a vapor by vaporizing the solid or liquid particles of an aerosol with one or more radiators, wherein one of the radiator is an evaporation body to which the particles are brought in at least one steam generating step by means of a carrier gas stream where they are vaporized by supplying heat of vaporization, wherein in a control mode, a first characteristic parameter of the one or more radiator is determined, which is controlled by a control / regulating device by varying heating energy fed into the radiator, in particular the first evaporator body to a desired value and the time course of at least one associated with the generation of heating power

Control parameter is stored in a log file. The invention also relates to a device for carrying out the method.

State of the art

Devices for generating a vapor from an aerosol are known for example from DE 10 2014 101 792 AI, WO 2012/175126 AI or DE 10 2014 109 196 AI. Devices of this type or methods for producing a vapor are used in the deposition of organic layers on a substrate, in particular in the production of OLEDs. In an rosolerzeuger is fed by means of a metering a constant, with respect to its mass flow but variable particle flow in a carrier gas stream fed. The carrier gas is an inert gas, for example nitrogen, which transports the particles in the form of an aerosol to a steam generator. The steam generator has at least one evaporation body, with which the evaporative heat is supplied to the aerosol particles in order to evaporate the aerosol particles. The vapor is transported through a vapor line to a reactor housing where it is fed to a gas inlet member which distributes the vapor into a process chamber in which the substrate to be coated is placed on top of a cooled substrate holder.

Summary of the invention

The invention has for its object to increase the reliability of a steam generator or specify an alternative operating mode for operating the evaporator. The problem is solved by the invention specified in the claims. The subclaims represent not only advantageous developments of the invention specified in the independent claims. They also form each with individual features of independent developments of the prior art, wherein individual features of various sub-claims can be combined with each other.

The aforementioned method is developed by a control mode in which the protocol data or control data obtained from the protocol data are used to feed without the determination of the characteristic parameter, the heating power in a radiator, in particular in the first evaporation body. Is it the radiator to an evaporation body, the particles of the aerosol are evaporated with the heating power. While in the control mode, a first characteristic parameter, for example, a temperature of the radiator, in particular evaporation body, is determined and this is controlled by the control / regulating device by varying heating power fed into the radiator, in particular evaporation body to a desired value, the feed takes place Heating power in the radiator, in particular evaporator body in the control mode without control, but using the data obtained in the control mode data. A device according to the invention can thus continue to be operated, for example in the event of failure of a sensor with which the characteristic parameter is determined, without immediate replacement of the sensor being undertaken. To a certain extent, the device operates in a "blmd mode" without determination of the characteristic parameter, for example without a temperature measurement, so that production interruptions can be avoided. <br/><br/> The device according to the invention can also include, in addition to a first evaporation body, further evaporation bodies, for example a second, third and / or second evaporation body It can be provided that each additional evaporation body is regulated in a control mode to a nominal temperature assigned to it individually For this purpose it can be provided that for each of the further evaporation bodies an individually assigned sensor, in particular a temperature sensor, is provided The actual temperature of the further evaporating body is determined, for example, by means of the control / regulating device, this value, in particular the temperature actual value, being regulated against a desired value this further evaporation body both in a control mode in which a characteristic parameter, for example the actual temperature, is controlled by varying the heat output fed into the further evaporation body against a desired value, for example a desired temperature. In a control mode, for example after failure of a temperature sensor, the respective further becomes Vaporizing body operated unregulated, the data obtained in the control mode log data are used to feed heating power in the evaporator body. It is thus provided in particular that in certain process steps, in particular steam generating steps, in which a steam is generated by the device, all evaporation bodies are operated in control mode or at least one evaporation body is operated in a control mode. It can also be provided that all evaporation bodies are operated in the control mode, wherein the heat output is controlled using the protocol data or control data obtained from the protocol data. The desired values of the one or more characteristic parameters are preferably contained in a recipe. The recipe can be a data record which contains the essential characteristic parameters for one or more successive process steps. The process steps can be heating steps, cooling steps, temperature steps and one or more steam generation steps. The formulation preferably stores the desired time profiles of one or more characteristic parameters, wherein the characteristic parameters may be the desired partial vapor pressure of the vapor which is measured in the steam line with a vapor pressure sensor arrangement as known from the aforementioned prior art , However, the characteristic parameter can also be a desired temperature of the at least one evaporation body. It is further provided that in the recipe also values for the time course of a total pressure, the mass flow of the carrier gas and / or the delivery rate of the aerosol generator are stored. If the characteristic parameter is the temperature of an evaporation body, then the device has a temperature sensor with which the temperature of the evaporation body can be measured. For this purpose, a plurality of thermocouples or other temperature sensors may be provided, wherein it is provided in particular that the temperature of each one or more evaporation body is determined individually. In a preferred variant of the invention provided that in a steam generating step, at least one or more evaporation body is operated in the control mode, but the last evaporation body in the flow direction is regulated to a desired temperature. The one or more evaporation bodies of the evaporator are preferably arranged one behind the other in the flow direction of the carrier gas so that the aerosol enters and flows through a first evaporation body in the flow direction, at least parts of the aerosol particles in the first evaporation body being vaporized. However, it is also possible for this evaporation body to be tempered at a temperature which is controlled below a vaporization temperature of the aerosol particles so that the aerosol particles are not vaporized in the first evaporation body in the direction of flow, but accumulate there. A night temperature control can be carried out in the direction of flow downstream of the first evaporation body further evaporation body, wherein the temperature of the last evaporation body in the flow direction for process stability is relevant. The control data used to control the at least one evaporation body in the control mode is preferably obtained by data optimization of the log data stored in the log file. It can be an averaging. Not only the respective characteristic parameters can be used to form the control data. Other measured values stored in the protocol file can also be used, for example the control data can be formed using in particular the use of initial temperatures, final temperatures, values for the steepness of a temperature ramp, the carrier gas pressure, the carrier gas flow and / or the particle feed rate , where the particles may be solid or liquid particles. The radiator either controlled or controlled according to the invention can not be just an evaporator body. The radiator may also be a preheater, with which a carrier gas is preheated. The inventive device is characterized in that the control / control device has a protocol data memory and in particular also a control data memory and is programmed so that in a control mode log data are obtained, which are used in a control mode for control.

Brief description of the drawings

An embodiment of the invention will be explained below with reference to the accompanying drawings. Show it:

1 shows schematically a device according to the invention for coating a substrate 14 with a layer of an organic material,

Fig. 2a shows the time course of the temperature Tl, T2, T3, T4, with

 Temperatursens oren 7.1, 7.2, 7.3, 7.4 are measured in various process steps PI, P2, P3, P4, P5,

2b shows the heating powers II, 12, 13, 14, in the process steps PI,

 P2, P3, P4, P5 are fed in the control mode in the evaporator body 6.1, 6.2, 6.3, 6.4 and

Fig. 3 shows schematically in a representation according to Figure 1 another

 Embodiment.

Description of the embodiments

Figures 1 and 3 show roughly schematically a device for the production of OLEDs. In a reactor housing 12, which is closed to the outside gas-tight and which is evacuated, there is a The substrate holder 15 carries the substrate 14 to be coated. The side of the substrate 14 to be coated faces a gas outlet surface of a gas inlet member 13, into which a steam line 11 opens, which can be heated and by means of a carrier gas a vapor is promoted, which condenses on the surface of the substrate 14, wherein for structuring the deposited on the substrate 14 layer, a mask, not shown, for example, shadow mask, is provided.

With a vapor pressure sensor arrangement 10, for example a QCM sensor, the partial pressure of the steam within the vapor line 11 can be determined.

Upstream of the steam line 11 is an evaporator 5, which in the embodiment has four or three successively arranged in the flow direction evaporation body 6.1, 6.2, 6.3, 6.4. The evaporation body 6.1, 6.2, 6.3, 6.4 are spaced from each other by a free space. But you can also touch touching each other. The evaporation body 6.1, 6.2, 6.3, 6.4 have evaporation surfaces. Through the evaporation body 6.1, 6.2, 6.3, 6.4, a gas can flow through. The evaporation body 6.1, 6.2, 6.3, 6.4 may for example be formed from an electrically conductive solid state foam, so that the solid state foam can be heated by passing an electric current. The heating power feeders denoted by 8.1, 8.2, 8.3 and 8.4 in FIG. 1 can thus be electrical lines with which an electrical current for transmitting the heating power is fed into the evaporating body 6.1, 6.2, 6.3, 6.4.

In each of the evaporation body 6.1, 6.2, 6.3, 6.4 is a respective evaporation body 6.1, 6.2, 6.3, 6.4 each individually assigned Temperature sensor 7.1, 7.2, 7.3, 7.4 arranged. The temperature sensors 7.1, 7.2, 7.3, 7.4 may be a thermocouple. However, it is also provided for measuring the temperature of the evaporation body 6.1, 6.2, 6.3, 6.4 optical temperature sensors to use oren. Upstream of the evaporator 5 is an opening into the evaporator 5 Aerosol 4, through which an aerosol is fed into the evaporator 5. By the evaporation body 6.1, 6.2, 6.3, 6.4 transfer heat of vaporization to the particles of the aerosol, the aerosol particles are evaporated. The aerosol is generated with an aerosol generator 3, which is arranged upstream of the aerosol line 4. The particle flow rate generated by the aerosol generator 3 can be adjusted. For this purpose, the aerosol generator 3 may have a metering element. In the drawings, a screw is shown for this purpose, which can be operated at varying speeds. The metering element can also be a perforated disk operated at a varying speed.

[0016] A carrier gas line 2 through which a carrier gas G is fed, with which the aerosol particles or the aerosol particle stream, which depends on the delivery rate, is transported through the aerosol line 4 to the evaporator 5, flows into the aerosol generator 3. The volume flow or the mass flow of the carrier gas G can be regulated. In the embodiment, a mass flow controller 1 is provided for this purpose.

For carrying out the method according to the invention, a control / regulating device 9 has a protocol data memory 16 and, if appropriate, also a control data memory 17. / Control device 9 a controller or microcomputer 18 for electronic data processing. The fiction, contemporary device can be operated in one or more temporally successive process steps PI, P2, P3, P4, P5. A recipe is stored in a recipe data memory 19, which contains in particular the temperatures T 1, T 2, T 3, T 4 of the evaporation bodies 6.1, 6.2, 6.3, 6.4 in the various process steps PI, P 2, P 3, P 4, P 5. In addition or as an alternative thereto, however, the steam partial pressure or vapor mass flow to be generated can also be stored in the recipe data memory 19 for each process step PI to P5. The reference numeral 6 denotes a preheater in Figures 1 and 3, which is also regulated to a desired temperature. The temperature is determined by a temperature sensor 7. It can be a thermocouple. An inert gas, for example nitrogen or a noble gas, is fed into a space upstream of the preheating body 6 by means of an inert gas feed line (not shown). The inert gas, which also forms a carrier gas, is heated in the preheater 6 to an elevated temperature.

FIG. 2a shows, by way of example, the temperature setpoint values T1 to T4, as they are to be set in each of the process steps PI to P5 to be carried out one after the other. It can be seen that when changing from one process step PI to P4 to the respective subsequent process step P2 to P5, a temperature ramp is passed through when the temperature Tl to T4 changes.

The device according to the invention is initially operated in a regular mode. In this control mode, a characteristic parameter whose setpoint is specified in the recipe is controlled to the setpoint. at the characteristic parameter may be the vapor pressure determined by the vapor pressure sensor arrangement 10. In the embodiment, however, as a characteristic parameter, for the sake of simplicity, the respective temperature Tl to T4 of the individual evaporation bodies 6.1 to 6.4 are discussed.

In a control mode, the device is initially operated such that successively the individual process steps PI to P5 are performed in which the temperatures Tl to T4 respectively by feeding heat output II, 12, 13, 14 by the heating power feeds 8.1, 8.2 , 8.3, 8.4 are regulated in the evaporation body 6.1, 6.2, 6.3, 6.4 to a desired value. The heating power II, 12, 13, 14 is varied according to an individual control characteristic (for example PID). At least the time sequences of the heating powers II to 14 are stored in the log data memory. However, the respective progressions of the actual temperatures of the evaporation bodies 6.1 to 6.4 and further measured values, such as the partial pressure of the steam, the total pressure, the aerosol delivery rate or the mass flow of the carrier gas G, can additionally be stored.

Once in one or more passes in which the evaporation bodies 6.1, 6.2, 6.3, 6.4 are operated in control mode and protocol data in the log data memory 16 have been collected, at least one evaporation body 6.1, 6.2, 6.3, 6.4 can be used in a later run be operated in a control mode. No control is performed in this control mode. The actual temperature of the evaporation body 6.1, 6.2, 6.3, 6.4 is not determined. The Heizleistungseinspeisung 8.1 to 8.4 takes place here exclusively borrowed by using the stored in the log data memory 16 log data. With this type of operation of one or more of the evaporation bodies 6.1, 6.2, 6.3, 6.4 can not only on a failure of a temperature sensors 7.1, 7.2, 7.3, 7.4. It is also possible to use the device according to plan in a new operating mode, in which the temperature of at least one of the evaporation bodies 6.1, 6.2, 6.3, 6.4 is not regulated, but controlled. The control of the one or more evaporation body 6.1, 6.2, 6.3, 6.4 fed heating power II to 14 can be done with the help of obtained from the log data control data. These can be stored in the control data memory 17. The control data are preferably calculated by averaging the log data obtained in the control mode. FIG. 2b shows, for example, control data for controlling the heating powers II to 14. In a process step PI, the device is in an idle state. There is no heat input. The current flowing through the electrically conductive evaporation bodies 6.1, 6.2, 6.3, 6.4 is 0 A. In a process step P2, only the last two evaporation bodies 6.3 and 6.4 in the flow direction are introduced by feeding a

Electricity heated. Due to heat conduction or heat radiation, however, the upstream evaporation bodies 6.1 and 6.2 also heat up. In the transition from process step P2 to process step P3, the heating power 13, 14 is first lowered and then increased in the form of a ramp. In process step P4, the upstream evaporation bodies 6.1, 6.2 are heated in two successive time periods with different heat outputs, which are kept constant over their feed time.

In a preferred variant of the invention it is provided that the device is operated in one or more passes in the control mode, wherein in each case all process steps PI to P5 are performed in succession. In the subsequent runs, the device is used in the control operated mode, wherein either all or some evaporation body 6.1, 6.2, 6.3, 6.4 are operated in the control mode or exclusively in the flow direction last evaporator body 6.4 is operated in control mode.

Also, the preheater 6 can be operated both in the control mode and in the control mode.

The above explanations serve to explain the inventions as a whole, which further develop the state of the art, at least by the following feature combinations, wherein two, several or all of these feature combinations can also be combined, namely:

A method which is characterized in that in a control mode, the log data stored in the log data or control data obtained from the log data are used to feed without determining the characteristic parameter, the heating power in the radiator, in particular the first evaporator body 6.1.

A method which is characterized in that the time course of the critical parameter is stored in the log file.

A method which is characterized in that in the control mode a second, third and / or fourth characteristic parameter of a second, third and / or fourth heating element, in particular evaporation body 6.2, 6.3, 6.4 is determined, which is associated with the control Control device 9 is controlled by varying in the second, third and / or fourth radiator, in particular evaporation body 6.2, 6.3, 6.4 fed heating power to a desired value and the time course at least one with the generation of stored in the second, third and / or fourth radiator, in particular Evaporator 6.2, 6.3, 6.4 heating power associated second, third and / or fourth control parameters is stored in the log file, and in the control mode, the log data and / or control data obtained from the log data be used to determine without determining the second, third and / or fourth characteristic parameters, the heating power in the second, third and / or fourth radiator, in particular evaporation body

6.2, 6.3, 6.4 to vaporize the particles of the aerosol.

A method, which is characterized in that the setpoint values of the one or more characteristic parameters are included in a recipe, in particular also the setpoint values of one or more characteristic parameters of further process steps, such as one or more heating steps, one or more cooling steps or contains one or more tempering or one or more further steam generating steps. A method characterized in that the one or more characteristic parameters are one of a temperature sensor 7.1, 7.2,

7.3, 7.4 determined actual temperature of the first, second, third and / or fourth radiator, in particular evaporation body is 6.1 to 6.4.

A method characterized in that the characteristic parameter is a vapor pressure of the vapor determined by a vapor pressure sensor arrangement 10.

A method which is characterized in that in a process step in which at least the first heating body, in particular evaporation body 6.1 is operated in the control mode, at least one of the second, third and / or fourth radiator, in particular evaporation body 6.2, 6.3, 6.4 is operated in control mode.

A method which is characterized in that at least the temperature of a last in the flow direction of the carrier gas radiator, in particular evaporation body 6.4 is controlled to a desired value.

A method which is characterized in that the control data are obtained by a data optimization, in particular an averaging, from the protocol data.

A method which is characterized in that the data stored in the protocol file additionally include the time profile of a carrier gas pressure, a carrier gas flow of a particle feed rate and / or initial temperatures and / or final temperatures of a process step.

A device which is characterized in that the control / regulating device 9 is programmed such that in a control mode, a first characteristic parameter of the radiator is determined, which with a control device 9 by varying in the first radiator , in particular evaporating body 6.1 fed-in heating power is controlled to a desired value and the time profile of at least one associated with the generation of heating power control parameter is stored in a protocol file, wherein in a control mode, the log data stored in the log data or control data obtained from the log data are used in order, without determining the characteristic parameter, to feed the heating power into the heating body, in particular the first evaporating body 6.1. A device which is characterized in that the control / regulating device 9 has a control data memory 17, are stored in the control data obtained from the protocol data.

All disclosed features are essential to the invention (individually, but also in combination with one another). The disclosure of the associated / attached priority documents (copy of the prior application) is hereby also incorporated in full in the disclosure of the application, also for the purpose of including features of these documents in claims of the present application. The subclaims characterize, even without the features of a claimed claim, with their features independent inventive developments of the prior art, in particular in order to make divisional applications based on these claims. The invention specified in each claim may additionally have one or more of the features described in the preceding description, in particular with reference numerals and / or given in the reference numerals. The invention also relates to design forms in which individual features mentioned in the above description are not realized, in particular insofar as they are recognizably dispensable for the respective intended use or can be replaced by other technically equivalent means.

List of reference numbers

1 mass flow controller 14 substrate

 2 carrier gas line 15 substrate holder

 3 Aerosol generator 16 Log data memory

4 Aerosol line 17 Control data memory

5 evaporator 18 microcomputer

6 Preheater 19 Recipe data memory

6.1 Evaporative body

 6.2 Evaporative body

 6.3. Evaporator body G carrier gas

 6.4 Vaporization body 11 heating power

 7 temperature sensor 12 heating power

 7.1 Temperature sensor 13 Heating power

 7.2 Temperature sensor 14 Heating power

 7.3 Temperature sensor PI Process step

 7.4 Temperature sensor P2 Process step

 8 Heating power supply P3 Process step

 8.1 Heating power feed P4 Process step

 8.2 Heating power supply P5 Process step

 8.3 Heating power input Tl temperature

 8.4 Heating power supply T2 Temperature

 9 Control device T3 temperature

 10 steam pressure T4 temperature

 sensor arrangement

 11 steam line

 12 reactor housing

 13 gas inlet member

Claims

 claims A method of generating a vapor by vaporizing the solid or liquid particles of an aerosol with one or more radiators, one of the radiators being an evaporating body (6.1) to which the particles are brought in at least one steam generating step by means of a carrier gas flow They are vaporized by supplying heat of vaporization, wherein in a control mode, a first characteristic parameter of the one or more radiator is determined, which with a control / regulating device (9) by varying in the radiator, in particular the first evaporating body (6.1) supplied heating power is controlled to a desired value and the temporal History of at least one associated with the generation of heating power control parameter is stored in a log file, being used in a control mode, the log data stored in the log data or control data obtained from the log data to determine without determining the characteristic parameter, the heating power in the radiator, in particular the first Feeding the evaporation body (6.1). 2. The method according to claim 1, characterized in that the time profile of the critical parameter is stored in the log file. 3. The method according to any one of the preceding claims, characterized in that in the control mode, a second, third and / or fourth characteristic parameters of a second, third and / or fourth radiator, in particular evaporation body (6.2, 6.3, 6.4) is determined, with the Control device (9) by varying in the second, third and / or fourth radiator, in particular evaporation body (6.2, 6.3, 6.4) fed heating power to a desired value is stored and the time course of at least one with the generation of the second, third and / or fourth radiator, in particular evaporation body (6.2, 6.3, 6.4) heat input associated second, third and / or fourth control parameters in the log file, and in Control mode, the log data and / or derived from the log data control data used to feed without determining the second, third and / or fourth characteristic parameters, the heating power in the second, third and / or fourth radiator, in particular evaporation body (6.2, 6.3, 6.4) to vaporize the particles of the aerosol. Method according to one of the preceding claims, characterized in that the setpoint values of the one or more characteristic parameters are contained in a formulation, in particular the setpoint values of one or more characteristic parameters of further process steps, such as one or more heating steps, one or more cooling steps or or more tempering steps or one or more further steam generating steps. Method according to one of the preceding claims, characterized in that the one or more characteristic parameters determined by a temperature sensor (7.1, 7.2, 7.3, 7.4) actual temperature of the first, second, third and / or fourth radiator, in particular evaporation body (6.1 to 6.4). 6. The method according to any one of the preceding claims, characterized in that the characteristic parameter is one of a vapor pressure sensor arrangement (10) determined vapor pressure of the vapor. Method according to one of the preceding claims, characterized in that in a process step in which at least the first radiator, in particular evaporation body (6.1) is operated in the control mode, at least one of the second, third and / or fourth radiator, in particular evaporation body (6.2, 6.3 , 6.4) is operated in control mode. A method according to claim 7, characterized in that at least the temperature of a last in the flow direction of the carrier gas radiator, in particular evaporation body (6.4) is regulated to a desired value. 9. The method according to any one of the preceding claims, characterized in that the control data by a data optimization, in particular an averaging, are obtained from the protocol data. Method according to one of the preceding claims, characterized in that the data stored in the log file additionally include the time profile of a carrier gas pressure, a carrier gas flow of Partikelzuführrate and / or start temperatures and / or final temperatures of a process step. Device for carrying out the method according to one of the preceding claims, having a carrier gas line (2) opening into an aerosol generator (3) for feeding a volume- and / or mass-controlled carrier gas, one connected to an aerosol line (4) with the aerosol generator (3), at least one heating element, in particular evaporation body (6.1, 6.2, 6.3, 6.4), having an evaporator (5) and a control / regulating device (9) which stores a log data storage Rather, (16), characterized in that the control device (9) is programmed such that in a control mode, a first characteristic parameter of the radiator is determined, which is connected to a control device (9) by varying in the first heating body, in particular evaporation body (6.1) fed heating power is controlled to a desired value and the time course of at least one associated with the generation of the heating power control parameter is stored in a log file, wherein in a control mode, the log data stored in the log data or control data obtained from the log data used to without Determining the characteristic parameter, the heating power in the radiator, in particular the first evaporator body (6.1) feed. Apparatus according to claim 11, characterized in that the control / regulating device (9) has a control data memory (17) are stored in the control data obtained from the protocol data. Apparatus or method characterized by one or more of the characterizing features of any one of the preceding claims.