WO2021078644A1 - Procédé pour faire fonctionner un capteur à microbalance à cristal de quartz - Google Patents

Procédé pour faire fonctionner un capteur à microbalance à cristal de quartz Download PDF

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Publication number
WO2021078644A1
WO2021078644A1 PCT/EP2020/079185 EP2020079185W WO2021078644A1 WO 2021078644 A1 WO2021078644 A1 WO 2021078644A1 EP 2020079185 W EP2020079185 W EP 2020079185W WO 2021078644 A1 WO2021078644 A1 WO 2021078644A1
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WO
WIPO (PCT)
Prior art keywords
phase
temperature
power
cleaning
sensor
Prior art date
Application number
PCT/EP2020/079185
Other languages
German (de)
English (en)
Inventor
Nael Al Ahmad
Claudia Cremer
Original Assignee
Apeva Se
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Apeva Se filed Critical Apeva Se
Publication of WO2021078644A1 publication Critical patent/WO2021078644A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/22—Details, e.g. general constructional or apparatus details
    • G01N29/32—Arrangements for suppressing undesired influences, e.g. temperature or pressure variations, compensating for signal noise
    • G01N29/326—Arrangements for suppressing undesired influences, e.g. temperature or pressure variations, compensating for signal noise compensating for temperature variations
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F1/00—Measuring the volume flow or mass flow of fluid or fluent solid material wherein the fluid passes through a meter in a continuous flow
    • G01F1/76—Devices for measuring mass flow of a fluid or a fluent solid material
    • G01F1/78—Direct mass flowmeters
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/021—Gases
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0256—Adsorption, desorption, surface mass change, e.g. on biosensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/028—Material parameters
    • G01N2291/02809—Concentration of a compound, e.g. measured by a surface mass change
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/028—Material parameters
    • G01N2291/02836—Flow rate, liquid level
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/04—Wave modes and trajectories
    • G01N2291/042—Wave modes
    • G01N2291/0426—Bulk waves, e.g. quartz crystal microbalance, torsional waves

Definitions

  • the invention relates to a method for operating a sensor which has a vibrating body which can be brought into oscillation, the oscillation frequency of which depends on the mass of a condensate of an organic vapor deposited on the surface of the vibrating body, the sensor being part of a device for the deposition of organic layers by condensation of the vapor on a substrate, a value of a change in the oscillation frequency over time for the determination of the mass transport of the vapor through a feed line to a gas inlet element through which the vapor conveyed by a carrier gas is transported to the substrate, is used and wherein the sensor with a heating device in a preparation phase, during which no steam is conveyed to the substrate, is brought to a predetermined operating temperature and in a process phase, while the steam is conveyed to the substrate, is operated at the operating temperature.
  • the invention also relates to a device for performing the method, in particular for depositing organic layers, in particular OLEDs on a substrate.
  • a sensor arrangement for determining a mass flow of an organic vapor from a source in the direction of an OVPD reactor, which has a gas inlet in the form of a showerhead, through which the organic vapor is fed into a process chamber in order to be able to use a mask to condense masked substrate, is in DE 102014102484 Al loading wrote.
  • DE 102017106968 A1 describes a QCM sensor which has an oscillating body that is set into oscillation. The oscillation frequency of the vibrating body is influenced by the mass condensed on the surface of the vibrating body.
  • a vapor pressure of the vapor in a feed line to a gas inlet element in which the sensor is located can be determined from the change in frequency over time.
  • the mass flow of the organic vapor to the gas inlet element can be determined from a mass flow or volume flow of a carrier gas which flows through the feed line.
  • the sensor is cleaned in a cleaning phase by heating the surface of the oscillating body.
  • the process cycles can be longer than 30 minutes, but can also be a few minutes.
  • the process phase can last a few minutes or even just a few seconds.
  • the invention is based on the object of further developing the method mentioned at the beginning and a device for carrying out the method in a manner which is advantageous in terms of use, with provision being made in particular to specify measures with which the times of a process cycle can be reduced and in particular allows the temperature of the sensor surface to be kept more constant during the process phase.
  • the temperature of the surface of the vibrating body is not regulated during the process phase, but rather controlled or such a set of regulating parameters is used in the regulation that the regulation takes place so slowly that it equates to a control .
  • a value for a power is obtained that is fed into the heating device of the sensor in the process phase.
  • the temperature of the vibrating body of the sensor is regulated against a setpoint value.
  • a mean value of the heating power transmitted to the vibrating body in the power determination phase is preferably formed.
  • This mean power value is used in the process phase that preferably follows immediately in order to heat the oscillating body. Due to the electrical power fed into the heating device during the process phase, no temperature fluctuations occur when the organic material condenses on the surface of the oscillating body during the process phase. It can be provided that the duration of the power determination phase is greater than the duration of the process phase during which steam is fed into the process chamber. It is therefore advantageous if the temperature of the sensor body and in particular its surface is only regulated a time before the process phase and is only controlled in the actual process phase or is regulated with such high time constants that this regulation is technically equivalent to a control.
  • a second aspect of the invention relates to the cleaning phase, during which the vibrating body is heated to an elevated temperature at which organic material evaporates from the surface of the vibrating body.
  • the radiator is operated until it reaches a cleaning temperature with a first output that is at least 95 percent of the maximum possible output, but which can also be 100 percent of the maximum possible output.
  • the first step can, however, also be carried out for a specified time. According to a preferred embodiment of the method, the first cleaning step is carried out until either a predetermined cleaning temperature is reached or a predetermined first time has passed.
  • the temperature of the surface of the vibrating body increases at a maximum rate of temperature change.
  • the heating device is operated with the maximum power of a power supply designed to operate the heating device.
  • the maximum possible power can also be the maximum power that can be fed into the heating device without destroying it.
  • a second step preferably immediately following the first step of the cleaning phase, provides that only a minimal amount of power is supplied to the heating device. This can be 0. It should be a maximum of 5 percent of the maximum output.
  • the surface temperature of the vibrating body drops. This can be done, for example, by extracting heat from the oscillating body and / or the heating device according to DE 102017106968 A1.
  • a cooling device can be provided for this purpose.
  • the second step which is a cooling step, is carried out until a switching temperature is reached.
  • the value of the switching temperature can be between the operating temperature and the cleaning temperature. It can be provided that the switching temperature differs from the operating temperature by an additive value, which is determined in a calibration process.
  • the process cycle contains a phase in which the temperature of the sensor body and in particular the sensor surface is regulated to a predetermined value and a subsequent phase in which the temperature is controlled, namely in particular by that a maximum Power is fed into the heating device or the sensor body is cooled with a maximum cooling power by reducing the heating power to 0.
  • a third step of the cleaning phase which can directly follow the second step of the cleaning phase, the heating device is operated with a predetermined third power. This is less than a power averaged during a power determination phase to reach the operating temperature. As a result, the cooling of the surface of the vibrating body is delayed.
  • the third step of the cleaning phase can be carried out for a predetermined third time.
  • the third step of the cleaning phase can be followed by a fourth step of the cleaning phase, in which the control device regulates the temperature of the oscillating body against the setpoint value. During this regulated operating phase, the power increases continuously until an equilibrium is reached in which the power fluctuates around an average value.
  • the predetermined third power with which the heating device is operated in the third cleaning phase can be in a predetermined ratio to the averaged power determined in the power determination phase for reaching the operating temperature.
  • the power value for reaching the operating temperature can be multiplied by a factor greater than 0 and less than 1.
  • the method according to the invention preferably leads not only to an improved process result, but also to a shortened process duration due to reduced cleaning times.
  • Fig. 2 schematically shows a sensor according to DE 102017106968 A1, as it can be used to carry out the method and
  • FIG. 3 schematically shows a device according to DE 102014102484 A1, as it can be used to carry out the method.
  • FIG. 3 An apparatus on which the method according to the invention can be carried out is shown in FIG. 3.
  • an inert gas for example nitrogen
  • the mass flow controller 14 can be regulated by a control device 12.
  • an aerosol generator 13 which can also be regulated by the control device 12
  • an aerosol of an organic starting material is generated, which is fed into an evaporation body 15 of the evaporation device heated to an evaporation temperature.
  • the aerosol particles are evaporated on the surfaces of the evaporation body 15. Downstream of the evaporation body 15 is a sensor 11, with which the partial pressure of the organic vapor within a feed line 8 to an OVPD reactor 1 can be determined.
  • the mass flow of the organic vapor to the OVPD reactor 1 can be determined.
  • this has a heater 9 with which the surface temperature of the wall of the supply line 8 is kept at a temperature which is above the condensation on temperature of the organic vapor.
  • the sensor 11 is a QCM. It has an oscillating body 16 with a free surface 16 'on which the vapor of the organic material can kondensie Ren. With its side facing away from the free surface 16 ', the oscillating body 16 is connected to a heating device 17 in a temperature-conducting manner. The heating device 17 is in turn connected to a cooling element 18 via an insulation element 19 in a less thermally conductive manner. If the Bankeinrich device 17 is heated with a certain power, then both heat is dissipated to the oscillating body 16 and to the cooling element 18. In this mode of operation, in which a net heat flow flows to the oscillating body 16, the oscillating body 16 can be brought to a temperature at which condensed material can evaporate there.
  • the heating device 17 is heated with a lower power, heat can be drawn from the oscillating body 16 and dissipated through the heating device 17 and the insulation element 19 to the cooling element 18.
  • the surface 16 'of the oscillating body 16 is kept at a temperature at which organic material can condense on the surface 16'.
  • the cooling element 18 is preferably operated exclusively in a controlled manner by feeding a coolant with a predetermined cooling temperature into the cooling element 18, for example.
  • the cooling element 18 it can be can also be a Peltier element that is operated with a specified cooling capacity.
  • FIG. 1 shows an example of a process cycle for depositing an organic layer on a substrate 10, which is located on a substrate holder 5 of an OVPD reactor 1.
  • the substrate holder 5 hasdeka channels 6 through which a cooling liquid can flow.
  • a process chamber 7 is located above the substrate holder 5 or the substrate 10 resting on the substrate holder 5. At the top, the process chamber 7 is delimited by a gas outlet surface of a gas inlet element 2 which has a gas distribution chamber 3, of which a plurality of gas outlet openings 4 in the gas outlet surface open.
  • the gas distribution chambers 3 are fed from the feed line 8 with the organic vapor transported by the carrier gas.
  • the process cycle shown in FIG. 1 is repeated several times in succession. It consists of a preparation phase V, in which no steam is fed into the process chamber 7, and a process phase B, in which steam is fed into the process chamber 7.
  • the preheating phase V includes a power determination phase A, a cleaning phase, which has sections C, D, F and an optional phase G, in which essentially only the temperature of the oscillating body is maintained.
  • this phase G at a mean humidity P m, the temperature of the Schwingkör pers 16 and in particular the surface temperature of the surface 16 'is regulated against a target value, so that the temperature assumes a process temperature T p. This is done by means of the control device 12.
  • phase G the humidity and the temperature in FIG. 1 are shown fluctuating around a mean value.
  • a power determination phase A in which the temperature of the oscillating body 16 and in particular its surface 16 'is also regulated, an averaged power P is determined. This takes place without organic steam being fed into the process chamber 7 or without aerosol particles being evaporated by the evaporation body 15.
  • a process phase B in which organic vapor is generated, for example in that aerosol particles are fed into the evaporation body 15 or the evaporation body 15 is brought to an evaporation temperature
  • the heating device 17 is operated in an uncontrolled manner. It is electrically energized with a constant heating power, where this power corresponds to the power that has been determined in the power determination phase A.
  • the duration of the performance determination phase A can be greater than the duration of process phase B, which can only last a few seconds (less than 20 seconds).
  • the surface 16 'of the oscillating body 16 can be cleaned.
  • the surface 16 ' is heated to a cleaning temperature. According to the invention, this takes place during a cleaning phase.
  • the cleaning phase has four steps:
  • the heating device 17 is entered with maximum power P M&X .
  • the time of the first step can be provided. However, the time of the first step can also be a maximum value.
  • the first step can be ended, for example, when either a predetermined time has elapsed or the cleaning temperature TR has been reached.
  • the power with which the heating device 17 is operated can be an electrical power source that generates maximum power. gen can. However, the maximum power can also be the maximum power that can be fed into the heating device 17 without destroying the heating device 17.
  • the heating device 17 is applied with minimum power, preferably not at all with power, so that the cooling element 18 can unfold its maximum power.
  • the second step of the cleaning phase can be ended when the surface temperature of the oscillating body 16 reaches a predetermined value. This can be, for example, T p + X2, where X2 is a calibration parameter that can vary from system to system. This calibration value can be determined in preliminary tests.
  • the heating device 17 is subjected to a power which is between 0 and the mean power P m to reach the operating temperature T p .
  • the power fed in in this step preferably has a level which is sufficiently high to avoid the temperature not falling below the process temperature. This step ensures that in the third step described below, the temperature does not drop below a predetermined value.
  • the third step E is followed by a fourth step F of the cleaning phase, in which the heating device 17 against the setpoint of the operating temperature T p is regulated.
  • a method which is characterized in that the temperature of the surface 16 'of the oscillating body 16 is regulated to a setpoint value by a control device 12 in the preparation phase V, and in the process phase B the heating device is operated with a first predetermined power P will practice.
  • a method which is characterized in that the Schueinrich device 17 in a first step C of the cleaning phase for a predetermined first time and / or until reaching the cleaning temperature TR with a first power that is at least 95 percent of a maximum possible power is operated and in a second step D, which immediately follows the first step C of the cleaning phase, is operated with a second power, which is a maximum of 5 percent of the maximum possible power, until a switching temperature Ts is reached whose value lies between the operating temperature T p and the cleaning temperature TR.
  • a method which is characterized in that, following the third step E of the cleaning phase, in a fourth step L of the cleaning phase, the temperature of the oscillating body is regulated to a target value by means of the regulating device 12.
  • a device which is characterized in that the control device 20 is set up in such a way that the temperature of the surface 16 'of the oscillating body 16 changes according to one of the preceding claims 1 to 8.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Acoustics & Sound (AREA)
  • Fluid Mechanics (AREA)
  • Cleaning In General (AREA)

Abstract

L'invention concerne un procédé permettant de faire fonctionner un capteur QCM, selon lequel la surface (16') du corps flottant (16) est réglée pendant une phase de préparation (V) à une valeur de consigne par un dispositif de réglage (12) et pendant la phase de traitement (B), un dispositif de chauffage (17) est actionné à une première puissance prédéfinie. Pour nettoyer le capteur, dans une première étape (C) de la phase de nettoyage, le dispositif de chauffage (17) est actionné, pendant une première période et/ou jusqu'à ce que la température de nettoyage (TR) est atteinte, à une première puissance qui représente 95 pour cent d'une puissance maximale possible, et dans une seconde étape (D), qui intervient immédiatement dans le prolongement de la première étape (C), ledit dispositif ce chauffage est actionné à une seconde puissance qui représente au plus 5 pour cent de la puissance maximale possible, jusqu'à ce qu'une température de commutation (TS) est atteinte, dont la valeur se situe entre la température de fonctionnement (TP) et la température de nettoyage (TR).
PCT/EP2020/079185 2019-10-22 2020-10-16 Procédé pour faire fonctionner un capteur à microbalance à cristal de quartz WO2021078644A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102019128515.1A DE102019128515A1 (de) 2019-10-22 2019-10-22 Verfahren zum Betrieb eines QCM-Sensors
DE102019128515.1 2019-10-22

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WO2021078644A1 true WO2021078644A1 (fr) 2021-04-29

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WO (1) WO2021078644A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102020116271A1 (de) 2020-06-19 2021-12-23 Apeva Se Vorrichtung und Verfahren zum Verdampfen eines organischen Pulvers

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4748367A (en) * 1985-05-28 1988-05-31 Frequency Electronics, Inc. Contact heater for piezoelectric effect resonator crystal
US20040018650A1 (en) * 2002-06-11 2004-01-29 Hitachi Kokusai Electric Inc. Substrate processing apparatus
DE20221736U1 (de) * 1974-10-23 2007-05-16 Avl List Gmbh Vorrichtung zur Bestimmung des nichtflüchtigen Anteils von Aerosolpartikeln in einer Gasprobe
DE102014102484A1 (de) 2014-02-26 2015-08-27 Aixtron Se Verwendung eines QCM-Sensors zur Bestimmung der Dampfkonzentration beim OVPD-Verfahren beziehungsweise in einem OVPD-Beschichtungssystem
WO2018077388A1 (fr) * 2016-10-25 2018-05-03 Applied Materials, Inc. Ensemble de mesure pour mesurer une vitesse de dépôt, source d'évaporation, appareil de dépôt et procédé associé
DE102017106968A1 (de) 2017-03-31 2018-10-04 Aixtron Se Vorrichtung und Verfahren zur Bestimmung der Konzentration eines Dampfes

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5854731B2 (ja) * 2010-11-04 2016-02-09 キヤノン株式会社 成膜装置及びこれを用いた成膜方法
DE102015104240A1 (de) * 2015-03-20 2016-09-22 Aixtron Se Durch Aufheizen zu reinigender QCM-Sensor und dessen Verwendung in einem OVPD-Beschichtungssystem

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE20221736U1 (de) * 1974-10-23 2007-05-16 Avl List Gmbh Vorrichtung zur Bestimmung des nichtflüchtigen Anteils von Aerosolpartikeln in einer Gasprobe
US4748367A (en) * 1985-05-28 1988-05-31 Frequency Electronics, Inc. Contact heater for piezoelectric effect resonator crystal
US20040018650A1 (en) * 2002-06-11 2004-01-29 Hitachi Kokusai Electric Inc. Substrate processing apparatus
DE102014102484A1 (de) 2014-02-26 2015-08-27 Aixtron Se Verwendung eines QCM-Sensors zur Bestimmung der Dampfkonzentration beim OVPD-Verfahren beziehungsweise in einem OVPD-Beschichtungssystem
WO2018077388A1 (fr) * 2016-10-25 2018-05-03 Applied Materials, Inc. Ensemble de mesure pour mesurer une vitesse de dépôt, source d'évaporation, appareil de dépôt et procédé associé
DE102017106968A1 (de) 2017-03-31 2018-10-04 Aixtron Se Vorrichtung und Verfahren zur Bestimmung der Konzentration eines Dampfes

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