WO1997030185A1 - Procede et dispositif pour la regulation d'un processus de revetement sous vide - Google Patents

Procede et dispositif pour la regulation d'un processus de revetement sous vide Download PDF

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Publication number
WO1997030185A1
WO1997030185A1 PCT/DE1997/000264 DE9700264W WO9730185A1 WO 1997030185 A1 WO1997030185 A1 WO 1997030185A1 DE 9700264 W DE9700264 W DE 9700264W WO 9730185 A1 WO9730185 A1 WO 9730185A1
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WO
WIPO (PCT)
Prior art keywords
coating
source
weight
vacuum chamber
signal
Prior art date
Application number
PCT/DE1997/000264
Other languages
German (de)
English (en)
Inventor
Klaus Goedicke
Christoph Metzner
Bert Scheffel
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Publication of WO1997030185A1 publication Critical patent/WO1997030185A1/fr

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3476—Testing and control
    • H01J37/3479—Detecting exhaustion of target material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/304—Controlling tubes by information coming from the objects or from the beam, e.g. correction signals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching
    • H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3402—Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
    • H01J37/3405—Magnetron sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/31—Processing objects on a macro-scale
    • H01J2237/3128—Melting

Definitions

  • the invention relates to a method and a device for controlling an evaporation or atomization process in a vacuum chamber. Following the procedure in particular ⁇ be sondere disk and tape-like substrates or tools with functional layers coated be ⁇ .
  • the coating rate It is known to measure the coating rate at one or more locations near the substrate or to measure the steam flow between the coating source and the substrate, it being possible for the coating source to be an evaporator or an atomization source.
  • the coating rate There are a large number of methods for determining the coating rate, such as, for example, measuring the layer thickness by means of quartz crystal or microbalance in the vicinity of the substrate (Kienel, G .: Vacuum Coating Volume 3 - Plant Automation, VDI-Verlag, Düsseldorf, 1994, p.25 ff, P.35 ff, p.40 ff).
  • the coating rate is determined using these methods for measuring the layer thickness. With the signal obtained, the evaporation speed and thus the evaporation or atomization process are regulated via a control loop.
  • the main disadvantage of these methods is the measuring arrangement.
  • the sensors must be arranged in the steam chamber and are therefore subject to such a high steam and heat load that they have to be replaced after a relatively short time. This means that frequent process interruptions are necessary and long-term operation is hardly possible. For this reason, these processes for controlling coating processes are only suitable for low coating rates. Furthermore, only a small part of the steam flow is measured, from which the entire steam flow reaching the substrate is deduced. This has a particularly disadvantageous effect on large-area substrates, since the sensors, in order not to shade the substrate, are at a different distance and angle to the coating source than the substrate are arranged and therefore the vapor flow density to the sensor has a different size than the vapor flow density to the substrate. This leads to errors.
  • the sensors involved are not located directly in the steam flow, but are laterally offset from the steam flow.
  • the main disadvantage of these methods is that, besides the steam flow, the measured variables also depend to a large extent on other coating parameters, such as depend on the coating material, ionization and excitation of the steam. These measuring arrangements must therefore be recalibrated for each coating material, which is very complex.
  • a further disadvantage is that the sensors have to be arranged in the steam space and are therefore in turn subject to a gradual coating. As a result, process interruptions for changing the sensors are also required, which is disadvantageous for long-term operation.
  • the rate of evaporation in evaporation processes has hitherto only been determined as an average over time by interrupting the coating process at greater intervals and weighing the evaporation material before and after coating.
  • this method is unsuitable for industrial use, since the evaporation rate is only averaged over large time intervals and is therefore not available for constant control of the coating process, or the coating process for weighing would have to be interrupted continuously.
  • no suitable method is known that is able to evaluate the current evaporation rate or atomization rate during the process.
  • a method for monitoring the fill level of evaporator crucibles with light or laser beams is known.
  • a light beam is reflected on the surface of the coating material and closed from the beam path to the fill level of the crucible (DE 38 27 920 A1).
  • This method has the disadvantage that the beam path is disturbed by possible wave movements of the surface of the evaporation material.
  • the method also has the deficiency that the beam, by having to be guided through the areas of highest vapor density, is subject to scattering and absorption, which leads to a falsification of the measurement result. For this reason, this method is only suitable to a limited extent to regulate a coating process in order to meet the high requirements for the stability of the coating rate and the exact composition of the vapor-deposited layer.
  • the invention has for its object to provide a method and a device which allow a vacuum coating process to be adapted to a given coating technology by monitoring the coating process, in particular evaporation by means of electron beams, and influencing its parameters in such a way that a individual, plate-shaped or ribbon-shaped substrates are reactively or non-reactively vapor-deposited with high layer quality, with uniform layer thicknesses being achieved with a predetermined layer composition, in particular in the case of large-area substrates.
  • the process should also be suitable for atomization processes, in particular for long-term processes.
  • the atomization sources should be arranged in any position.
  • the coating process should be simple and reliable to carry out over a long period of time.
  • the device should be simple in terms of apparatus.
  • the coating rate by weighing In contrast to the known methods for determining the coating rate by weighing, it was found to measure the use of the weight during the coating process and to process this value further as a signal. This is done by differentiating the measurement signal obtained over time. With this differentiated signal and the measurement signal, it is possible to use a control circuit known per se. ter of the evaporation or atomization process, in particular the nominal evaporation rate or atomization rate.
  • the differentiated signal determined is a direct measure of the effective evaporation rate or atomization rate. There is the difference between the nominal rate of evaporation or atomization rate and the rate of condensation of steam or gas particles on the coating material.
  • the most important advantage is that in this method a signal is determined from the consumption of coating material in order to regulate parameters of the evaporation or atomization in such a way that the evaporation rate or the atomization rate remains constant or during the coating process is specifically changed in accordance with the coating technology.
  • the coating process is thus regulated in a direct manner, since the properties of the applied layers are essentially determined by evaporation or atomization.
  • the weight can be measured simply and continuously without interrupting the coating process, which means that the signal obtained can also be used to continuously control it.
  • the entire flow of coating material and not just a partial area for characterization is measured via this signal.
  • the coating source is fixed in the vacuum chamber by means of force cells.
  • the load cells are e.g.
  • the surfaces of the coating material may be contaminated, which consequently leads to a change in the rate of evaporation or atomization and to a change in the composition of the layer material.
  • the flow of the reactive gas into the vacuum chamber can also be controlled, so that with the weight obtained and differentiated signal of the gas inlet is controlled so that the differentiated signal adjusts to a predetermined setpoint.
  • the regulation of a coating process is carried out as follows.
  • the weight of the evaporation or sputtering material is measured together with the weight of the evaporator or the sputtering source during the evaporation or sputtering process ⁇ by one or more load cells continuously.
  • the weight is converted by the load cells into an electrical analog or digital signal.
  • This signal from the load cells is first subjected to filtering in a known manner. This filtering can be carried out analogously with an electronic low-pass filter or through digital filters.
  • the filtered signal is then differentiated over time. This differential formation takes place in an analog or digital way.
  • the filtered signal of the weight and the differentiated signal as a measure of the rate of evaporation or atomization rate are supplied as measured variables to a known control circuit which acts on the parameters determining the evaporation or atomization.
  • a large number of parameters can be controlled by this method in order to control the evaporation or atomization and thus have a direct influence on the coating process.
  • the measurement signal obtained from the weight can advantageously be used to influence these deflection parameters and / or to focus the beam.
  • a further advantageous embodiment of the method for controlling coating processes consists in using the undifferentiated signal in the case of evaporator crucibles with continuously working refill devices for the evaporation material in order to regulate the refill quantity in such a way that the quantity of the evaporation material or the fill level remains constant in the evaporator crucible. Long-term stability of the evaporation rate is thereby achieved, since this also depends on the filling level.
  • the consumption of coating material or the instantaneous filling level of the evaporator crucible or the depth of erosion of the target of the atomization source can be determined from the measurement signal.
  • the coating process is regulated by regulating the beam focusing and / or the deflection parameters during evaporation or a magnetic field penetrating the target during atomization in order to avoid a change in the coating rate. This also determines the time and the amount for refilling the evaporation material or the change of the target.
  • the device for carrying out the method has the advantage that existing devices can also be retrofitted without great effort, since the coating sources are no longer directly connected to the vacuum chamber, but instead force measuring cells are arranged between the coating source and the vacuum chamber. Furthermore, a conventional control circuit is necessary, which in the simplest case consists of a filter, a differentiating element and a controller with which the measurement signal is processed in order to regulate the corresponding parameters of the coating process.
  • FIG. 2 shows a section through a device for carrying out the method with a magnetron sputtering source
  • an electron gun 2 of the axial type is arranged on one side of a vacuum chamber 1, the electron beam 3 of which is applied to a titanium-filled evaporator crucible 4.
  • the evaporator crucible 4 is fastened in the vacuum chamber 1 by means of load cells 5, consisting of elastic elements with applied strain gauges.
  • a substrate 6 to be coated is arranged above the evaporator crucible 4.
  • the filter 7 connected downstream of the load cells 5 prepares the signals of the forces measured with the load cells 5.
  • the output signals of the filter 7 are a difference ornamental element 8 supplied.
  • the output signals of the filter 7 and the differentiator 8 are then fed to a controller 9. This processes the signals and compares them with specified target values.
  • the desired value for the power controller 10 of the electron gun 2 is tracked.
  • the setpoint parameters for the deflection control 11 are changed by the controller 9.
  • the vacuum chamber 1 there is also a refill device 12 with which evaporation material is continuously fed to the evaporator crucible 4.
  • This refill device 12 is controlled by the controller 9 so that the output signal of the filter 7 remains constant.
  • two magnetrons 13 with a titanium target and adjustable magnetic device are arranged within a vacuum chamber 1.
  • the magnetrons 13 are fastened in the vacuum chamber 1 by means of force measuring cells 5, consisting of elastic elements with applied strain gauges.
  • the substrate 6 to be coated is arranged above the magnetron 4.
  • the filters 7 connected downstream of the load cells 5 process the signals of the forces measured with the load cells 5.
  • the output signals of the filters 7 are fed to a differentiator 8.
  • the output signals of the filter 7 and the differentiator 8 are then fed to a controller 9. This processes the signals and compares them with specified target values. If the output signal of the differentiating element 8 deviates from a desired value for the atomization rate, the desired value for the adjustable magnetic device of the magnetrons 13 is adjusted so that the output signal of the differentiating element 8 remains constant.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

Dans les procédés connus permettant la régulation du processus de revêtement sous vide, des variables mesurables telles que l'émission de plasma et la vitesse de revêtement sont mesurées dans le plasma ou la vapeur afin de réguler le processus de revêtement sous vide à l'aide de paramètres de processus de la vaporisation ou de la pulvérisation cathodique. Les capteurs sont soumis à de fortes sollicitations, et leur longévité s'en trouve affectée. A l'aide du poids comme variable mesurable dérivée du poids du matériau de revêtement et de la source de revêtement, le processus de revêtement sous vide est régulé par la mesure de la perte de poids lors du revêtement. La source de revêtement est disposée dans la chambre à vide à l'aide de transducteurs de force, et le signal émanant de ces transducteurs de force sert à réguler, par exemple, l'énergie électrique pour chauffer le matériau de vaporisation, la déflection du faisceau ou le flux de gaz, sans que les capteurs viennent en contact avec le plasma ou la vapeur. Ce procédé et ce dispositif permettent de réguler des processus de revêtement sous vide, notamment pour revêtir des outils et des substrats laminaires avec des couches fonctionnelles.
PCT/DE1997/000264 1996-02-14 1997-02-07 Procede et dispositif pour la regulation d'un processus de revetement sous vide WO1997030185A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE1996105315 DE19605315C1 (de) 1996-02-14 1996-02-14 Verfahren und Einrichtung zur Regelung eines Vakuumbeschichtungsprozesses
DE19605315.3 1996-02-14

Publications (1)

Publication Number Publication Date
WO1997030185A1 true WO1997030185A1 (fr) 1997-08-21

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DE (1) DE19605315C1 (fr)
WO (1) WO1997030185A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104651779A (zh) * 2015-02-11 2015-05-27 烟台首钢磁性材料股份有限公司 一种用于钕铁硼磁体的镀膜设备及镀膜工艺

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004006530B4 (de) * 2004-02-10 2007-04-05 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren und Vorrichtung zum Einbringen von Gasen bei Vakuumbeschichtungsprozessen
DE102010040044B4 (de) * 2010-08-31 2014-03-06 Von Ardenne Anlagentechnik Gmbh Beschichtungsanlage und Verfahren für eine physikalische Gasphasenabscheidung
DE102013219999A1 (de) * 2013-10-02 2015-04-02 Singulus Technologies Ag Tiegelverdampfer

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD239810A1 (de) * 1985-07-31 1986-10-08 Ardenne Forschungsinst Einrichtung zur kontrolle einer plasmatronquelle
DE3827920A1 (de) * 1988-08-17 1989-01-19 Hugh Burns Neill Methode und geraet zum ertasten von unterschiedlichen ebenen

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD239810A1 (de) * 1985-07-31 1986-10-08 Ardenne Forschungsinst Einrichtung zur kontrolle einer plasmatronquelle
DE3827920A1 (de) * 1988-08-17 1989-01-19 Hugh Burns Neill Methode und geraet zum ertasten von unterschiedlichen ebenen

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104651779A (zh) * 2015-02-11 2015-05-27 烟台首钢磁性材料股份有限公司 一种用于钕铁硼磁体的镀膜设备及镀膜工艺

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Publication number Publication date
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