Classifications

• • 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
  • C23C14/04—Coating on selected surface areas, e.g. using masks
  • C23C14/046—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
• • 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
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/12—Organic 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
  • C23C14/243—Crucibles for source material
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
  • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
  • H10K71/10—Deposition of organic active material
  • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
  • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
  • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
  • H10K85/30—Coordination compounds
  • H10K85/341—Transition metal complexes, e.g. Ru(II)polypyridine complexes
  • H10K85/342—Transition metal complexes, e.g. Ru(II)polypyridine complexes comprising iridium

Definitions

• the invention relates to a method for coating a substrate having a plurality of material layers of at least two different materials according to the preamble of claim 1.
• the invention also relates to a multi-material delivery device according to claim 8.
• the invention relates to the field of coating substrates with material layers of a plurality of different materials.
• Applications of such methods are present in various fields of technology, e.g. B. for the production of organic light emitting diodes (OLED).
• OLED organic light emitting diodes
• three or more layers are deposited on a substrate in a predetermined order, wherein it is desirable that a uniform material deposition occurs and the layers are formed in a desired layer thickness.
• DE 60 2005 002 033 T2 discloses a vapor deposition of temperature-sensitive materials for OLED devices.
• a material in a vaporization device is metered at a controlled rate from a first heating area to a second heating area in which the material is finally vaporized.
• temperature-sensitive organic materials are spared, because they do not have to be held constantly for a long time at high temperature.
• the object is achieved according to claim 1 by a method for coating a substrate with a plurality of material layers of at least two different materials, the material layers being produced on the substrate by means of a material dispensing rate-controllable material dispensing device, wherein the material dispenser is a multi-material dispensing device, Stock levels of the at least two different materials are simultaneously held in the multi-material delivery device and the at least two different materials are deposited on the substrate by controlling the multi-material delivery device thereof in the desired order.
• the object is further achieved according to claim 8 by a multi-material dispensing device, configured for carrying out the aforementioned coating method or other subsequently mentioned coating methods, wherein the multi-material dispenser is controllable with respect to the dispensing rate of materials to be dispensed from the multi-material dispenser and one or more pantries for receiving the storage quantities of the at least two different materials.
• the invention has the advantage that, in comparison with the prior art, substrates can be coated more efficiently, faster and thus more cost-effectively with a plurality of material layers, wherein in particular a high process quality and repeatability of the coating processes can be achieved.
• layers of material can be formed on the substrate of at least two different materials without substantial mixing of the materials. So a material layer of a first material and thereon a material layer of a second material are deposited, wherein the materials essentially do not mix as mentioned, apart from due to the materials used possibly unavoidable transitions at the interfaces of the material al harshen .. It can thus be practical pure layers are produced from the materials held in the multi-material delivery device.
• such coating processes can be realized in a large-scale industrial scale and, for example, OLED lamps in mass production can be produced at favorable costs.
• the invention is also particularly well suited for the inner coating of substrates which are formed as hollow bodies, for example for the production of OLED bulbs in classic "light bulbs” shape or “fluorescent tubes” form, which have an inner coating with the OLED materials.
• By controlling the material dispensing device with regard to the material dispensing rate defined dispensing rates of the respective material can be generated. Due to the design of the material delivery device as a multi-material delivery device which has storage quantities of the at least two different materials at the same time, the coating process can be made more efficient.
• the deposition of the at least two different materials on the substrate can be carried out without intermediate replacement of the multi-material delivery device or interim repositioning of the multi-material delivery device with materials, ie during the coating process.
• the coating process can be carried out continuously in a sequence, which is particularly efficient in coating processes with a larger number of different materials or processes with frequent changes of materials, in particular in the production of OLED lamps.
• the control of the multi-material delivery device can be material-specific, ie the material release rate and further material delivery parameters can be set specifically depending on the type of material just dispensed by the multi-material delivery device.
• the Ver- driving is particularly advantageous in a RESIZE ßeren sequence of different materials, which can be repeated in the sequence of materials individual types of material.
• an electronic control device may be provided for the control of the multi-material delivery device, which is coupled to the multi-material delivery device and is set up with regard to the control of the material delivery rate, for. B. by programming a computer, z. As a microprocessor or micro- controller, the electronic control device.
• the control program is then designed in such a way that the electronic control device is designed to carry out, by means of the control of the multi-material delivery device, a method of the type described above or below, when the control program is executed on a computer of the electronic control device.
• a target layer thickness to be generated is predetermined for each material layer.
• the material layers are deposited on the substrate with the desired layer thickness to be generated solely by controlled actuation of the multi-material delivery device without a layer thickness measurement being carried out during the coating process.
• the fact that no layer thickness measurement during the coating process is required in the method according to the invention has further significant advantages over the prior art.
• it has hitherto been common practice to measure the rate of the deposited material or the layer thickness during the coating process for example by means of a quartz crystal which was arranged in the vicinity of the substrate to be coated.
• the layer thickness was measured, for example, by means of a frequency shift of the vibrating quartz as a result of a thicker material layer.
• either direct control without regulation of the multi-material delivery device can take place if, as described in more detail below, the materials to be dispensed are kept in a predefined manner and there is a clear, previously known relationship between the control input data of the multi-material dispenser and the material dispensing rate.
• a local control loop can be set up, in which only internal values of the multi-material delivery device are reported back to the electronic control device as a set value, such as, for example, B. the current position of a feed device.
• the multicomponent delivery device is controlled by means of an electronic control device on the basis of parameters of the materials held in the multi-material delivery device and / or geometry parameters of the surface of the substrate to be coated.
• the mentioned parameters can z. B. be stored in advance in the electronic control device and then called by the electronic control device in the course of the coating process.
• parameters of reproached in the multi-material delivery device materials can, for. B. the type of material (chemical composition), the material-specific evaporation temperature, the order or position of the respective material in the storage chamber, the respective amount of material or their spatial extent are stored in the pantry.
• the geometric shape of the substrate for example, a flat surface or a hollow body shape, such as a spherical shape or an ellipsoidal shape, stored.
• the electronic control device can control the coating process solely on the basis of the parameters predetermined in advance. Precise pre-definable coatings of the substrate with high repeatability can be achieved with the mentioned method.
• the material to be deposited is evaporated by at least one controllable by an electronic control device heater.
• the electronic control device controls the heater in response to the respective material to be evaporated to a predetermined heating temperature.
• an adapted and targeted control can be carried out by an electronic control device, which may be the same as the aforementioned electronic control device.
• the materials to be vaporized can thus be optimally processed in each case so that, in particular, sensitive materials are not or only minimally damaged and yet a maximum processing speed can be achieved.
• the method is particularly advantageous for a larger sequence of different materials.
• the heater is operated in each case adapted to the currently being evaporated material.
• the Mehrmateria- lienabgabe listening is at least partially, in particular with a material discharge head (also called distributor head or injector) introduced into a cavity of the substrate and the cavity is coated with the materials to be deposited from the inside.
• a material discharge head also called distributor head or injector
• OLED bulbs are manufactured in conventional "bulbs" shape or “fluorescent tubes” shape.
• the abschechei- materials in the multi-material delivery device in defined spatial dimensions.
• An electronic control device which may be the aforementioned electronic control device, controls the multi-material dispenser taking into account data of at least one of the spatial dimensions of the held materials.
• the electronic control device z. B. the feed of a material in the Mehrmaterialienabgabe coupled and the heating temperature of a heater based on the information about the at least one spatial dimension of the materials held automatically control
• the electronic control device can also take into account the respective operating position of the feed device advantageous.
• the multi-material delivery device for generating a feed of the materials in the storage chamber having a motor drive.
• the electronic control device then controls the motor drive in such a way that, depending on the material currently to be evaporated located on the heating device, the further advance of the material against the heating device is controlled.
• the heating device is controlled to a material-specific tuned heating temperature.
• the controller can detect when a material is completely evaporated and the next material is supplied to the heater.
• the control device can then adjust the heating temperature of the heating device to the new material and predefine a further feed rate adapted to the material by controlling the motor drive of the multi-material dispensing device.
• supply quantities of the at least two different materials in the multi-material discharge device are kept stacked in solid form in the same storage chamber.
• the solid form encompasses all types of solids, as opposed to liquids and gases.
• the materials can z.
• the multi-material delivery device may have a single storage chamber in which all materials to be dispensed are kept stacked. It is also possible to form the multi-material delivery device with more than one pantry, z. B. with two or more pantries. In this case, each stack of different materials or only a single material can be kept in the individual pantries. Depending on the configuration, the multi-material delivery device can also have as many storage chambers as different materials to be dispensed. In this case, each pantry can be equipped with a single material. If a pantry is populated with a single material, no material mixing can occur even if materials are not kept in solid form. According to an advantageous development of the invention, the multi-material delivery device is designed to dispense at least two different materials, which are held in more than one storage chamber, wherein one or more materials are held in each storage chamber.
• the materials can be stored in the pantry, or in the pantries, at room temperature or by means of a cooling device, or kept heated by means of a heating device. However, it is on To ensure that a reasonable common temperature is selected for all materials in the storage chamber, which does not lead to damage to the materials. In particular, the temperature of the storage chamber should be kept below the lowest evaporation temperature of all materials located therein. If several pantries are available, they can be operated at the same or different temperatures depending on the materials contained therein.
• a storage chamber of the multi-material delivery device can also be equipped with a separation material which is not adapted to be deposited on the substrate.
• the separation material can be arranged, in particular when a plurality of different materials are arranged in one and the same storage chamber, as a separation layer between two materials intended for deposition on the substrate in order to improve a separation of the materials in the storage chamber and / or around the transitions in dispensing the two different materials from the multi-material delivery facility.
• a separation material is provided between two materials to be deposited on the substrate, which have greatly different sublimation temperatures.
• the separation material can compensate for the different sublimation temperatures by e.g. has a mean sublimation temperature.
• the separation material can be used in particular as a "sacrificial material" which is not deposited on the substrate via a material discharge head but is conducted via a separate discharge line into a collecting container the separation material is passed to the collecting container and not to the substrate,
• acrificial material which is not deposited on the substrate via a material discharge head but is conducted via a separate discharge line into a collecting container the separation material is passed to the collecting container and not to the substrate
• an organic material can be used as the separating material.
• the multi-material dispensing device has at least one controllable motor, by the control of which the material dispensing rate of the multi-material dispensing device is controlled. is recoverable.
• the controllable motor may be formed, for example, as a stepper motor, which drives an appropriate amount of material against the heater depending on the specification of a corresponding number of setting steps by an electronic control device.
• a material delivery targeted with regard to the material delivery rate can also be achieved without additional detection of a feed of the materials by the engine.
• the signal of the position sensor may be supplied to the electronic control device, which controls the heating device and the controllable motor in response to this signal.
• the controllable motor acts on at least one piston of the multi-material delivery device, wherein the piston is retractable by means of the motor in at least one of the storage chambers.
• the piston can z. B. be connected via a spindle drive to the engine.
• the multi-material delivery device can also have a plurality of pistons, each with its own motor or together
• the multi-material dispensing device has at least one controllable heating device, which is set up to vaporize the material to be separated in the respective storage chamber
• the controllable heating device can in particular be controlled by the electronic control device explained above.
• the heating devices are then of the electronic control device separately controllable to a respective matched to the material to be evaporated heating temperature.
• the heater can, for. B. be designed as a heating grid, ie have a grid shape, which is formed for example of a metal material.
• the metal material may be passivating coated, eg to avoid catalytic reactions.
• the heater may be formed, for example, as a heating grid, which has been etched into a silicon wafer. This can be used for passivation z. B. are oxidized.
• the heating device is arranged on the side of the storage chamber opposite the piston.
• the piston can press against the materials present in the storage chamber and presses them against the heating device.
• a certain pressure of the materials is exerted on the heater, so that a targeted and uniform evaporation of the materials can be realized by the heater.
• the material delivery rate of the Mehrmaterialienabga- device is particularly precisely controlled.
• the multi-material dispensing device has a common material dispensing head, on which the at least two different materials deposited from the multi-material dispenser are dispensed.
• This has the advantage that the two materials or, if required, also all the materials are dispensed from the same location, which is also advantageous in the coating of non-hollow body-shaped substrates, since defined deposition conditions are present.
• a particular advantage results for the inner coating hollow body-shaped substrates, since the common material discharge head must be retracted only once in the cavity and then all materials can be introduced via the same material discharge head into the cavity.
• the multi-material dispenser may also include multiple dispensing heads, e.g. B. similar to a lathe in bottling. As a result, a series production of organic light-emitting diodes can be carried out particularly efficiently.
• the multi-material dispenser may also have a separate material dispensing head for certain materials.
• the multi-material dispensing device has a separate material dispensing head for each material or for each storage chamber.
• the multi-material dispensing device can also be designed with only one single material dispensing head, from which all materials to be deposited by the multi-material dispensing device are dispensed.
• the material dispensing head may be shaped differently. It is advantageous to adapt the externa ßere shape of the material discharge head at least approximately to the inner contour of a cavity to be coated.
• the material dispensing head may, for. B. be designed as a rotationally symmetrical body, in particular in the form of a sphere, a cylinder or an ellipsoid.
• z. B. also be designed as a rotationally symmetrical body, in which z. B. for each material to be dispensed a certain surface portion of the rotationally symmetrical body is provided, for. B. a surface area of a sphere, such as in each case a quarter ball.
• the material discharge head is arranged at a distance from the storage chamber and / or the heating device or directly thereto.
• the material dispensing head can eg via a tubular or tubular connection with the pantry or the heater be connected. This allows in particular a favorable material introduction into cavities of substrates, in particular if the material discharge head has to be inserted relatively far into the substrate.
• the material dispensing head is formed heatable.
• the material dispensing head may have an integrated heating device or be heated from the outside by a heating device. This has the advantage that the material discharge head can be specifically heated. As a result, the temperature of the material discharge head can be kept above the sublimation temperature of the respective delivered material during the delivery of material, which has the advantage that discharged material does not or only to a negligible extent precipitates on the material delivery head itself.
• Such heating of the material dispensing head is advantageous, in particular in the inner coating of hollow bodies, in order to ensure that the dispensed material condenses only after leaving the material dispensing head in the comparatively colder hollow body.
• It shows a multi-material delivery device and a substrate to be coated from the inside and deposited on the substrate material layers.
• 1 shows a multi-material delivery device 1 9 with the following elements: 1 0 Electronic control device
• the multi-material delivery device 19 is used for coating a substrate 8, which has a hollow body shape, according to one of the methods described in the introduction.
• the substrate 8 should be coated from the inside.
• the material discharge head 1 8 is inserted into the interior of the substrate 8 and positioned approximately centrally.
• the substrate 8 may be, for example, a glass hollow body or a hollow body made of another transparent material.
• the substrate 8 is held by a holder 9 for the purpose of the coating operation.
• a storage chamber 1 3 is formed in the material storage cylinder 1 2 .
• different materials 1, 2, 3, 4, 5, 6, 7 are provided in solid form.
• the materials 1, 2, 3, 4, 5, 6, 7 are arranged between the piston 1 5 and the heater 1 6 one behind the other in a stack, so to speak.
• the materials 1, 2, 3, 4, 5, 6, 7 may be materials with which the layers of an OLED illuminant can be produced.
• the materials are described below with reference to FIG.
• the piston 1 5 is connected via the push rod 14 to the motor 1 1.
• the engine 1 1 is a controllable engine, for. B. an electric motor, in particular a stepper motor.
• the push rod 1 4 z. B. be formed as a threaded spindle, which can be rotated by the motor 1 1 in rotation. This can the piston 1 5 are moved back and forth. In particular, the piston 1 5 can be moved against the materials 1, 2, 3, 4, 5, 6, 7 and thus press the materials against the heater 1 6.
• the heater B. may be formed as a heating grid, which is acted upon by electric current and thereby heated in the sense of resistance heating.
• the heater can, for. B. be designed as a heating grid, ie have a grid shape, the z. B. is formed of a metal material.
• the metal material may be passivatively coated, e.g. B. to avoid catalytic reactions.
• the heater can, for. B. may be formed as a heating grid, which has been etched into a silicon wafer. This can be used for passivation z. B. are oxidized.
• the electronic control device 1 0 is set up to control the motor 1 1 and the heater 1 6.
• the control device 10 has a computer and a control program executed by the computer.
• the electronic control device 1 0 control signals to the motor 1 1 delivered and thereby the advancement of the piston 1 5 and thus the feed of the materials 1, 2, 3rd , 4, 5, 6, 7 control against the heater 1 6.
• a sensor may be provided in the engine 1 1 or on the piston 1 5 or the push rod 1 4, u m to detect the respective position of the piston 1 5. The signal of the sensor is then transmitted to the electronic control device 10, as indicated by the arrow pointing to the control device 10 by the motor 11. If the motor 1 1 is designed as a stepper motor, can be dispensed with this sensing. In this case, the electronic control device 1 0 can determine itself on the basis of the predetermined steps to the motor 1 1 men, in which position the piston is 1 5.
• the electronic control device can recognize 1 0, which material is being pressed against the heater 1 6 and is evaporated by the heater 1 6. Accordingly, the elec- Ronic control device adapted to the type of material feed rate of the piston 1 5 and an adjusted heating temperature of the heater 1 6 adjust. For this purpose, the electronic control device 1 0 control signals to the heater 1 6 to set the heating temperature, as indicated by the arrow from the electronic control device 1 0 to the heater 1 6.
• the vaporized in the heater 1 6 materials are transported through the tube 1 7 to m material discharge head 1 8 and evenly distributed by this in the interior of the space I 8, as shown by the dotted arrows.
• the substrate 8 may have a vacuum for this purpose. In this way, the inner surface of the substrate 8 is coated with the materials 1, 2, 3, 4, 5, 6, 7 in the order named, i. H . the material 1 is first deposited on the substrate, the material 7 last.
• a plurality of material supply cylinders 1 2 with respective storage chambers 1 3 and motor drives 1 1 can also be provided in the multi-material delivery device 1 9, which then either to different material delivery heads or one and the same Material dispensing head 1 8 delivered the evaporated materials.
• a separate pantry can be provided.
• a heating of the pipe 1 7 can be provided.
• the material discharge head 1 8 may have an integrated heater. As a result, unwanted premature deposition of the materials to be dispensed can be avoided and an advantageous protection of the materials can be achieved.
• the invention is not limited to the example of the internal coating described above. tion of substantially closed hollow bodies, such as the spherical shape of the substrate 8, limited. Rather, other substrates can be coated, such. B. substrates in tubular form. It is possible with the invention, for example, to realize OLED bulbs in a classic "fluorescent tube" shape, the tubes to be coated from the inside being coated with glass or other transparent materials then being coated via a material delivery head inserted into the tube, for example the die
• the circular cylinder may, for example, extend over the entire length of the tube to be coated, Other types of material dispensing heads for the internal coating of such tubes, which are moved slowly longitudinally through the tube during the coating process, are also conceivable.
• FIG. 2 shows the coating with the material layers 21, 22, 23, 24, 25, 26, 27 produced by the multi-material delivery device 19 of FIG. 1 on the inside of the substrate 8.
• an electrode is formed by respective outer layers 21, 27 made of organic light emitting diode.
• the layer 21 is z. B. formed from ITO. It is also possible to use other materials, wherein it is advantageous that a transparent anode of the light-emitting diode is thereby produced.
• a layer 22 z. B. 40 nm thick layer of N PD are deposited.
• As a layer 23, a z. B. 20 nm thick layer of CBP: lr (ppy) 3 are deposited.
• a fourth layer 24 for example, 1 0 nm thick BCP layer can be deposited.
• an eg 20 nm thick layer of Alq 3 can be deposited.
• a layer 26 of Li F can be deposited, the z. B. 0.5 nm thick.
• a layer 27 of aluminum is deposited as the cathode layer, for. B. with a thickness of 200 nm.
• OLED organic light emitting diode

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• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Electroluminescent Light Sources (AREA)

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• 2012
  • 2012-08-24 DE DE102012107824.6A patent/DE102012107824B3/de not_active Expired - Fee Related
• 2013
  • 2013-08-22 WO PCT/EP2013/067465 patent/WO2014029845A1/fr not_active Ceased

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