EP3140644A1 - Thermographie pour l'assurance qualité dans un procédé de fabrication génératif - Google Patents

Thermographie pour l'assurance qualité dans un procédé de fabrication génératif

Info

Publication number
EP3140644A1
EP3140644A1 EP15747744.9A EP15747744A EP3140644A1 EP 3140644 A1 EP3140644 A1 EP 3140644A1 EP 15747744 A EP15747744 A EP 15747744A EP 3140644 A1 EP3140644 A1 EP 3140644A1
Authority
EP
European Patent Office
Prior art keywords
component
recording
layer
images
heat distribution
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP15747744.9A
Other languages
German (de)
English (en)
Inventor
Alexander Ladewig
Georg SCHLICK
Günter Zenzinger
Joachim Bamberg
Thomas Hess
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MTU Aero Engines AG
Original Assignee
MTU Aero Engines AG
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 MTU Aero Engines AG filed Critical MTU Aero Engines AG
Publication of EP3140644A1 publication Critical patent/EP3140644A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/03—Observing, e.g. monitoring, the workpiece
    • B23K26/034—Observing the temperature of the workpiece
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/34—Laser welding for purposes other than joining
    • B23K26/342—Build-up welding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/72—Investigating presence of flaws
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J2005/0077—Imaging
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/48—Thermography; Techniques using wholly visual means

Definitions

  • the invention relates to a method for quality assurance of at least one component during its production according to the preamble of patent claim 1 and to an apparatus for carrying out the method according to the preamble of patent claim 11.
  • Laser thermography methods are known from the prior art which are used as non-destructive test methods (ZFP method ) are used to detect cracks in components.
  • ZFP method non-destructive test methods
  • the cooling of the surface of the component to be tested is detected with a laser thermography camera.
  • Due to the high energy of the laser there is a considerable heating of the surface of the component to be tested.
  • the manufacturing process must be interrupted in a generative manufacturing process.
  • a second energy source is required.
  • the invention is therefore based on the object to provide a method which, in a generative manufacturing process, a non-destructive testing of a metallic
  • the solution of the problem in a method for quality assurance of at least one component during its production, wherein the production is carried out by means of at least generative manufacturing process with at least one processing laser the following
  • Steps includes:
  • thermographic recording of at least one image of at least one component region on the laser beam by means of at least one recording sensor thermographic recording of at least one image of at least one component region on the laser beam by means of at least one recording sensor.
  • a photograph of a plurality of images is taken in a defined period of time, which detects a temporal change of heat distribution in a molten bath-free component area, upon occurrence of at least one defect such as a crack, a foreign matter, a pore, a bonding defect and the like in the uppermost component layer or including the component region has a characteristic temporal change of a heat distribution at the fault, the temporal course of the heat distribution and thus the error is made visible by means of the associated recording of the plurality of images.
  • a characteristic heat distribution on the defect is understood to be a temporal change of a heat distribution which arises in particular due to a material interruption at the defect.
  • the method according to the invention makes it possible to check during production the respectively last produced layer and some underlying layers of a component during the additive production. This results in a test in the form of an on-line method by means of which the entire component can be examined for defects during production or production and can be completely documented. Preferably, images are taken in each individual layer. With the method according to the invention, it is thus possible to carry out a test for defects such as cracks, foreign materials, pores, binding defects and the like with the aid of an on-line method without significant additional expenditure. Internal defects can be detected non-destructively, so that an aerospace permit of the component is possible without subsequent tests.
  • thermographic recording by means of the recording sensor in particular a photodiode array, and an optical scanning device detects the heat distribution through the laser beam.
  • the size of the recording sensor can be significantly smaller than the size of the recording sensors of thermographic devices according to the prior art, because the receiving area of the recording sensor is always directed by means of the optical scanning device on the currently under investigation construction area and not on the entire device layer.
  • the recorded component area may be closer to the laser beam.
  • thermographic image is taken after the construction of a component layer, wherein the processing laser sweeps the built-up component layer line by line and thereby increases the surface temperature of the component just so slightly that an influence on the heat distribution of the component layer is avoided. This makes it possible to check a complete component layer.
  • the pickup sensor is selected to be as small as possible, so that just a defined component area, which lies behind an incident surface of the laser beam with respect to the direction of movement of the laser beam, is detected.
  • a recording sensor as small as possible allows a high resolution rate and recording speed and thus a high accuracy of when taking pictures.
  • thermographic image is taken during the construction of a component layer, wherein the processing laser generates a local melt pool.
  • the component layer can still be examined during the construction.
  • the pick-up sensor is selected to be as small as possible, so that just a defined component region, which lies behind the molten bath in relation to the direction of movement of the laser beam and is already hardening or has already hardened, is detected.
  • the smallest possible photodiode array allows a high resolution rate or recording speed and thus a high accuracy when taking pictures.
  • At least some of the applied layers are subjected to a controlled heat treatment below the melting temperature of the component material before the thermographic image of the associated images, wherein the heat treatment emanates a thermal radiation emanating from the last applied layer, in particular in the infrared region at the edge of the visible spectrum and in the infrared spectrum Detection spectrum of the pickup sensor, which has a characteristic temporal heat distribution at the fault when at least one of a defect such as a crack, a foreign matter, a pore, a bonding defect and the like occurs in the film, this heat distribution and hence the error is made visible by means of the associated thermographic recording of the plurality of images.
  • a controlled heat treatment below the melting temperature of the component material before the thermographic image of the associated images
  • the additive manufacturing process may be a selective laser melting and / or a selective laser sintering. These methods are particularly well suited for the additive production of metallic components.
  • the error is corrected by reflowing the faulty location or the component layer.
  • the quality of the layer is not only tested, but also secured or guaranteed.
  • the images taken by the thermography device can be analyzed and, upon detection of the error, a signaling device activated and / or a re-melting of the faulty point or component layer triggered.
  • a signaling device activated and / or a re-melting of the faulty point or component layer triggered.
  • These method steps can be purely manual, fully automatic or partially automatic or partially manual.
  • Activating the signaling device may alert an operator when an error is detected. The operator can then interrupt the generative production of the component and set the processing laser for the generative manufacturing process so that the faulty site or component layer is remelted. Alternatively, the remelting of the faulty point or component layer can be triggered automatically. In addition, an alarm signal can be generated.
  • thermography device also comprises at least one optical scanning device, wherein the recording sensor has an adapted recording speed, by means of which a plurality of images in a defined period can be recorded and thus a temporal change of heat distribution in a defined melter bath-free component area can be displayed.
  • the size of the recording sensor can be significantly smaller than the size of the recording sensors of thermography devices according to the prior art, because according to the invention, the recording area of the recording sensor is always directed by means of the optical scanning device on the currently examined component area and not on the entire device layer.
  • the recording sensor comprises a photodiode array which has the smallest possible dimensions. Small dimensions allow high recording speeds. In a further specific embodiment, the recording speed of the recording sensor is at least 1000 fps. High sampling rates or recording speeds allow for high accuracy in image acquisition.
  • the processing laser of the generative manufacturing device can simultaneously be the source of energy for the controlled heat treatment.
  • the processing laser of the generative manufacturing device can simultaneously be the source of energy for the controlled heat treatment.
  • the processing laser of the generative manufacturing device can simultaneously be the source of energy for the controlled heat treatment.
  • the processing laser of the generative manufacturing device can simultaneously be the source of energy for the controlled heat treatment.
  • the device comprises at least one display device, at least one evaluation device, at least one signaling device for reporting an error such as a crack, a foreign material, a pore, a binding error and the like and at least one control of the processing laser of the generative manufacturing device.
  • the evaluation device is used for data processing.
  • the signaling device may alert an operator when an error is detected. The operator can then interrupt the generative production of the component and the processing laser for the generative Control manufacturing processes so that the faulty site or component layer is remelted. Alternatively, the remelting of the faulty point or component layer can be triggered automatically by the evaluation device by means of the control of the processing laser for the generative production method.
  • the signaling device can be activated.
  • FIG. 1 is a perspective view of a detail of a device according to the invention
  • FIG. 2 is a schematic side view of the device according to the invention according to FIG. 1
  • FIG. 3 is a perspective enlargement of a section of a component region
  • FIG. 4 is a schematic diagram of the device according to the invention.
  • FIG. 1 shows a perspective view of a section of a device 10 according to the invention, which comprises a generative production device 12 for producing a component 14.
  • Fig. 1 will be explained below in conjunction with Fig. 2, in which a schematic side view of the device 10 according to the invention shown in FIG. 1 is shown.
  • the device 10 serves to carry out a method for quality assurance of a component 14 during its manufacture.
  • the generative manufacturing device 12 itself is presently designed as a per se known selective laser melting system (SLM), i. a laser or processing laser 22 is the energy source for the melting process.
  • SLM selective laser melting system
  • the laser is directed downwards, so that the component 14 can be produced from the bottom to the top in layers to be applied one above the other.
  • thermography device 18 is arranged outside a construction space 16 (FIG. 2) of the generative production device 12 and serves to detect a temporal change in the heat history in the uppermost layer of the component 14 during its production.
  • the thermography Device 18 is directed to the respectively uppermost layer of component 14, wherein the detection angle of thermography device 18 only covers component region 17.
  • the thermography device is arranged in a vertical plane, which in this case corresponds to the image plane in FIG. 2, between the laser 22 and the outer boundaries of the installation space 16. As a result, an optical distortion, which could arise in the case of an excessively inclined thermography device 18, is avoided.
  • the thermography device 18 can take pictures due to this arrangement through the laser beam.
  • thermography device 18 Between the packaging space 16 ( Figure 2) and the thermography device 18, a laser protection glass 20 ( Figure 1) is arranged to prevent damage to a pick-up sensor or photodiode array of the thermography device 18, e.g. a camera, by the laser 22 of the generative manufacturing device 12 to prevent.
  • the thermography device 18 is thus located above the construction space 16 and outside the beam path II of the laser 22 of the generative manufacturing device 12. This ensures that the thermography device 18 is not located in the beam path II and that the laser 22 accordingly no energy loss through optical elements such as semi-transparent Mirror, grid or the like suffers. Furthermore, the thermography device 18 does not affect the manufacturing process of the component 14 and is also easily replaceable or retrofittable.
  • thermography device 18 comprises an IR-sensitive photodiode array having a recording speed of preferably at least 1000 fps.
  • a color sensor or a sensor with a broad spectral range provides comparatively more information, which permits a correspondingly more accurate assessment of the component region 17.
  • a high-temperature-resistant metal alloy is applied in a manner known per se to a platform (not shown) of the generative production device 12, locally melted by means of the laser 22 and solidified by cooling. Subsequently, the platform is lowered, applied a further powder layer and solidified again. This cycle is repeated until the component 14 is manufactured.
  • An exemplary component 14 consists of up to 2000 component layers and has a Total layer height of 40 mm. The finished component 14 can then be further processed or used immediately.
  • the respectively uppermost layer of the component 14 can be subjected to a heat treatment below the melting temperature of the component material.
  • This heat treatment causes thermal radiation emanating from the uppermost layer, which can be detected by means of a thermography device 18.
  • the heat radiation of the burst layer is adjusted so that it lies in the infrared region at the edge of the visible spectrum and also in the sensitivity range of the thermography device 18.
  • each applied layer is subjected to a heat treatment.
  • a subsequent heat treatment is eliminated. Instead, for error checking, the component area 17 with respect to the direction of movement of the laser (II in FIG. 2) is received behind a molten bath.
  • the temporal change of the heat profile in the uppermost layer of the component region 17 is determined with the aid of the thermography device 18 in the form of an image sequence.
  • the temporal change of the heat history in the uppermost layer of the component 14 and optionally further information derived therefrom, such as e.g. the finding of errors in the uppermost layer or below, are then spatially resolved and visualized, for example, via brightness values and / or colors by means of a display device 32 (FIG. 4).
  • thermography device 18 has neither during the generative production, nor during the examination of the
  • Component 14 an influence on the heat history in the component 14th
  • the optical thermography not only provides geometric information, but also information about the local temperature distribution and the temporal change of the heat flow in the relevant component region 17.
  • the distance traveled by the laser beam per individual image is between 10 mm and 120 mm, for example 10 mm, 20 mm, 30 mm, 40 mm, 50 mm, 60 mm, 70 mm, 80 mm, 90 mm, 100 mm, 110 mm or 120 mm.
  • each image sequence or a plurality of images is determined within 2 minutes in order to avoid excessive cooling of the component layers and a concomitant loss of information.
  • the component 14 may have an error in its uppermost layer, which may be a crack by way of example. Other possible defects are pores, foreign materials, binding defects and the like.
  • the crack may be a hot crack or a segmentation crack. 3 shows an enlargement of a section from the component area 17. By way of example, three layers 26, 28 of the component 14 are shown here. However, the component 14 may also include more or fewer layers 26 depending on the current manufacturing state. The two layers 26 shown here are flawless or crack-free layers whose crack-free state could be determined with the aid of the thermography device 18, so that the production process was continued.
  • the uppermost layer of the component 14 is a cracked layer 28.
  • the course and the shape of the crack 30 are shown here only schematically. In the layer 28, more than one crack 30 may occur.
  • the crack can take any random form.
  • the length and width of the crack 30 may vary and be in the range of a few microns. These small dimensions can only be detected by means of the thermography device 18.
  • cracks 30 of this order of magnitude can only be detected by the corresponding recording of the image sequence or a plurality of images described above for representing the temporal change of the heat distribution. It can also cracks in some layers below the uppermost layer 28 are determined. They are
  • the generative production can be continued. However, when the limits are reached or exceeded, the manufacturing process for the corresponding component 14 becomes premature terminated or the cracked layer 28 of the component 14 is corrected by a re-melting.
  • each component region is optically detected in the same way as the component region 17 with the aid of the thermography device 18 and displayed on the display device 32.
  • the thermography device is in operative connection with at least one evaluation device 34, so that the recorded images can be sorted and stored there and, if necessary, a command for interrupting the generative production process of the cracked component 14 can be triggered.
  • the evaluation device 34 is configured such that it can detect the crack 30 in the uppermost layer 28 of the component 14 with the aid of an algorithm. However, these processes can also be performed manually after evaluation of the images or images of the thermography device 18 on the display device 32 by an operator.
  • the generative production process can be interrupted and the cracked point or the entire layer 28 corrected by reflowing.
  • the remelting of the cracked layer 28 takes place, for example, in that the evaluation device 34 upon automatic detection of a crack 30 of the control 38 of the laser 22 gives a corresponding command for interrupting the generative production process and for reflowing.
  • the generative manufacturing process for a cracked component 14 can be terminated prematurely. This is done by a command, which is automatically triggered by the evaluation device 34, to the controller 38 of the laser 22.
  • the premature termination of the generative manufacturing process is preferably carried out when the component 14 has only a small number of layers 26, 28. If the component 14 is already almost finished, it is preferable to break and reflow the defective location or layer 28. Quite generally, the evaluation device 34 can also trigger an alarm in the form of acoustic or optical signals with the aid of a signal device 36, for example in the form of a warning message on the display device 32 or another computing device (not shown) connected to the generative manufacturing device 12. Then it can be decided by an operator whether and how the generative production of the components 14 is continued.
  • the evaluation device 34 and the signal device 36 including the required signal lines between the thermography device 18, the evaluation device, the signal device 36 and the controller 38 of the laser 22 of the generative manufacturing device 12 are components of the device 10th
  • the recording sensor or the photodiode array of the thermography device takes pictures through the beam path of the laser 22 through or measures the temporal change of the heat distribution.
  • the recording sensor used in this case has a small size, since the field of view of the recording sensor is always directed by the scanning optics to the currently examined position. As a result, the recording speed can be at least 1000 fps. As a result, a high measurement accuracy can be achieved.
  • the invention also relates to a method for quality assurance of at least one component (14) during its production, wherein the production by means of at least generative
  • Manufacturing process with at least one processing laser comprising the following steps:
  • a recording of a plurality of images takes place in a defined period of time, which detect a temporal change of a heat distribution in a molten bath-free component area, wherein at least one fault (30) such as a crack (30), a foreign material, a pore, a binding error and the like in the uppermost component layer or below the component area a characteristic temporal change of a fault (30) such as a crack (30), a foreign material, a pore, a binding error and the like in the uppermost component layer or below the component area a characteristic temporal change of a
  • the invention relates to a method for quality assurance of at least one component during its production, wherein the production takes place by means of at least generative production method with at least one processing laser, comprising the following steps:
  • a plurality of images are recorded within a defined period of time Detecting heat distribution in a molten bath-free component region, wherein when at least one defect such as a crack, a foreign material, a pore, a binding defect and the like in the uppermost component layer or below the component region has a characteristic temporal change of heat distribution at the fault, wherein the time course of Heat distribution and thus the error is made visible by means of the associated recording of the plurality of images.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Laser Beam Processing (AREA)
  • Radiation Pyrometers (AREA)

Abstract

L'invention concerne un procédé et un dispositif pour l'assurance qualité d'au moins un élément structural (14) durant sa production. La production est effectuée à l'aide d'au moins un procédé de fabrication génératif au moyen d'au moins un laser d'usinage (22). Le procédé comprend les étapes suivantes : - la réalisation, couche par couche, de l'élément structural (14); - la prise de vue thermographique d'une pluralité d'images d'au moins une zone (17) de l'élément structural au niveau du faisceau laser au moyen au moins d'un capteur de prise de vue, dans un laps de temps défini; - la détection de la variation dans le temps de la diffusion de chaleur dans une zone de l'élément structural exempte de bain de fusion, l'apparition d'au moins un défaut (tel qu'une fissure, un matériau étranger, un pore, un manque de fusion et un défaut similaire), dans la couche supérieure de l'élément structural ou en-dessous de ce dernier étant détectée au moyen d'une variation dans le temps, caractéristique, de la diffusion de chaleur au niveau du défaut (30).
EP15747744.9A 2014-05-09 2015-04-24 Thermographie pour l'assurance qualité dans un procédé de fabrication génératif Withdrawn EP3140644A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014208768.6A DE102014208768B4 (de) 2014-05-09 2014-05-09 Verfahren und Vorrichtung zur Qualitätssicherung
PCT/DE2015/200278 WO2015169309A1 (fr) 2014-05-09 2015-04-24 Thermographie pour l'assurance qualité dans un procédé de fabrication génératif

Publications (1)

Publication Number Publication Date
EP3140644A1 true EP3140644A1 (fr) 2017-03-15

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EP15747744.9A Withdrawn EP3140644A1 (fr) 2014-05-09 2015-04-24 Thermographie pour l'assurance qualité dans un procédé de fabrication génératif

Country Status (4)

Country Link
US (1) US20170066084A1 (fr)
EP (1) EP3140644A1 (fr)
DE (1) DE102014208768B4 (fr)
WO (1) WO2015169309A1 (fr)

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