EP3119928B1 - Procédé d'enlèvement de couches en matériau céramique dur de substrats en acier et en métal dur - Google Patents

Procédé d'enlèvement de couches en matériau céramique dur de substrats en acier et en métal dur Download PDF

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Publication number
EP3119928B1
EP3119928B1 EP14711234.6A EP14711234A EP3119928B1 EP 3119928 B1 EP3119928 B1 EP 3119928B1 EP 14711234 A EP14711234 A EP 14711234A EP 3119928 B1 EP3119928 B1 EP 3119928B1
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European Patent Office
Prior art keywords
holder
layer
workpieces
tools
hard material
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EP14711234.6A
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German (de)
English (en)
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EP3119928A1 (fr
Inventor
Birgit Wittel
Gunnar LAHTZ
Christian BÜCHEL
Jan Prochazka
Andreas Lümkemann
Peter WÄLCHLI
Tibor Cselle
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PLATIT AG
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PLATIT AG
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00—Electrolytic stripping of metallic layers or coatings
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/06—Etching of iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating

Definitions

  • the invention relates to a method for stripping ceramic hard coatings of steel and hard metal substrates, namely of steel and hard metal substrates, which have a ceramic hard material layer on a part of their surface. Furthermore, the invention relates to the method suitable mounts.
  • Carbide tools are used in the tool industry, among other things, and usually consist of tungsten carbide grains and cobalt as a matrix. In order to achieve an improvement in the surface properties, these tools, depending on the application with a hard material layer, such. As titanium nitride or chromium nitride, coated by vacuum coating method. Hard coatings, depending on the application of the tool, may exist as a single layer or as a multilayer, and include at least one of the chemical elements Al, Ti, Cr, Si, which may be oxides, nitrides, carbides or mixed compounds, e.g. Carbonitrides acts. These hard coatings are also called ceramic layers.
  • Decoating the hard material layer becomes necessary if the tool is to be reused after use and regrinding, or if a defective coating has to be removed from the tool.
  • the difficulty with the stripping consists on the one hand in the different applied materials which are used in a hard material layer or whether multilayers or single layers are present and on the other hand in the chemical instability of the cemented carbide per se.
  • Tools made of high-speed steel are coated with the same hard-coat materials as carbide tools. They are however in the production cheaper and easier to decoat as hard metal tools due to their chemical resistance.
  • the stripping processes are subdivided into groups of different layers of hard material, a first group comprising Ti and Al based on carbide tools and high speed steel tools, e.g. As TiN, TiCN, TiAIN, AlTiN, TiAlN / SiN, present as a monoblock layer, gradient layer or multilayer coating.
  • a decoating method which is based on the wet-chemical removal of hard material layers using complexly composed hydrogen peroxide solutions is customary here, wherein typically the hard metal tool is protected by the application of a protective voltage.
  • the decoating time is based on a 2 micron thick, monoblock hard material layer between 4 - 24 h and is thus very long.
  • the consumption of chemicals that need to be constantly renewed at these very long stripping times very high.
  • complex layer systems such as AITiCrN this method fails. A stripping is no longer possible.
  • wet-chemical removal of hard coatings is also performed using complex-composed hydrogen peroxide solutions, but without application of protective stress on the tool, but at elevated temperature.
  • the decoating time is based on a 2 micron thick, monoblock hard material layer between 1-4 h.
  • a second group comprises Cr-based coatings on cemented carbide tools and high speed steel tools, e.g. B. CrN, AlCrN.
  • a decoating method for both types of tools is customary here, which is based on the wet-chemical use of a mixture of permanganate solution and alkali. The consumption of chemicals here is low and the stripping times of a 2 micron thick layer of hard material, which is 1 hour, is relatively short.
  • a third group includes CrTi based coatings on cemented carbide tools and high speed steel tools, e.g. CrTiN, AlTiCrN.
  • high speed steel tools e.g. CrTiN, AlTiCrN.
  • the stripping of high-speed steel tools is based on an electrochemical process, which as electrolytes has a complex composition of basic peroxide solution.
  • the chemicals are quickly consumed during stripping and thus the effort is very high.
  • the process fails here.
  • a method for stripping carbide tools is from WO 99/54528 A1 known, which allows the breaking off of a hard material layer of the hard metal tool.
  • a tungsten oxide layer is electrolytically formed on the hard metal tool, which then has to be removed in a mechanical aftertreatment. This process is very fast, as it promises stripping times of the first and second groups under 30 min.
  • the disadvantage here is the need for a mechanical aftertreatment of the tungsten oxide layer formed.
  • a method which removes surface areas by means of pulsed current from components.
  • a turbine blade is specified by way of example, which consists of a nickel-cobalt superalloy.
  • the layer to be removed is metallic, in particular of the composition MCrAIY, where M stands for an element from the group consisting of iron, cobalt or nickel.
  • M stands for an element from the group consisting of iron, cobalt or nickel.
  • the object of the present invention is to propose a process for stripping which removes hard material layers of the first group more quickly and easily from cemented carbide tools but nonetheless removes layers of hard material of the second group of cemented carbide and high speed steel tools, and third group stratum materials, which can not yet be removed chemically, or only partially, can decoat quickly and easily on carbide and high-speed steel tools.
  • the object of the invention is achieved by a method according to claim 1.
  • the measures of the invention initially have the consequence that for ceramic-coated hard metal workpieces and for workpieces with a ceramic hard material layer, a method is provided which removes the ceramic layer up to an adhesive layer or up to the hard metal layer.
  • the workpiece in particular in the area in which there is no ceramic layer, is spared from chemical attack.
  • this becomes very thin adhesion-promoting layer removed, namely - as is well known and customary - with peroxide solutions under protective voltage on the tool.
  • the process according to the present invention will lead to rapid stripping times, but the hard metal will be attacked here and has to be aftertreated by mechanical methods, such as regrinding, polishing or microblasting.
  • the method according to the present invention is intended for ceramic hard coatings of the second and third groups. If an adhesion-promoting layer of TiN is present, it is stripped to this with the new process and removed in a second step with conventional methods, this very thin primer layer. This is done with peroxide solutions at elevated temperature. If there is no bonding layer of TiN, the process is completely stripped. However, in a further step, it is advisable to use a peroxidic stripping bath customary in the prior art under elevated temperature in order to remove discolorations which may arise during use of the novel process.
  • the end point detection is carried out by measuring or determining the voltage required to reach a certain current, after observing a drop in the voltage, the voltage returns to its original value.
  • the workpieces are placed in a holder which is designed to accommodate workpieces of different diameters, to contact them and at the same time to protect the uncoated material surfaces against attack, in order to then dispose them in a pulsed process ,
  • the voltage source is a current of 10 A to 50 A, preferably 20 A to 40 A and most preferably 26 A to 35 A, current-controlled pulsed, preferably unipolar and most preferably unipolar with a rectangular pulse shape with a Frequency of 1 Hz to 40 Hz, preferably 2 Hz to 20 Hz and most preferably 3 Hz to 8 Hz and a duty cycle (duty cycle) of greater than 25%, preferably greater than 50% and most preferably greater than 75%.
  • a current of 10 A to 50 A preferably 20 A to 40 A and most preferably 26 A to 35 A
  • current-controlled pulsed preferably unipolar and most preferably unipolar with a rectangular pulse shape with a Frequency of 1 Hz to 40 Hz, preferably 2 Hz to 20 Hz and most preferably 3 Hz to 8 Hz and a duty cycle (duty cycle) of greater than 25%, preferably greater than 50% and most preferably greater than 75%.
  • a basic electrolyte when the voltage source is a current of 50 A to 200 A, preferably 80 A to 150 A and most preferably 90 A to 115 A, current-controlled pulsed, preferably unipolar and most preferably unipolar with a rectangular pulse shape with a frequency of 5 Hz to 40 Hz, preferably 10 Hz to 35 Hz and most preferably 20 Hz to 30 Hz and a duty cycle (duty cycle) of less than 50%, preferably less than 35% and most preferably less than 25%.
  • An advantageous holder for carrying out the method for a plurality of workpieces has a conductive base housing with electrical contact and at least one power supply, a lid with bore openings and seals for different plugs, which are preferably in turn provided with holes of different diameters.
  • the holder, the base housing and the cover and the power supply rails are coated with an electrically insulating layer, the insulator material is resistant to chemicals and not applied to the contact surfaces, the plug, which are provided with holes of different diameters to different To be able to accommodate diameters of workpieces, made of electrically non-conductive materials that are resistant to chemicals, preferably made of polyoxymethylene.
  • the plugs may be equipped with O-rings to prevent the ingress of chemicals between the workpiece and the plug.
  • An advantageous holder for carrying out the method for workpieces which have uncoated surfaces on several subregions, in particular hobs comprises an insulating base plate into which a steel receptacle with electrical contacts and power supply is inserted and serves as an anode and at the same time protects the male workpiece against chemical attack and preferably the workpiece holds upright.
  • a conductive cylinder which is provided as a cathode and which via electrical contacts can be contacted, a plastic plug 60 which protects the workpiece elsewhere from chemical attack.
  • the cylinder, the plastic receptacle and the steel receptacle can be exchangeable designed to cover the different sizes and shapes of workpieces and can contact.
  • Hard material layers of the first group and of the third group may have a TiN adhesion-promoting layer with a layer thickness of ⁇ 0.5 ⁇ m between the tool and the actual hard material layer as a result of the layer structure. It forms a transition phase to the actual functional hard material layer.
  • hard material layers of the second and third group can be stripped in a suitable wet chemical approach by means of electrical pulses targeted to either the TiN adhesion layer or in the absence of such to the surface of the high speed steel tool within a short time.
  • Hard material layers of the first group can not be stripped by this method on high speed steel tools because the wet chemical approach used here destroys the high speed steel substrate.
  • the coated tool serves as a positive pole (electrical anode), steel sheets or steel rings or other metallic objects as a negative pole (electric cathode).
  • the electrolyte used depends on the ceramic constituents in the hard material layer.
  • both electrolytes are operated at room temperature.
  • a uniformly positive current-pulsed signal is now induced until the descaling has occurred.
  • the decoating time is 2 microns thick hard material layer between 10 sec and 5 min., Depending on the hard material layer, electrolyte used and tool material used.
  • the applied current per tool is dependent on the coated surface, thus also on the diameter and geometry of the tool, on the type of ceramic coating and thus also on the electrolyte and can be determined specifically by means of experiments.
  • the applied current at the same Carbide shank tool as described above, but coated with a layer type of the first G group, but which is stripped with the acidic electrolyte is 3 A. If several tools clamped in the holder, the tools behave like resistors in a parallel circuit.
  • the frequency of the pulse and its functional form are also critical parameters in this type of stripping. It is pulsed current controlled, preferably with a uniform geometry and most preferably with a rectangular bipolar pulse shape.
  • the frequency of the pulse is basic Electrolytes at 5 Hz to 40 Hz, preferably 10 Hz to 35 Hz and most preferably 20 Hz to 30 Hz and a duty cycle (duty cycle) of less than 50%, preferably less than 35% and most preferably less than 25%.
  • the frequency is 1 Hz to 40 Hz, preferably 2 Hz to 20 Hz and most preferably 3 Hz to 8 Hz and a duty cycle (duty cycle) of greater than 50%, preferably greater than 70% and most preferably greater than 85%.
  • TiN adhesive layer is then stripped using a suitable for the base material, so high-speed steel or carbide, wet-chemical process.
  • a suitable for the base material so high-speed steel or carbide, wet-chemical process.
  • the TiN adhesion layer can be removed within 5 - 10 min. An attack of the carbide does not take place in this short time.
  • Uncoated surfaces such as shafts of shank tools
  • a suitable holder with protective plugs for shank tools
  • a holder with protective plug for the pulsed decoating method was specially developed.
  • the holder can also be used for z.
  • other chemical stripping methods where attacks on the cemented carbide can take place can be used.
  • the holder has the function of receiving shank tools with different diameters, thereby contacting them and at the same time protecting the uncoated shaft surfaces from attack and then stripping them in a pulsed process.
  • the holder 50 for shank tools consists of a conductive base housing 52 with electrical contact and at least one power supply element, in the present embodiment, a power supply rail 56, a cover 55 with bore openings and seals for different plugs 54, which are preferably in turn provided with holes of different diameters.
  • Base housing 52 and cover 55 and power supply rails 56 are coated with an insulator, which insulator material must be resistant to chemicals and must not be applied to the contact surfaces.
  • the plugs 54 which are provided with holes of different diameters to accommodate different diameters of shank tools, are made of non-conductive materials which are resistant to chemicals. The plug height varies to cover different high uncoated shaft lengths.
  • the plugs 54 are equipped with O-rings to prevent ingress of chemicals between the stem and plug 54.
  • a contact rail 57 is shown, on which the tool 10 is, and a two-sided contact spring 58, wherein the contact rail 57 serves as a clamping device for the contact spring.
  • a characteristic feature of using the holder in combination with the guide plugs is that after the pulsed stripping and subsequent removal of the TiN adhesion layer, a small ring of undeclared or slightly attacked surface remains on the shaft tool, as there is little overlap between plug and coated skirt surface and / or there is a slight overlap between free shaft surface and electrolyte.
  • a special embodiment of a holder has the function, e.g. To take hobs of different diameters, thereby contacting them while protecting the uncoated surfaces from attack, and then to disband them in a pulsed process.
  • the holder consists of a bottom plate 75, in which an insulating receptacle 74 is introduced and the male workpiece 10 protects against chemical attack and preferably the workpiece 10 holds upright.
  • An electrical contact 76 for the workpiece serves as the anode, a conductive cylinder 72 which is provided as a cathode and which can be contacted via electrical contacts, and an insulating plug 60 which protects the workpiece 10 from chemical attack elsewhere.
  • the cylinder 72, the insulating receptacle 74 and the insulating plug 60 can be exchanged to cover and contact the various sizes and shapes of the workpieces 10.
  • the method for stripping shank tools is described in the exemplary embodiment described here FIG. 1 - made as follows: 1.
  • the to be stripped shank tools 10 are inserted into the appropriate diameter and height protective plug and pressed into the holder 50.
  • the holder with the shank tools 10 to be stripped is contacted with the positive pole of a current pulse generator 40.
  • It has to be decided which electrolytic bath 30 to use namely an acidic electrolyte for layers of the first group and a basic electrolyte for layers of the second and third group.
  • the contacted holder 50 is placed in the selected electrolyte bath 30.
  • Two steel electrodes 20 are placed on both sides of the bracket and contacted with the negative pole of the current pulser.
  • the distance between the steel electrodes and the shaft tool is 0.5 cm to max. 2.5 cm. 6.
  • the conditions are set for shank tools (with diameter 6 mm to 12 mm). It is assumed that 9 shank tools per stripping.
  • the holders in the embodiment described here are designed for 9 tools.)
  • Shaft tools 10 of the first group use endpoint detection. In tools of the first groups, an effect was surprisingly detected that can serve as an end point detection.
  • the electrical voltage source generates a function of the current over the stripping time, thereby generating a constantly accurate stable current. Since the surface of the tools in the decoating process and thus also the resistance is changed, a decrease in the voltage is observed. When the titanium nitride layer is reached, the resistance increases so much until the voltage has reached its original value.
  • the voltage curve lies in the range of approx. 2-10 V and a voltage difference of approx. 2-4 V is to be expected.
  • the power supply is stopped every 20 to 30 seconds and the holder is checked for stripping with the shank tools. 9.
  • the stripping is finished depending on the composition of the hard material layer at 2 micron layer thickness within 10 sec to 30 min down to the tool or the TiN adhesion layer.
  • TiN adhesive layer is then completely stripped off with a conventional wet chemical approach. Decoating without TiN adhesion layer requires the same pulsed decoating time. A further chemical stripping is not necessary, but there is a mechanical aftertreatment because of the attack of the substrate.
  • FIG. 5 A somewhat different sequence is provided in one embodiment for stripping of hobs, shown in FIG. 5 : 1. To be stripped Hob 10 is contacted with the positive pole of a current pulse generator 30 and in the holder according to FIG. 6 and 7 placed and provided with a protective plug 60 .. 2. It has to be decided which electrolytic bath 30 to use, namely an acidic electrolyte for layers of the first group and a basic electrolyte for layers of the second and third group. 3. The contacted hob 10 is placed in the selected electrolyte bath 30. At a distance of 0.5 cm to max. 2.5 cm, a stainless steel ring-steel electrode, which has been gilded, is placed around the hob. This steel electrode is connected to the negative pole of the pulse generator 30.
  • Layers of the 1st group Layers of the 2nd and 3rd group: 1st example: 1st example: Hob with diameter 47 mm; Height 1510 mm Hob with diameter 47 mm; Height 1510 mm Electricity: 30 A Electricity: 30 A Voltage (U 0max ): 40 V current- controlled , pulse shape rectangular Voltage (U 0max ): 50 V Current-controlled , pulse shape rectangular Frequency 5 Hz Frequency 25 Hz Svmmetry / duty cycle: 98% Symmetry / duty cycle: 20% 2nd example: 2nd example: Hob with diameter 33 mm; Height 110 mm Hob with diameter 33 mm; Height 110 mm Electricity: 30 A Electricity: 30 A Voltage (U 0max ): 40 V current- controlled , pulse shape rectangular Voltage (U 0max ): 50 V Current-controlled , pulse shape rectangular Frequency 5 Hz Frequency 25 Hz Svmmetry / duty cycle: 98% Symmetry / duty cycle: 20% 2nd
  • the stripping begins instantly. 6. Every 20 to 30 sec., The power supply is stopped and the holder 50 is controlled with the milling cutter 10 on stripping. 7. The stripping is finished depending on the composition of the hard material layer at 2 micron layer thickness within 1 min to 10 min to the TiN adhesion layer.
  • TiN adhesive layer is then completely stripped off with a conventional wet chemical approach. Decoating without TiN adhesion layer requires the same pulsed decoating time. Another chemical stripping is not necessary, but a mechanical aftertreatment because of the attack of the substrate.
  • the TiN adhesion layer in a peroxidic Ent fürungsbad under the influence of protective voltage on the shank tools is complete stripped.
  • the stripping time here is about 5 to 10 minutes. In the scanning electron microscope, no attacks on the tools after decoating were found.
  • a cemented carbide hob (d 470 mm) with a 7.2 ⁇ m thick AITiN layer (layer-type table: layer # 6), a coloring cover layer consisting of Al, Ti, N and an existing TiN adhesion-promoting layer was used in a 12% nitric acid solution Electrolyte immersed, stripped at a pulsed current I function of 30 A with a frequency of 5Hz, a duty cycle of 98% to the adhesive layer layer TiN. The ring-steel electrode had a distance of 1.5 cm from the carbide tool. The stripping time was 3 min.
  • the TiN adhesion layer is completely stripped off in a peroxidic de-coating bath under the action of protective voltage on the shank tools.
  • the stripping time here is about 5 to 10 minutes. In the scanning electron microscope, no attacks on the tools after decoating were found.
  • the ring-steel electrode had a distance of 1.5 cm from the carbide tool.
  • the stripping time was 2 min.
  • the ring steel electrode had a clearance of 1.0 cm from the high speed steel hob.
  • the stripping time was 11 min.
  • the brownish discoloration that resulted from the pulsed stripping is removed in a peroxidic stripping bath at elevated temperature. The stay in the bath is about 5 minutes.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Claims (5)

  1. Procédé permettant d'enlever des couches en matériau céramique dur sur au moins une pièce (10) qui comporte sur une partie de sa surface une couche en matériau céramique dur, selon lequel :
    au moins une électrode (20) est positionnée en tant que cathode dans un liquide électrolytique (30),
    la pièce (10) est également positionnée au moins partiellement, dans le liquide électrolytique (30) en tant qu'anode,
    un moyen générateur d'impulsions (40) permettant de produire des impulsions de tension est monté entre la cathode et l'anode, et
    des éléments de protection sont prévus,
    ce procédé comprenant des étapes selon lesquelles :
    les pièces (10) sur lesquelles des couches doivent être enlevées sont enfichées dans les éléments de protection ayant un diamètre et une hauteur adaptés et sont insérées dans un support (50), ce support étant mis avec les pièces (10) sur lesquelles des couches doivent être enlevées en contact avec le pôle positif du moyen générateur d'impulsions (40),
    on choisit un bain électrolytique acide, on place le support (50) mis en contact dans le bain électrolytique choisi, on positionne au moins une électrode (20) à une distance prédéfinie du support (50), et on la met en contact avec le pôle négatif du moyen générateur d'impulsions (40),
    on effectue l'enlèvement de couches à l'aide du moyen générateur d'impulsions (40), on effectue en continu une identification du point final ou on effectue un contrôle de l'enlèvement de couches à intervalles dans le temps, l'identification du point final étant effectuée par mesure ou détermination de la tension qui est nécessaire pour atteindre un courant défini, après observation d'une baisse de tension, la tension ayant à nouveau atteint sa valeur initiale,
    caractérisé en ce qu'
    en tant qu'électrolytique on utilise des acides minéraux à 2 à 50 % à un pH de 0,5 à -1,1.
  2. Procédé conforme à la revendication 1,
    caractérisé en ce que
    les pièces (10) sont enfichées dans un support (50) pour les mettre en contact et simultanément protéger les surfaces de matériau non recouvertes contre l'attaque pour effectuer ensuite l'enlèvement des couches.
  3. Procédé conforme à l'une des revendications 1 ou 2,
    caractérisé en ce que
    la source de tension est réalisée de façon à fournir un courant de 10 A à 50 A pour une tension (U0Max) de 20 V à 60 V pulsée par commande de courant avec une fréquence de 1 Hz à 40 Hz et une durée de cycle supérieure à 25%.
  4. Procédé conforme à l'une des revendications 1 à 3,
    caractérisé en ce que
    l'on utilise en tant que support pour des pièces (10) qui comportent dans plusieurs zones partielles des surfaces non recouvertes, en particulier des fraises cylindriques, un support ayant une plaque de base (75) dans laquelle un logement de réception isolant protège la pièce à recevoir contre une attaque chimique, un contact électrique (76) pour l'alimentation en courant, constituant l'anode, un cylindre conducteur (72) qui est prévu en tant que cathode, et qui peut être mis en contact par l'intermédiaire de contacts électriques, de préférence un rail conducteur (56), et un tampon isolant (60) qui protège la pièce (10) contre une attaque chimique à d'autres endroits.
  5. Procédé conforme à la revendication 4,
    caractérisé en ce que
    l'on utilise un support dans lequel le cylindre (72) les logements de réception isolants et les tampons isolants (60) sont interchangeables pour pouvoir recouvrir et mettre en contact des pièces (10) ayant des dimensions et des formes différentes.
EP14711234.6A 2014-03-18 2014-03-18 Procédé d'enlèvement de couches en matériau céramique dur de substrats en acier et en métal dur Active EP3119928B1 (fr)

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PCT/EP2014/055376 WO2015139731A1 (fr) 2014-03-18 2014-03-18 Procédé d'enlèvement de couches en matériau céramique dur de substrats en acier et en métal dur

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EP3119928B1 true EP3119928B1 (fr) 2018-08-22

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US (1) US9879356B2 (fr)
EP (1) EP3119928B1 (fr)
JP (1) JP6440814B2 (fr)
KR (1) KR20170004970A (fr)
WO (1) WO2015139731A1 (fr)

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KR20170004970A (ko) 2017-01-11
US20170204530A1 (en) 2017-07-20
US9879356B2 (en) 2018-01-30
EP3119928A1 (fr) 2017-01-25
WO2015139731A1 (fr) 2015-09-24
JP6440814B2 (ja) 2018-12-19
JP2017508893A (ja) 2017-03-30

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