EP3017888A1 - Thermoforming tool - Google Patents
Thermoforming tool Download PDFInfo
- Publication number
- EP3017888A1 EP3017888A1 EP14197507.8A EP14197507A EP3017888A1 EP 3017888 A1 EP3017888 A1 EP 3017888A1 EP 14197507 A EP14197507 A EP 14197507A EP 3017888 A1 EP3017888 A1 EP 3017888A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tool
- relief
- base body
- raised
- metal
- 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.)
- Granted
Links
- 238000003856 thermoforming Methods 0.000 title 1
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 239000011241 protective layer Substances 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims description 25
- 229910000831 Steel Inorganic materials 0.000 claims description 23
- 239000010959 steel Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005242 forging Methods 0.000 claims description 7
- 238000010285 flame spraying Methods 0.000 claims description 3
- 238000007750 plasma spraying Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000007751 thermal spraying Methods 0.000 claims description 2
- 238000001947 vapour-phase growth Methods 0.000 claims description 2
- 238000010618 wire wrap Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000012447 hatching Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 235000013980 iron oxide Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000669 Chrome steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 239000011364 vaporized material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B25/00—Mandrels for metal tube rolling mills, e.g. mandrels of the types used in the methods covered by group B21B17/00; Accessories or auxiliary means therefor ; Construction of, or alloys for, mandrels or plugs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B19/00—Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work
- B21B19/02—Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work the axes of the rollers being arranged essentially diagonally to the axis of the work, e.g. "cross" tube-rolling ; Diescher mills, Stiefel disc piercers or Stiefel rotary piercers
- B21B19/04—Rolling basic material of solid, i.e. non-hollow, structure; Piercing, e.g. rotary piercing mills
Definitions
- the invention is in the field of manufacturing tubular metal workpieces and relates to forming tools, especially piercing mandrels, forged mandrels and billets with improved stability.
- Seamless steel tubes are generally manufactured in three forming steps on respective rolling mills by hot forming.
- a massive steel block heated to about 1200 ° C. is shaped to form a hollow block by means of an internal tool, the piercing mandrel, on a so-called perforated piercing mill.
- the block is driven by means of inclined rollers on the piercer.
- the hollow block is reduced in a longitudinal rolling process over the inner tool, a rolling rod, in diameter and wall thickness and stretched in the longitudinal direction.
- the rolling stock is converted to the required dimensions in diameter and wall thickness, with no internal tool is usually used.
- the inner tools in the first two forming stages are exposed to high temperatures and high mechanical pressures during production.
- the inner tools are made of heat-resistant steel.
- successive heating of the inner tool is often unavoidable.
- the strength of the tool decreases and the tool can then no longer withstand the mechanical loads.
- the tool deforms and breaks.
- piercing mandrels are provided with natural scale layers. These scale layers inhibit the heat flow from the forming material into the tool and protect the tool against rapid heating and rapid loss of strength. When forming higher alloyed materials, however, the scale layer is quickly removed and thermal protection fails.
- the service life of the tools could be improved if the thickness of the oxide layer could be increased. Then the heat insulation would be better and with abrasive wear the protective layer would remain longer.
- the protective layer which is naturally formed from the base material by conversion into iron oxides, does not have high stability. It is brittle and porous and can therefore easily be destroyed by mechanical and thermal stress. Therefore, these protective layers are limited in their thickness. The limit of the layer is about 0.8 mm. The protective effect of such a layer is therefore limited accordingly. Heat therefore penetrates into the body of the tool and reduces its strength, which then leads to premature failure of the tool. For highly alloyed products, the abrasion is relatively fast, i. after a small length of rolled material for removal of the protective layer.
- the object of the present has therefore been to provide hot forming tools with improved stability, which are free of the disadvantages described above.
- these tools should have a higher strength oxide layer which, moreover, can be applied easily and without material loss.
- a first subject of the invention relates to a hot forming tool consisting of a tool base body with at least partial surface coating, which is obtainable by providing the base body with a raised metallic relief, which is then completely or partially oxidized and converted into a protective layer.
- the hot forming tools of the present invention are preferably a piercer or a forging mandrel, which are typically steel.
- the invention fundamentally also encompasses any other metallic workpiece in which the base body is to be protected against heat flow.
- the term metal is not limited to iron and steel, but also includes other metallic materials including metal-containing composites that are to be subjected to hot working.
- the surface coating according to the invention can be advantageously used.
- the internal tools in the rolling mills with a plurality of rolling mills arranged one behind the other in the second forming stage particular care must be taken to ensure that the friction between the tool and the rolling stock is low. Therefore, the surface layer according to the invention must be ground and polished for this application. Also, an additional layer e.g. be applied from chrome on the protective layer according to the invention.
- the raised relief which is applied to the base body, can be pronounced differently, the alternative embodiments are all in principle suitable to fulfill the task fully.
- the raised relief may simply be a wrapping of the base body with a wire, preferably a steel wire.
- the raised relief may be a metal mesh or metal net applied to the base.
- the metallic bodies applied to the surface of the tool preferably consist of a steel mesh, for example with a steel wire thickness of about 1 to about 5 mm and preferably about 1.5 mm and a mesh size of about 1 to 5 mm and in particular about 2.5 mm.
- Mesh size is the distance between the center lines of two adjacent fabric elements.
- the raised relief may be an irregular coating as achieved by chemical or physical vapor deposition of metal.
- the application of the raised relief can be done according to very different - simple and complex - method, but all solve the task of the invention fully.
- the basic body is simply wrapped with a wire, preferably a metal wire.
- a metal mesh or a metal mesh is used instead of the wire. This can be preformed, for example by deformation to the shape of the tool and then mounted on the body. To increase the strength, it is advisable to weld the wire winding or the metal mesh to the base body.
- chemical vapor deposition refers to a group of coating processes which are used inter alia in the production of microelectronic components and optical waveguides.
- a solid component is deposited due to a chemical reaction from the gas phase.
- volatile compounds of the layer components exist, which deposit the solid layer at a certain reaction temperature.
- the process of chemical vapor deposition is characterized by at least one reaction on the surface of the workpiece to be coated. At least one gaseous starting compound (starting material) and at least two reaction products - at least one of which in the solid phase - must be involved in this reaction.
- starting material At least one gaseous starting compound (starting material) and at least two reaction products - at least one of which in the solid phase - must be involved in this reaction.
- the process is preferably carried out at reduced pressure.
- the preferred PVD converts the feedstock into the gas phase.
- the gaseous material is then passed to the substrate to be coated, where it condenses and forms the target layer.
- Examples include classical evaporation methods, such as thermal evaporation, electron beam evaporation or laser beam evaporation (Pulsed Laser Deposition).
- sputtering is preferred in which the starting material is atomized by ion bombardment and transferred into the gas phase, from which it can then be deposited again onto the base body. All these methods have in common that the material to be deposited in solid form in the most evacuated coating chamber is present.
- the target By bombardment with laser beams, magnetically deflected ions or electrons as well as by arc discharge, the target is vaporized.
- the amount of atoms, ions or larger clusters in the vapor varies from process to process.
- the vaporized material moves either ballistically or by electric fields guided through the chamber and strikes the parts to be coated, where it comes to film formation.
- Typical working pressures are in the range of 10 -4 Pa to about 10 Pa.
- areas that are invisible from the location of the vapor source are coated at a lower coating rate.
- unlike usual is dispensed with a rotation of the substrate.
- a fourth alternative embodiment for the formation of relief comprises the so-called thermal spraying.
- This filler materials, the so-called spray additives inside or outside of a spray burner off, on or melted, accelerated in a gas stream in the form of spray particles and thrown onto the surface of the component to be coated.
- the component surface is not melted (in contrast to build-up welding) and only subjected to a low thermal load.
- a layer formation takes place because the spray particles flatten more or less depending on the process and material when hitting the component surface, stick primarily by mechanical clamping and layer by layer build up the spray layer.
- Quality features of sprayed coatings are low porosity, good adhesion to the component, freedom from cracks and homogeneous microstructure.
- the achieved coating properties are significantly influenced by the temperature and the speed of the spray particles at the time of their impact on the surface to be coated.
- the surface condition purity, activation, temperature
- the surface condition also has a significant influence on quality features such as adhesion.
- the base body can be coated not only with metals but also with oxide-ceramic materials and carbide materials (or in general composite materials).
- the coating is carried out with an iron / ceramic mixture.
- the body is preferably made of steel
- the requirement for the material forming the raised relief is that it be at least partially capable of forming an oxide layer.
- this is iron or steel, so that an iron oxide layer, preferably scale is produced.
- a mixture of iron / steel and ceramics may also be used, for example in a weight ratio of about 20:80 to about 80:20.
- the relief can have a variety of forms, ranging from regular (round, square, etc.) to any free-form.
- Material composites can also be used, i.
- a molybdenum fabric which is applied to the body made of steel.
- the fabric element may also consist of a composite of hard chrome steel (inside) and good oxidizable steel (outside).
- spacers and combustible materials can be used. It is also possible to store ceramic for better thermal insulation.
- the complete or partial conversion of the metallic relief into an oxide protective layer can be carried out by known processes of the prior art, for example by flame spraying, plasma spraying or by a thermochemical process.
- oxide is also formed in the interstices between the bodies, for example, between the tool body and the applied steel mesh and within the mesh of the steel mesh.
- the result is a particularly thick protective layer reinforced by internal bodies.
- the layer thickness is not limited to a few millimeters. Layer thicknesses of 10 millimeters and more can be produced without difficulty and at low cost.
- Another object of the invention relates to the use of the new tool described in detail above, especially as a piercer, forging mandrel or roll bar for the production of seamless tubes or for hot forging tubular metal workpieces.
- illustration 1 shows a hot tool in the form of a piercer in a side view.
- the tool 1 has a tool base 2, which has a working area 3 , which extends over a certain length in the direction of an axis a.
- the tool is provided with a coating 4 , which protects the tool 1 against thermal or mechanical stress.
- Figures 2 and 3 show the detail "Z" in the horizontal section through the tool according to illustration 1 once for the basic material body with raised relief before and after the oxide protective layer is created ("scaling").
- Fig. 2a one recognizes the saw-shaped relief, which was created according to Example 1 by applying a wire mesh.
- the main body is denoted by the reference numeral 6
- the network by the reference numeral 7 .
- Fig. 2b it can be seen that a part of the surface of the relief has been converted into oxide, but also between the meshes of the mesh the surface of the base has been oxidized (hatching with the reference numeral 8 ).
- Figures 3a and 3b are analogous, but the relief here has no square, but a round cross-section.
- the oxide layer hatchching
- the oxide layer is formed in equal proportions above and below the original surface of the iron-containing body.
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Coating By Spraying Or Casting (AREA)
- Forging (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Vorgeschlagen wird ein Warmumformwerkzeug 1 bestehend aus einem Werkzeuggrundkörper 2 mit wenigstens anteiliger Oberflächenbeschichtung 4, welches dadurch erhältlich ist, dass man den Grundkörper mit einem erhabenen metallischen Relief versieht, welches anschließend ganz oder teilweise oxidiert und in eine Schutzschicht umgewandelt wird.Proposed is a hot forming tool 1 consisting of a tool body 2 with at least proportionate surface coating 4, which is obtainable by providing the base body with a raised metallic relief, which is then completely or partially oxidized and converted into a protective layer.
Description
Die Erfindung befindet sich auf dem Gebiet der Herstellung von rohrförmigen Metallwerkstücken und betrifft Umformungswerkzeuge, speziell Lochdorne, Schmiededorne und Walzstangen mit verbesserter Standfestigkeit.The invention is in the field of manufacturing tubular metal workpieces and relates to forming tools, especially piercing mandrels, forged mandrels and billets with improved stability.
Nahtlose Stahlrohre werden im Allgemeinen in drei Umformstufen auf entsprechenden Walzwerken durch Warmumformung gefertigt. In einer ersten Stufe wird auf einem sogenannten Lochschrägwalzwerk ein auf etwa 1200°C erhitzter massiver Stahlblock mittels eines Innenwerkzeuges, des Lochdornes, zum Hohlblock umgeformt. Dabei wird der Block mittels schräg gestellter Walzen über den Lochdorn getrieben. In der zweiten Umformstufe wird der Hohlblock in einem Längswalzprozess über dem Innenwerkzeug, einer Walzstange, in Durchmesser und Wanddicke reduziert und in Längsrichtung gestreckt. In der dritten Umformstufe wird das Walzgut zu den geforderten Maßen in Durchmesser und Wanddicke umgeformt, wobei in der Regel kein Innenwerkzeug verwendet wird.Seamless steel tubes are generally manufactured in three forming steps on respective rolling mills by hot forming. In a first stage, a massive steel block heated to about 1200 ° C. is shaped to form a hollow block by means of an internal tool, the piercing mandrel, on a so-called perforated piercing mill. The block is driven by means of inclined rollers on the piercer. In the second forming step, the hollow block is reduced in a longitudinal rolling process over the inner tool, a rolling rod, in diameter and wall thickness and stretched in the longitudinal direction. In the third forming step, the rolling stock is converted to the required dimensions in diameter and wall thickness, with no internal tool is usually used.
Die Innenwerkzeuge in den beiden ersten Umformstufen sind bei der Produktion hohen Temperaturen und hohen mechanischen Drücken ausgesetzt. In den meisten Fällen bestehen die Innenwerkzeuge aus hochwarmfestem Stahl. Bei der Produktion speziell mit größeren Walzzeiten ist eine sukzessive Erwärmung des Innenwerkzeuges oft nicht zu vermeiden. Infolge der Erwärmung nimmt die Festigkeit des Werkzeuges ab und das Werkzeug kann dann den mechanischen Belastungen nicht mehr standhalten. Das Werkzeug deformiert sich und bricht.The inner tools in the first two forming stages are exposed to high temperatures and high mechanical pressures during production. In most cases, the inner tools are made of heat-resistant steel. In production, especially with longer rolling times, successive heating of the inner tool is often unavoidable. As a result of the heating, the strength of the tool decreases and the tool can then no longer withstand the mechanical loads. The tool deforms and breaks.
Um hohe Standzeiten zu erreichen, werden Lochdorne mit natürlichen Zunderschichten versehen. Diese Zunderschichten hemmen den Wärmezufluss vom Umformgut in das Werkzeug und schützen das Werkzeug vor schneller Erwärmung und raschem Festigkeitsverlust. Bei der Umformung von höher legierten Werkstoffen wird die Zunderschicht jedoch schnell abgetragen und der Wärmeschutz versagt.To achieve long service life, piercing mandrels are provided with natural scale layers. These scale layers inhibit the heat flow from the forming material into the tool and protect the tool against rapid heating and rapid loss of strength. When forming higher alloyed materials, however, the scale layer is quickly removed and thermal protection fails.
Bei Walzstangen werden je nach Umformverfahren natürlich verzunderte oder mit einer Chromschicht versehene Werkzeuge verwendet. Entsprechende Lochdorne sind beispielsweise aus der Deutschen Patentanmeldung
Die Standzeit der Werkzeuge ließe sich verbessern, wenn die Dicke der Oxidschicht vergrößert werden könnte. Dann wäre die Wärmeisolation besser und bei abrasivem Verschleiß bliebe die Schutzschicht länger erhalten.The service life of the tools could be improved if the thickness of the oxide layer could be increased. Then the heat insulation would be better and with abrasive wear the protective layer would remain longer.
Die Schutzschicht, die natürlich aus dem Grundmaterial durch Umwandlung in Eisenoxide gebildet ist, weist jedoch keine hohe Stabilität auf. Sie ist spröde und porös und kann daher leicht bei mechanischer und thermischer Belastung zerstört werden. Daher sind diese Schutzschichten in ihrer Dicke begrenzt. Der Grenzwert der Schicht liegt bei etwa 0.8 mm. Die Schutzwirkung einer solchen Schicht ist daher entsprechend begrenzt. Wärme dringt daher in den Grundkörper des Werkzeuges ein und vermindert seine Festigkeit, wodurch es dann zum frühzeitigen Versagen des Werkzeuges kommt. Bei hochlegiertem Umformgut führt die Abrasion relativ schnell, d.h. nach einer kleinen Länge gewalzten Materials zum Abtrag der Schutzschicht.However, the protective layer, which is naturally formed from the base material by conversion into iron oxides, does not have high stability. It is brittle and porous and can therefore easily be destroyed by mechanical and thermal stress. Therefore, these protective layers are limited in their thickness. The limit of the layer is about 0.8 mm. The protective effect of such a layer is therefore limited accordingly. Heat therefore penetrates into the body of the tool and reduces its strength, which then leads to premature failure of the tool. For highly alloyed products, the abrasion is relatively fast, i. after a small length of rolled material for removal of the protective layer.
Aus der internationalen Patentanmeldung
Ähnliche Werkzeuge, bei denen die Beschichtung aus Molybdän besteht, sind aus der
In der Praxis erweist sich die Herstellung solcher profilierter Werkzeuge jedoch als aufwendig, da die Profile einzeln in die Dorne geschnitten werden müssen, und außerdem zu Werkstoffverlusten führen. Die Herstellungskosten eines Profils erhöhen sich überproportional mit der Größe der einzubringenden Vertiefungen. Eine Wirtschaftlichkeits- und Machbarkeitsgrenze ist schon bei wenigen Millimetern erreicht. Ein weiterer Nachteil des in den Grundkörper geschnittenen Profils ist die Beschränkung des Werkstoffs auf gut oxidierbare Stähle. Diese haben insbesondere einen geringen Chromanteil und damit geringe Härte.In practice, however, the production of such profiled tools proves to be expensive, since the profiles must be cut individually into the mandrels, and also lead to material losses. The manufacturing costs of a profile increase disproportionately with the size of the wells to be introduced. A profitability and feasibility limit is reached even at a few millimeters. Another disadvantage of the profile cut into the base body is the limitation of the material to steels which are readily oxidizable. These have in particular a low chromium content and thus low hardness.
Die Aufgabe der vorliegenden hat daher darin bestanden, Warmumformwerkzeuge mit verbesserter Standfestigkeit zur Verfügung zu stellen, die frei von den eingangs geschilderten Nachteilen sind. Insbesondere sollten diese Werkzeuge im Vergleich zum Stand der Technik eine Oxidschicht mit höherer Festigkeit aufweisen, die sich zudem leicht und ohne Werkstoffverlust aufbringen lässt.The object of the present has therefore been to provide hot forming tools with improved stability, which are free of the disadvantages described above. In particular, in comparison to the prior art, these tools should have a higher strength oxide layer which, moreover, can be applied easily and without material loss.
Ein erster Gegenstand der Erfindung betrifft ein Warmumformwerkzeug bestehend aus einem Werkzeuggrundkörper mit wenigstens anteiliger Oberflächenbeschichtung, welches dadurch erhältlich ist, dass man den Grundkörper mit einem erhabenen metallischen Relief versieht, welches anschließend ganz oder teilweise oxidiert und in eine Schutzschicht umgewandelt wird.A first subject of the invention relates to a hot forming tool consisting of a tool base body with at least partial surface coating, which is obtainable by providing the base body with a raised metallic relief, which is then completely or partially oxidized and converted into a protective layer.
Ein weiterer Aspekt der Erfindung umfasst ein Verfahren zur Herstellung eines Warmumformwerkzeugs bestehend aus einem Werkzeuggrundkörper mit wenigstens anteiliger Oberflächenbeschichtung, bei dem man
- (a) den Grundkörper mit einem erhabenen metallischen Relief versieht, und
- (b) nachfolgend das metallische Relief ganz oder teilweise oxidiert und in eine Schutzschicht umwandelt.
- (a) provides the base body with a raised metallic relief, and
- (B) Subsequently, the metallic relief completely or partially oxidized and converted into a protective layer.
Das Aufbringen eines erhabenen Reliefs stellt den umgekehrten Fall zu einer Profilierung des Werkzeugs dar. Im Sinne der Erfindung wird also Werkstoff hinzugefügt und nicht entfernt. Überraschendweise wurde gefunden, dass die Reliefbildung im Gegensatz zur Profilierung nicht nur wesentlich einfacher zu realisieren ist, sondern durch vollständige oder teilweise Umwandlung des Reliefmaterials selbst eine deutlich härtere und damit beständigere Oxidschicht erhalten wird, was zu einer signifikanten Verbesserung der Lebensdauer des Werkzeugs führt. Die Erfindung bietet zudem die Möglichkeit, durch Auswahl des Reliefmaterials die Qualität des Oberflächenschutzes zu variieren und den Prozessbedingungen anzupassen.The application of a raised relief represents the opposite case to a profiling of the tool. For the purposes of the invention, therefore, material is added and not removed. Surprisingly, it was found that the relief formation in contrast to the profiling not only much easier to implement, but by completely or partially transforming the relief material itself a much harder and thus more resistant oxide layer is obtained, resulting in a significant improvement in the life of the tool. The invention also offers the possibility of varying the quality of the surface protection by selection of the relief material and of adapting the process conditions.
Der wirtschaftliche Nutzen der Erfindung liegt auf der Hand und besteht insbesondere in der Verringerung der Werkzeugkosten bei der Erzeugung von Stahlprodukten sowie der Verlängerung der Walzzeit, was in der Regel mit größeren Walzgutlängen und vermindertem Materialausschuss verbunden ist.The economic benefits of the invention are obvious and consist, in particular, in the reduction of tooling costs in the production of steel products and the extension of the rolling time, which is usually associated with larger rolling stock lengths and reduced rejects.
Bei den Warmumformungswerkzeugen der vorliegenden Erfindung handelt es sich vorzugsweise um einen Lochdorn oder einen Schmiededorn, die in der Regel aus Stahl bestehen. Die Erfindung umfasst unter diesem Oberbegriff jedoch grundsätzlich auch jedes andere metallische Werkstück, bei dem der Grundkörper gegen Wärmezustrom geschützt werden soll. Dabei ist der Begriff Metall nicht auf Eisen und Stahl beschränkt, sondern umfasst auch andere metallische Werkstoffe einschließlich metallhaltiger Verbundwerkstoffe, die einer Warmumformung zugeführt werden sollen.The hot forming tools of the present invention are preferably a piercer or a forging mandrel, which are typically steel. However, the invention fundamentally also encompasses any other metallic workpiece in which the base body is to be protected against heat flow. The term metal is not limited to iron and steel, but also includes other metallic materials including metal-containing composites that are to be subjected to hot working.
Doch nicht nur bei Dornen, den Innenwerkzeugen beim Lochen durch Schrägwalzen, auch bei den anderen Innenwerkzeugen, die bei der Herstellung nahtloser Stahlrohre verwendet werden, kann die erfindungsgemäße Oberflächenbeschichtung vorteilhaft angewandt werden. Bei den Walzstangen, den Innenwerkzeugen bei den Walzwerken mit mehreren hintereinander angeordneten Walzgerüsten in der zweiten Umformstufe ist insbesondere darauf zu achten, dass die Reibung zwischen Werkzeug und Walzgut gering ist. Daher muss für diesen Anwendungsfall die erfindungsgemäße Oberflächenschicht geschliffen und poliert werden. Auch kann eine zusätzliche Schicht z.B. aus Chrom auf die erfindungsgemäße Schutzschicht aufgetragen werden.However, not only for thorns, the internal tools for punching by means of oblique rolling, but also for the other internal tools used in the production of seamless steel tubes, the surface coating according to the invention can be advantageously used. In the case of the rolling rods, the internal tools in the rolling mills with a plurality of rolling mills arranged one behind the other in the second forming stage, particular care must be taken to ensure that the friction between the tool and the rolling stock is low. Therefore, the surface layer according to the invention must be ground and polished for this application. Also, an additional layer e.g. be applied from chrome on the protective layer according to the invention.
Das erhabene Relief, das auf den Grundkörper aufgebracht wird, kann ganz unterschiedlich ausgeprägt sein, wobei die alternativen Ausführungsformen alle grundsätzlich geeignet sind, die gestellte Aufgabe vollumfänglich zu erfüllen.The raised relief, which is applied to the base body, can be pronounced differently, the alternative embodiments are all in principle suitable to fulfill the task fully.
In einer ersten Ausführungsform kann es sich bei dem erhabenen Relief schlicht um eine Umwicklung des Grundkörpers mit einem Draht, vorzugsweise einem Stahldraht handeln.In a first embodiment, the raised relief may simply be a wrapping of the base body with a wire, preferably a steel wire.
In einer zweiten Ausführungsform kann das erhabene Relief ein Metallgewebe oder Metallnetz darstellen, das auf den Grundkörper aufgebracht wird.In a second embodiment, the raised relief may be a metal mesh or metal net applied to the base.
Die auf die Oberfläche des Werkzeuges aufgebrachten metallischen Körper bestehen vorzugsweise aus einem Stahlgewebe, beispielsweise mit einer Stahldrahtdicke von etwa 1 bis etwa 5 mm und vorzugsweise etwa 1,5 mm und einer Maschenweite von etwa 1 bis 5 mm und insbesondere etwa 2,5 mm. Unter Maschenweite ist der Abstand der Mittellinien zweier benachbarter Gewebeelemente zu verstehen.The metallic bodies applied to the surface of the tool preferably consist of a steel mesh, for example with a steel wire thickness of about 1 to about 5 mm and preferably about 1.5 mm and a mesh size of about 1 to 5 mm and in particular about 2.5 mm. Mesh size is the distance between the center lines of two adjacent fabric elements.
In einer dritten Ausführungsform kann es sich bei dem erhabenen Relief um eine unregelmäßige Beschichtung handeln, wie sie durch chemische oder physikalische Abscheidung von Metall aus der Dampfphase erreicht wird.In a third embodiment, the raised relief may be an irregular coating as achieved by chemical or physical vapor deposition of metal.
Das Aufbringen des erhabenen Reliefs kann nach sehr unterschiedlichen - einfachen wie komplexen - Verfahren erfolgen, die doch alle die Aufgabe der Erfindung voll umfänglich lösen.The application of the raised relief can be done according to very different - simple and complex - method, but all solve the task of the invention fully.
In einer ersten Ausführungsform wird der Grundkörper schlicht mit einem Draht, vorzugsweise einem Metalldraht umwickelt.In a first embodiment , the basic body is simply wrapped with a wire, preferably a metal wire.
In einer zweiten alternativen Ausführungsform wird statt des Drahtes ein Metallgewebe oder ein Metallnetz eingesetzt. Dieses kann beispielsweise durch Umformung auf die Form des Werkzeugs vorgeformt und dann auf den Grundkörper aufgezogen werden. Um die Festigkeit zu erhöhen empfiehlt es sich, die Drahtwicklung oder das Metallgewebe mit dem Grundkörper zu verschweißen.In a second alternative embodiment , a metal mesh or a metal mesh is used instead of the wire. This can be preformed, for example by deformation to the shape of the tool and then mounted on the body. To increase the strength, it is advisable to weld the wire winding or the metal mesh to the base body.
In einer dritten alternativen Ausführungsform ist es möglich, das Relief auf der Oberfläche des Grundkörpers durch Chemische oder Physikalische Dampfphasenabscheidung (Chemical/Physical Vapour Phase Deposition, CVD/PVD) zu erzeugen.In a third alternative embodiment , it is possible to produce the relief on the surface of the base body by chemical or physical vapor phase deposition (CVD / PVD).
Unter dem Begriff chemische Gasphasenabscheidung versteht man eine Gruppe von Beschichtungsverfahren, welche unter anderem bei der Herstellung von mikroelektronischen Bauelementen und Lichtwellenleitern eingesetzt werden. An der erhitzten Oberfläche eines Substrates wird aufgrund einer chemischen Reaktion aus der Gasphase eine Feststoffkomponente abgeschieden. Voraussetzung hierfür ist, dass flüchtige Verbindungen der Schichtkomponenten existieren, die bei einer bestimmten Reaktionstemperatur die feste Schicht abscheiden. Das Verfahren der chemischen Gasphasenabscheidung zeichnet sich durch mindestens eine Reaktion an der Oberfläche des zu beschichtenden Werkstücks aus. An dieser Reaktion muss mindestens eine gasförmige Ausgangsverbindung (Edukt) und mindestens zwei Reaktionsprodukte - davon mindestens eines in der festen Phase - beteiligt sein. Um gegenüber konkurrierenden Gasphasen-Reaktionen jene Reaktionen an der Oberfläche zu fördern und damit die Bildung von festen Partikeln zu vermeiden, wird das Verfahren vorzugsweise bei vermindertem Druck durchgeführt.The term chemical vapor deposition refers to a group of coating processes which are used inter alia in the production of microelectronic components and optical waveguides. On the heated surface of a substrate, a solid component is deposited due to a chemical reaction from the gas phase. The prerequisite for this is that volatile compounds of the layer components exist, which deposit the solid layer at a certain reaction temperature. The process of chemical vapor deposition is characterized by at least one reaction on the surface of the workpiece to be coated. At least one gaseous starting compound (starting material) and at least two reaction products - at least one of which in the solid phase - must be involved in this reaction. In order to promote surface reactions to competing gas phase reactions and thus avoid the formation of solid particles, the process is preferably carried out at reduced pressure.
Anders als bei der CVD wird mithilfe der bevorzugten PVD das Ausgangsmaterial in die Gasphase übergeführt. Das gasförmige Material wird anschließend zum zu beschichtenden Substrat geführt, wo es kondensiert und die Zielschicht bildet. Beispiele hierfür sind klassische verdampfungsverfahren, wie das thermische Verdampfen, Elektronenstrahlverdampfen (Electron Beam Evaporation) oder das Laserstrahlverdampfen (Pulsed Laser Deposition). Im Sinne der vorliegenden Erfindung bevorzugt ist das Sputtern, bei dem das Ausgangsmaterial durch lonenbeschuss zerstäubt und in die Gasphase überführt wird, aus der es dann auf den Grundkörper wieder abgelagert werden kann. Allen diesen Verfahren ist gemein, dass das abzuscheidende Material in fester Form in der meist evakuierten Beschichtungskammer vorliegt. Durch den Beschuss mit Laserstrahlen, magnetisch abgelenkten Ionen oder Elektronen sowie durch Lichtbogenentladung wird das Target verdampft. Wie hoch der Anteil an Atomen, Ionen oder größeren Clustern im Dampf ist, ist von Verfahren zu Verfahren unterschiedlich. Das verdampfte Material bewegt sich entweder ballistisch oder durch elektrische Felder geführt durch die Kammer und trifft dabei auf die zu beschichtenden Teile, wo es zur Schichtbildung kommt.Unlike CVD, the preferred PVD converts the feedstock into the gas phase. The gaseous material is then passed to the substrate to be coated, where it condenses and forms the target layer. Examples include classical evaporation methods, such as thermal evaporation, electron beam evaporation or laser beam evaporation (Pulsed Laser Deposition). For the purposes of the present invention, sputtering is preferred in which the starting material is atomized by ion bombardment and transferred into the gas phase, from which it can then be deposited again onto the base body. All these methods have in common that the material to be deposited in solid form in the most evacuated coating chamber is present. By bombardment with laser beams, magnetically deflected ions or electrons as well as by arc discharge, the target is vaporized. The amount of atoms, ions or larger clusters in the vapor varies from process to process. The vaporized material moves either ballistically or by electric fields guided through the chamber and strikes the parts to be coated, where it comes to film formation.
Damit die Dampfteilchen die Bauteile auch erreichen, und nicht durch Streuung an den Gasteilchen verloren gehen, muss im Unterdruck gearbeitet werden. Typische Arbeitsdrucke liegen im Bereich von 10-4 Pa bis ca. 10 Pa. Da sich die Dampfteilchen geradlinig ausbreiten, werden Flächen, die vom Ort der Dampfquelle aus gesehen nicht sichtbar sind, mit einer geringeren Beschichtungsrate beschichtet. Um ein Relief und keine homogene Beschichtung erzeugen, wird anders als üblich auf eine Rotation des Substrates verzichtet.In order for the vapor particles to reach the components, and not be lost by scattering on the gas particles, it is necessary to work under reduced pressure. Typical working pressures are in the range of 10 -4 Pa to about 10 Pa. As the vapor particles propagate in a straight line, areas that are invisible from the location of the vapor source are coated at a lower coating rate. In order to produce a relief and no homogeneous coating, unlike usual is dispensed with a rotation of the substrate.
Eine vierte alternative Ausführungsform zur Reliefbildung umfasst das so genannte thermische Spritzen. Dabei werden Zusatzwerkstoffe, die so genannten Spritzzusätze, innerhalb oder außerhalb eines Spritzbrenners ab-, an- oder aufgeschmolzen, in einem Gasstrom in Form von Spritzpartikeln beschleunigt und auf die Oberfläche des zu beschichtenden Bauteils geschleudert. Die Bauteiloberfläche wird dabei (im Gegensatz zum Auftragschweißen) nicht angeschmolzen und nur in geringem Maße thermisch belastet. Eine Schichtbildung findet statt, da die Spritzpartikel beim Auftreffen auf die Bauteiloberfläche prozess- und materialabhängig mehr oder minder abflachen, vorrangig durch mechanische Verklammerung haften bleiben und lagenweise die Spritzschicht aufbauen. Qualitätsmerkmale von Spritzschichten sind geringe Porosität, gute Anbindung ans Bauteil, Rissfreiheit und homogene Mikrostruktur. Die erzielten Schichteigenschaften werden maßgeblich beeinflusst von der Temperatur und der Geschwindigkeit der Spritzpartikel zum Zeitpunkt ihres Auftreffens auf die zu beschichtende Oberfläche. Der Oberflächenzustand (Reinheit, Aktivierung, Temperatur) übt ebenfalls maßgeblichen Einfluss auf Qualitätsmerkmale wie die Haftfestigkeit aus.A fourth alternative embodiment for the formation of relief comprises the so-called thermal spraying. This filler materials, the so-called spray additives, inside or outside of a spray burner off, on or melted, accelerated in a gas stream in the form of spray particles and thrown onto the surface of the component to be coated. The component surface is not melted (in contrast to build-up welding) and only subjected to a low thermal load. A layer formation takes place because the spray particles flatten more or less depending on the process and material when hitting the component surface, stick primarily by mechanical clamping and layer by layer build up the spray layer. Quality features of sprayed coatings are low porosity, good adhesion to the component, freedom from cracks and homogeneous microstructure. The achieved coating properties are significantly influenced by the temperature and the speed of the spray particles at the time of their impact on the surface to be coated. The surface condition (purity, activation, temperature) also has a significant influence on quality features such as adhesion.
Als Energieträger für die An- oder Aufschmelzung des Spritzzusatzwerkstoffes dienen elektrischer Lichtbogen (Lichtbogenspritzen), Plasmastrahl (Plasmaspritzen), Brennstoff-Sauerstoff-Flamme bzw. Brennstoff-Sauerstoff-Hochgeschwindigkeitsflamme (konventionelles und Hochgeschwindigkeits-Flammspritzen), schnelle, vorgewärmte Gase (Kaltgasspritzen) und Laserstrahl (Laserstrahlspritzen). Laut DIN-Norm EN 657 werden die Spritzverfahren nach diesen Kriterien eingeteilt.As an energy source for the on or melting of the spray additive used electric arc (arc spraying), plasma jet (plasma spraying), fuel-oxygen flame or fuel-oxygen high-speed flame (conventional and high-speed flame spraying), fast, preheated gases (cold gas spraying) and Laser beam (laser beam spraying). According to DIN standard EN 657, the spraying processes are classified according to these criteria.
Mit Hilfe dieses Verfahrens kann der Grundkörper nicht nur mit Metallen, sondern auch oxidkeramischen Werkstoffen und carbidischen Werkstoffen (bzw. allgemein Verbundwerkstoffen) beschichtet werden. Vorzugsweise erfolgt bei dieser Ausführungsform die Beschichtung mit einer Eisen/Keramikmischung.With the aid of this method, the base body can be coated not only with metals but also with oxide-ceramic materials and carbide materials (or in general composite materials). Preferably, in this embodiment, the coating is carried out with an iron / ceramic mixture.
Während der Grundkörper vorzugsweise aus Stahl besteht, gilt für das Material, welches das erhabene Relief bildet, die Anforderung, dass es wenigstens anteilig zur Ausbildung einer Oxidschicht befähigt ist. Vorzugsweise handelt es sich hierbei um Eisen oder Stahl, sodass eine Eisenoxidschicht, vorzugsweise Zunder erzeugt wird. Es kann wie gesagt auch eine Mischung aus Eisen/Stahl und Keramik verwendet werden, beispielsweise in einem Gewichtsverhältnis von etwa 20:80 bis etwa 80:20.While the body is preferably made of steel, the requirement for the material forming the raised relief is that it be at least partially capable of forming an oxide layer. Preferably, this is iron or steel, so that an iron oxide layer, preferably scale is produced. As stated, a mixture of iron / steel and ceramics may also be used, for example in a weight ratio of about 20:80 to about 80:20.
Es versteht sich, dass das Relief unterschiedlichste Formen aufweisen kann, die von regelmäßig (rund, eckig etc.) bis zu jeder beliebigen Freiform reichen. Es können auch Materialverbunde eingesetzt werden, d.h. beispielsweise ein Molybdängewebe, das auf den Grundkörper aus Stahl aufgebracht wird. Das Gewebeelement kann auch aus einem Verbund von hartem Chromstahl (innen) und gut oxidierbarem Stahl (außen) bestehen. Als Abstandshalter können auch brennbare Materialien eingesetzt werden. Es ist ebenfalls möglich, zur besseren Wärmedämmung Keramik mit einzulagern.It is understood that the relief can have a variety of forms, ranging from regular (round, square, etc.) to any free-form. Material composites can also be used, i. For example, a molybdenum fabric, which is applied to the body made of steel. The fabric element may also consist of a composite of hard chrome steel (inside) and good oxidizable steel (outside). As spacers and combustible materials can be used. It is also possible to store ceramic for better thermal insulation.
Die vollständige oder teilweise Umwandlung des metallischen Reliefs in eine oxidische Schutzschicht kann nach bekannten Verfahren des Stands der Technik erfolgen, beispielsweise durch Flammspritzen, Plasmaspritzen oder durch ein thermochemisches Verfahren erfolgt.The complete or partial conversion of the metallic relief into an oxide protective layer can be carried out by known processes of the prior art, for example by flame spraying, plasma spraying or by a thermochemical process.
Bei der Oxidation des Werkzeuges mit dem auf seiner Oberfläche aufgebrachten metallischen Körper, zum Beispiel einem Stahlgewebe, wird ein Teil der Oberfläche des Werkzeuggrundkörpers sowie ein Teil des auf der Oberfläche aufgebrachten metallischen Reliefs in Oxid umgewandelt. Gleichzeitig wird auf allen Oberflächen eine zusätzliche Oxidschicht gebildet, die typischerweise etwa 500 bis etwa 3.000 µm und insbesondere etwa 1.500 bis etwa 2.500 µm beträgt. Dadurch wird auch Oxid in den Zwischenräumen zwischen den Körpern, zum Beispiel zwischen Werkzeuggrundkörper und aufgebrachten Stahlgewebe und innerhalb der Maschen des Stahlgewebes gebildet. Im Ergebnis erhält man eine besonders dicke Schutzschicht, die durch innenliegende Körper verstärkt ist. Insbesondere ist die Schichtdicke anders als bei der Herstellung von Vertiefungen nicht auf wenige Millimeter begrenzt. Schichtdicken von 10 Millimeter und mehr lassen sich ohne Schwierigkeit und mit geringen Kosten erzeugen.During the oxidation of the tool with the metallic body applied to its surface, for example a steel mesh, a part of the surface of the tool base and a part of the metal relief applied to the surface are converted into oxide. At the same time an additional oxide layer is formed on all surfaces, which is typically about 500 to about 3,000 microns, and more preferably about 1,500 to about 2,500 microns. As a result, oxide is also formed in the interstices between the bodies, for example, between the tool body and the applied steel mesh and within the mesh of the steel mesh. The result is a particularly thick protective layer reinforced by internal bodies. In particular, unlike the production of depressions, the layer thickness is not limited to a few millimeters. Layer thicknesses of 10 millimeters and more can be produced without difficulty and at low cost.
Ein weiterer Gegenstand der Erfindung betrifft die Verwendung des oben ausführlich beschriebenen neuen Werkzeugs, speziell als Lochdorn, Schmiededorn oder Walzstange zur Herstellung von nahtlosen Rohren oder zum Warmschmieden von rohrförmigen Werkstücken aus Metall.Another object of the invention relates to the use of the new tool described in detail above, especially as a piercer, forging mandrel or roll bar for the production of seamless tubes or for hot forging tubular metal workpieces.
Auf der Oberfläche eines Lochdorns wurde ein durch Umformung an die Form des Grundkörpers vorgeformtes Stahlgewebe mit einer Stahldrahtdicke von 1.5 mm und einer Maschenweite von 2.5 mm aufgelegt und verschweißt. Anschließend wurde der Verbund einer thermo-chemischen Oxidation ausgesetzt. Es wurde eine zusammenhängende lückenlose Oxidschicht von 2.500 µm Dicke erhalten.On the surface of a piercer a preformed by forming to the shape of the body steel fabric was placed with a steel wire thickness of 1.5 mm and a mesh size of 2.5 mm and welded. Subsequently, the composite was subjected to a thermochemical oxidation. It was obtained a coherent gapless oxide layer of 2,500 microns thickness.
Die Abbildungen 2 und 3 zeigen die Einzelheit "Z" im horizontalen Schnitt durch das Werkzeug gemäß
In
Die Abbildungen 3a und 3b sind analog, jedoch weist das Relief hier keinen eckigen, sondern einen runden Querschnitt auf. Auch hier erkennt man, dass die Oxidschicht (Schraffur) sich zu gleichen Anteilen ober- und unterhalb der ursprünglichen Oberfläche des eisenhaltigen Körpers bildet. Figures 3a and 3b are analogous, but the relief here has no square, but a round cross-section. Here, too, it can be seen that the oxide layer (hatching) is formed in equal proportions above and below the original surface of the iron-containing body.
Claims (15)
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BR112017007858-9A BR112017007858A2 (en) | 2014-11-07 | 2015-11-04 | hot forming tool |
CN201580060124.1A CN107206442B (en) | 2014-11-07 | 2015-11-04 | Thermoforming tool |
US15/519,988 US20170333964A1 (en) | 2014-11-07 | 2015-11-04 | Hot forming tool |
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DE102014016502.7A DE102014016502A1 (en) | 2014-11-07 | 2014-11-07 | Hot forming tool with reinforced oxide protective layer |
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EP3590622A1 (en) * | 2018-07-04 | 2020-01-08 | KME Germany GmbH & Co. KG | Thermoforming tool and method for producing same |
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RU2017118964A3 (en) | 2018-12-07 |
CN107206442B (en) | 2020-04-07 |
CN107206442A (en) | 2017-09-26 |
US20170333964A1 (en) | 2017-11-23 |
WO2016071423A1 (en) | 2016-05-12 |
RU2017118964A (en) | 2018-12-07 |
DE102014016502A1 (en) | 2016-05-12 |
JP2017536237A (en) | 2017-12-07 |
EP3017888B1 (en) | 2019-04-24 |
KR20170086519A (en) | 2017-07-26 |
RU2687321C2 (en) | 2019-05-13 |
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