EP2006398B1 - Procédé de fabrication d'un acier - Google Patents

Procédé de fabrication d'un acier Download PDF

Info

Publication number
EP2006398B1
EP2006398B1 EP07741346.6A EP07741346A EP2006398B1 EP 2006398 B1 EP2006398 B1 EP 2006398B1 EP 07741346 A EP07741346 A EP 07741346A EP 2006398 B1 EP2006398 B1 EP 2006398B1
Authority
EP
European Patent Office
Prior art keywords
steel material
semi
temperature
product steel
pearlite
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.)
Not-in-force
Application number
EP07741346.6A
Other languages
German (de)
English (en)
Other versions
EP2006398A4 (fr
EP2006398A1 (fr
Inventor
Hitoshi Kataoka
Hirotaka Eguchi
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.)
Proterial Ltd
Original Assignee
Hitachi Metals Ltd
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 Hitachi Metals Ltd filed Critical Hitachi Metals Ltd
Publication of EP2006398A1 publication Critical patent/EP2006398A1/fr
Publication of EP2006398A4 publication Critical patent/EP2006398A4/fr
Application granted granted Critical
Publication of EP2006398B1 publication Critical patent/EP2006398B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/002Heat treatment of ferrous alloys containing Cr
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C21D8/0263Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment following hot rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24Ferrous alloys, e.g. steel alloys containing chromium with vanadium

Definitions

  • the present invention relates to a process for producing a steel material having a pearlite nose at which transformation completes for not less than 30 minutes. More particularly, the invention relates to a process for producing a steel material, including a first hot working step a second, hot working step, and process annealing of a semi-product steel material (semi-finished steel product) between the first and the second hot working steps.
  • a steel material is subjected to a first hot working step such as hot forging or hot rolling and then is subjected to a second hot working step such as hot forging or hot rolling
  • its metallographic structure changes into a hard martensitic structure when it is kept in the atmosphere to cool after the completion of the first hot working step step, if the steel material has extremely high hardenability.
  • a delayed crack then occurs in a short time.
  • the worked steel material (semi-product steel material) is cooled (2 in Fig. 2 ) after the completion of a hot working step 1 such as hot forging or hot rolling.
  • the steel material is promptly introduced into a heating furnace (25 in Fig. 2 ) for an annealing step 3.
  • the steel material is heated to and kept at a desired temperature not less than the Ac3 point (26 in Fig. 2 ) under control to completely transform it into austenite.
  • the steel material is controlled to be then cooled in such a slow cooling rate (27, 28, 29 in Fig. 2 ) as to sufficiently cause pearlitic transformation even if the semi-product steel material has extremely high hardenability, thereby completing process annealing.
  • the process-annealed semi-product steel material is adjusted to have a low hardness as well as the adjustment of the metallographic structure, thus providing the material to be subjected to hot working in the second step.
  • JP 11302725 discloses a tool steel annealing method which involves granulation annealing in a furnace after reaching particular point between pearlite nose temperature and Ac1 transformation temperature.
  • JP-A-8-260058 As another means of performing slow cooling for generating pearlitic transformation, application of a special cooling chamber provided with a heat insulating material is proposed in JP-A-8-260058 (see Patent document 1).
  • Patent document 1 JP-A-8-260058
  • the semi-product steel material after the hot working step is allowed to pass the transformation point repeatedly in the process annealing to form the pearlite structure and reducing the hardness without generating any cracks in the steel material. For this reason, the hot working forms a stable austenitic structure, and then the steel material is cooled into a martensitic transformation region or a bainitic transformation region.
  • the process annealing so as to repeat transformation, in which the semi-product steel material is thereafter introduced into a heating furnace to be completely transformed into austenite at not lower than the Ac3 point, and then carefully cooled slowly.
  • An object of the present invention is to provide a process for producing a steel material, which does not use any furnace but has the same effect as process annealing using a furnace, in the case of process annealing a alloy steel material having a pearlite nose transformation completion point of not shorter than 30 minutes and having extremely high hardenability.
  • the present invention is achieved in consideration of the above-described problems.
  • the present invention provides a process for producing a steel material having a pearlite nose transformation completion point of not shorter than 30 minutes, the process including a first hot working step, a second hot working step and process annealing performed between the first and the second hot working steps, the process annealing including steps of introducing a semi-product steel material after the first hot working step into a heat-insulation vessel, recuperating heat in the steel material, and holding the semi-product steel material at a temperature within a range of the pearlite nose transformation completion point plus/minus 20°C for not shorter than 30 minutes with use of transformation latent heat from the semi-product steel material, so that the semi-product steel material is transformed into pearlite
  • the process for producing the steel material includes holding the semi-product steel material introduced into the heat-insulation vessel at the temperature of the pearlite nose transformation completion point plus/minus 20°C for not shorter than 2 hours.
  • the process for producing the steel material includes holding the semi-product steel material introduced into the heat-insulation vessel at the temperature within the pearlite nose transformation completion point plus/minus 10°C for not shorter than 2 hours. Further preferably, the maximum surface temperature of the semi-product steel material when introduced into the heat-insulation vessel is within the range between the transformation completion point at pearlite nose plus 100°C and the transformation completion point at pearlite nose minus 200°C.
  • the hardness of the semi-product steel material after the process annealing is not higher than 300 HB, according to the process for producing the steel material.
  • the process for producing the steel material according to the invention is particularly favorable for the semi-product steel material having a weight of not less than 500 kg.
  • the process for producing the steel material according to the invention is particularly desirable for a semi-product steel material having a chemical composition containing, by mass percent: 0.10 to 2.0% of C; not more than 2.0% of Si; not more than 2.0% of Mn; 1.0 to 15.0% of Cr; and not more than 10.0% of Mo; at least one of not more than 4.0% of Ni, not more than 4.0% of V, not more than 20.0% of W, and not more than 10.0% of Co; and the balance being substantially Fe.
  • the temperature of the steel material is maintained by introducing the steel material into the heat-insulation vessel and utilizing pearlite transformation latent heat of the steel material, instead of using a heating furnace, thereby achieving the same effect as that of process annealing.
  • a process for producing a steel material having a pearlite nose transformation completion point of not shorter than 30 minutes includes, for example, a melting step of casting a molten steel to obtain a steel ingot, a step of performing hot working a certain number of times on the steel ingot obtained by the melting step, and process annealing performed between executions of hot working.
  • the hot-worked and process annealed material may be subjected to heat treatment such as annealing or quenching and tempering.
  • Process annealing according to the invention is defined as annealing performed between the first and the second hot working steps as described above.
  • first and second annealings correspond to the process annealing according to the invention.
  • the invention is applied to production of a steel material having a pearlite nose transformation completion point of not shorter than 30 minutes and having high hardenability, for which independent process annealing under strict temperature control has been considered indispensable.
  • the steel material having a pearlite nose transformation completion point of not shorter than 30 minutes includes e.g. alloy tool steels such as SKD11, SKD61 and SKT4.
  • the steel material annealing method according to the invention is more advantageously applied to a steel material having a pearlite nose transformation completion point of not shorter than 60 minutes, more preferably, to a steel material having a pearlite nose transformation completion point of not shorter than 90 minutes, and further preferably to a steel material having a pearlite nose transformation completion point of not shorter than 2 hours.
  • the pearlite nose transformation completion point may be measured as described below.
  • a steel material of e.g. SKD61 is transformed to have an austenitic metallographic structure, quenched to a certain temperature not higher than the A1 point and held at the temperature. After a certain time period from the start of holding at the temperature, pearlitic transformation starts. With a lapse of time, the transformation ends. When the material is cooled before the completion of the transformation, the remaining austenite is transformed into martensite. Therefore, the time period before the end of the transformation can be obtained by measuring the hardness.
  • pieces of steel material heated to a hot forging temperature are introduced into furnaces at temperatures set every 25°C steps in a range from 700 to 775°C and are held for 2, 5, 15 and 24 hours.
  • the pieces of steel material held at the temperatures and for the periods as described above are taken out of the furnaces and cooled by air, and the hardness of the steel material is measured.
  • the pearlite nose transformation completion point is in the vicinity of at 750°C for 5 hours, that is shortest-time point in the points where the hardness decreases abruptly.
  • a pearlite nose transformation completion point located at a holding time of 30 minutes is referred to as a pearlite nose transformation completion point of 30 minutes (a curved line represented by a dotted line in Fig. 3 ), and a pearlite nose transformation completion point located on the longer-holding-time side including 30 minutes is referred to as a pearlite nose transformation completion point of not shorter than 30 minutes (a curved line represented by a solid line in Fig. 3 ).
  • specified process annealing is performed on the above-described steel material having a pearlite nose transformation completion point of not shorter than 30 minutes and having good hardenability.
  • the reason for the process annealing method specified in the invention will be described in detail with reference to a heat pattern shown in Fig. 1 .
  • the semi-product steel material is cooled (2 in Fig. 1 : a post-hot-working cooling step).
  • the semi-product steel material is introduced into a heat insulation vessel and an annealing step 3 is started.
  • the semi-product steel material is introduced into the heat insulation vessel to recuperate the surface temperature of the semi-product steel material (21 in Fig. 1 ).
  • Recuperation is defined as follows.
  • the semi-product steel material introduced into the heat insulation vessel is increased in the surface temperature through heat conduction from an inner portion of the semi-product steel material and radiant heat from the walls of the heat insulation vessel, and the temperature difference between the internal temperature of the semi-product steel material and the surface temperature of the semi-product steel material is reduced. This is a preparation to temperature holding with use of transformation latent heat of the semi-product steel material.
  • the temperature is held (22 in Fig. 1 ) with the transformation latent heat of the semi-product steel material in the heat insulation vessel.
  • the invention utilizes heat generated when the semi-product steel material transforms to keep the temperature of the material. That is, the present invention keeps the temperature of the semi-product steel material in a constant temperature range for a certain time period utilizing transformation latent heat of the semi-product steel material to transform the material to pearlite.
  • the held temperature range and the time period are extremely important.
  • held temperature is at a temperature within a range of the pearlite nose transformation completion point plus 20°C and the pearlite nose transformation completion point minis 20°C for not shorter than 30 minutes. Holding in such a particular temperature range enables obtaining an annealed state, which has not been obtained. Moreover, according to the invention, the efficiency is extremely high as a result of finding that transformation latent heat in the semi-product steel material can be utilized, which will be described below in detail.
  • a temperature range exceeding the pearlite nose transformation completion point plus 20°C requires a longer time to complete the pearlitic transformation and is, therefore, uneconomical, and a problem also arises that the metallographic structure easily becomes coarser.
  • a temperature range below the pearlite nose transformation completion point minus 20°C also requires a longer time to complete pearlitic transformation and is, therefore, uneconomical, and entails a problem that pearlitic transformation cannot occur and progress, resulting in insufficient reduction of the hardness.
  • the preferable temperature range is within a range of the pearlite nose transformation completion point plus/minus 10°C.
  • the reason why the holding time is selected to be not shorter than 30 minutes is because pearlitic transformation may not complete if the holding time is shorter than 30 minutes, and, in such a case, softening will be insufficient due to insufficient precipitation of carbides and a fault such as a crack will be generated.
  • a preferable holding time at the temperature is not shorter than 1 hour.
  • a more preferable holding time is not shorter than 2 hours.
  • a further more preferable range of the holding time is 2 to 24 hours.
  • the hardness after process annealing can be reduced to not higher than 300 HB, which is preferable for process-annealed material.
  • the hardness after process annealing is preferably not higher than 270 HB, more preferably not higher than 250 HB.
  • the maximum surface temperature of the semi-product steel material when the semi-product steel material is introduced into the heat insulation vessel, is in a range between the pearlite nose transformation completion point plus 100°C and the pearlite nose transformation completion point minus 200°C.
  • the temperature of the semi-product steel material will become excessively high by recuperation of heat from the semi-product steel material and the metallographic structure will easily have coarser grains. This coarsening of the structure is noticeable in a temperature range not lower than the pearlite nose transformation completion point plus 200°C. Therefore, the preferable upper limit of the temperature at which the semi-product steel material is introduced into the heat insulation vessel, is determined to be the pearlite nose transformation completion point plus 100°C in consideration of recuperation of heat from the semi-product steel material.
  • the lower limit of the maximum surface temperature of the steel material, when the material is introduced into the heat insulation vessel, is determined to be the pearlite nose transformation completion point minus 200°C. This is because heat-recuperation is difficult to heat the semi-product steel material to the temperature within the pearlite nose transformation completion point plus/minus 20°C in the heat insulation vessel if the maximum surface temperature of the steel material is lower than the pearlite nose transformation completion point minus 200°C.
  • the maximum temperature of the material surface is between the pearlite nose transformation completion point plus 50°C and the pearlite nose transformation completion point minus 150°C.
  • the maximum surface temperature of the steel material refers to the temperature of a region where the temperature is highest in the entire surface of the steel material.
  • the temperature of the semi-product steel material surface is defined according to the invention.
  • the temperature of the material surface may be measured, for example, by a radiation thermometer.
  • the heat insulation vessel referred to in the invention is, for example, a box-like member or lid-like member with which the semi-product steel material is covered.
  • the heat insulation vessel has no heating sources. It may be of any structures which enables the semi-product steel material to be transformed into pearlite with the transformation latent heat from the material by holding the material in a certain temperature range for a certain time period, for example, by providing a heat insulating member inside of the box-like or lid-like member to form an enclosed space.
  • the heat insulation vessel may be provided with holes or the like, e.g., for insertion of a thermocouple thermometer, for visually checking of the color tone of the steel material in the vessel or an opening having an openable/closable structure for adjusting the temperature of the material surface. It is not necessarily required to form an enclosed space completely isolated from the external atmosphere.
  • the heat insulation vessel 7 may have a structure shown in schematic front and side views in Figs. 5A to 5D , in which a semi-product steel material 4 is placed on a heat insulation vessel base 5 and a heat insulation vessel upper lid 6 is put over the base 5 to form an enclosed space surrounding the material 4.
  • a semi-product steel material 4 is placed on a heat insulation vessel base 5 and a heat insulation vessel upper lid 6 is put over the base 5 to form an enclosed space surrounding the material 4.
  • it may have a structure shown in schematic front and side views in Figs. 6A to 6D , in which the semi-product steel material 4 is placed in a heat insulation vessel lower lid 8 and a heat insulation vessel upper lid 6 is put to form an enclosed space surrounding the material 4.
  • it may have a truck-type structure shown in Fig.
  • the semi-product steel material 4 is placed on a heat insulation vessel base 5 and a heat insulation vessel 7 with wheels 10 capable of traveling on rails 11 is caused to move in the direction of the arrow to form an enclosed space surrounding the material 4.
  • the vessel 7 may be fixed and the base provided with wheels may be moved.
  • the structure of the heat insulation vessel may be designed by considering the shape and weight of the semi-product steel material, according to the invention.
  • the vessel in a case where the semi-product steel material is in a form of a round bar, for which collapse of a stack possibly occurs, the vessel may have a structure shown in Figs. 7A and 7C , in which the lower lid 7 is formed to have a triangular section where round bars of the material 4 are loaded in the lower lid 7 and the upper lid 6 is put thereon.
  • a heat insulation vessel having a structure shown in Figs. 5C and 5D , Figs. 6A to 6D or Figs. 7A to 7D in terms of workability and working safety.
  • Figs. 5A and 5B , Figs. 6A, and 6B and Figs. 7A and 7B show states where enclosed spaces are not formed
  • Figs. 5C and 5D , Figs. 6C and 6D and Figs. 7C and 7D show states where enclosed spaces are formed.
  • the annealing step 3 is executed, in which a temperature of the semi-product steel material is kept by using the above-described heat insulation vessel, and the semi-product steel material is taken out from the vessel (23 in Fig. 1 ) to be subjected to slow cooling (24 in Fig. 1 ), thus completing the annealing step 3.
  • the invention is particularly preferably applied to a large-sized piece of semi-product steel material having a weight of not less than 500 kg. This is because the large-sized piece of the material having a weight of not less than 500 kg ensures a necessary amount of heat for keeping a temperature for recuperation with transformation latent heat for a sufficient time for pearlitic transformation.
  • the above-described effect may be further obtained for a large piece of the semi-product steel material having a weight of not less than 1 ton. It is further effective for a piece of not less than 4 ton.
  • the semi-product steel material is held at a temperature by utilizing pearlitic transformation latent heat so as not to form a martensitic metallographic structure.
  • substantially same effect is achieved as the conventional process annealing using a furnace.
  • Step material (or steel product) referred to in the invention is a steel material worked into a desired shape by working such as rolling, forcing or drawing.
  • "Semi-product steel material” referred to in the invention corresponds to "billet” in the JIS terminology and is a material to be formed into the above-described steel product by hot working.
  • “semi-product steel material” includes “slab”, “bloom”, “billet”, “sheet bar” or a circular billet having a diameter larger than 130 mm in the JIS terminology.
  • the packing rate is not less than 15%, the heat amount of the semi-product steel material is large enough and the time before recuperation is therefore shortened. As a result, the effect of reliably keeping the temperature within the range of the pearlite nose transformation completion point plus/minus 20°C can be obtained. Conversely, if the packing rate is lower than 15%, the amount of loaded material is small, which is disadvantageous in terms of economy. Since the heat amount of the material is small, the time taken before recuperation becomes long. Further, it may be necessary to improve the effect of thermally insulation of the vessel.
  • a preferable upper limit of the packing rate is 95%. If 100% is reached, the vessel is necessary to have the same size as that of pieces of the material, and there is no freedom in designing the size of pieces of the material, resulting in a low usability. It is, therefore, desirable to determine a preferable upper limit of 95%.
  • the process for producing a semi-product steel material according to the invention is effective for alloys belonging to the category of tool steel in JIS standard.
  • the process is particularly effective for alloys having a composition described below. Note that content of each element below is denoted by mass percent.
  • the reason for determine the carbon content to be 0.10 to 2.0% is as follows. Carbon may not be diffused into grains so that no carbides are precipitated in grains and pearlitic transformation does not generate as desired, if the carbon content is lower than 0.10 %. Preferably, the carbon content is not lower than 0.1%. If the carbon content exceeds 2.0%, the amount of carbides is in excess and the toughness is reduced. Preferably, the carbon content is 0.20 to 0.60%.
  • Silicon is added as a deoxidizer at the time of melting. If a large amount of silicon is added, the toughness is reduced. According to the invention, therefore, the silicon content is not less than 2.0%. Preferably, the content is 0.15 to 1.20%.
  • Manganese is added as a deoxidizer and desulfurizing agent at the time of melting. If a large amount of manganese is added, the toughness is reduced. According to the invention, therefore, the manganese content is not more than 2.0%. Preferably, the content is 0.30 to 1.00%.
  • Chromium increases the hardenability and improves the tensile strength and toughness. However, if a large amount of chromium is contained, the toughness is conversely reduced. According to the invention, therefore, the chromium content is 1.0 to 15.0%. Preferably, the content is 1.0 to 13.0%.
  • Molybdenum improves the hardenability. Also, molybdenum forms a fine carbide through tempering to increase the high-temperature tensile strength. However, if a large amount of molybdenum is contained, the toughness is conversely reduced. Therefore, the molybdenum content is not more than 10.0%. Preferably, the content is 0.20 to 5.0%.
  • Nickel, Vanadium, Tungsten and Cobalt described below are selective elements. One or more of them are contained.
  • Nickel increases the hardenability and improves the toughness. However, if a large amount of nickel is contained, the transformation point is lowered, so that the high-temperature strength is reduced. Therefore, if nickel is contained, the content is not more than 4.0%, preferably not more than 2.0%.
  • Vanadium makes crystal grains finer and increases the toughness. Vanadium forms a high-hardness carbonitride through tempering to increase the tensile strength. However, if a large amount of vanadium is added, the toughness is reduced. Therefore, if vanadium is contained, the content is not more than 4.0%, preferably 0.10 to 1.10%.
  • Tungsten increases the hardenability. Also, tungsten forms a fine carbide through tempering to form the high-temperature tensile strength. However, if a large amount of W is contained, the toughness is reduced. Therefore, if tungsten is contained, the content is not more than 4.0 %, preferably 0.10 to 1.10%.
  • Cobalt increases the red-heat hardness and increases the high-temperature tensile strength. However, if a large amount of cobalt is added, the toughness is reduced. Therefore, if cobalt is contained, the content is not more than 10.0%.
  • the balance being substantially Fe
  • the balance other than the elements specified above is substantially Fe.
  • impurities may be inevitably contained.
  • niobium and titanium are elements effective in making crystal grains finer, they may be contained in a range of not more than 0.20% such that the toughness is not disadvantageously reduced.
  • Aluminum is an element which makes diffusion of carbon faster and is effective in promoting precipitation of carbides during pearlitic transformation. Therefore, aluminum may be contained in a range of not more than 0.20%.
  • JIS SKD61 (steel No. 1), JIS SKT4 (steel No. 2) and JIS SKD11 (steel No. 3) were produced by melting in the atmosphere to obtain ingots having chemical compositions shown in Table 1.
  • Table 1 (mass%) No. C Si Mn Cr Ni Mo V balance JIS steels 1 0.40 1.0 0.4 5.0 - 1.4 0.7 Fe and inevitable impurities SKD61 2 0.55 0.2 0.8 1.2 1.6 0.3 0.1 Fe and inevitable impurities SKT4 3 1.50 0.2 0.4 11.7 - 0.8 0.2 Fe and inevitable impurities SKD11
  • the three ingots were hot-forged to obtain semi-product steel materials, and test pieces are taken to measure a pearlite nose transformation completion point.
  • Measurement of a pearlite nose transformation completion point on the semi-product steel material (JIS steel SKD61) having the chemical component No. 1 was performed as follows. Test pieces were heated to a hot forging temperature (1150°C), thereafter were introduced into furnaces at temperatures set every 25°C steps in a range from 700 to 775°C to be held for 2, 5, 15 and 24 hours. After the isothermal holding, the test pieces were taken out from the furnaces and cooled by air and the hardness thereof was measured. A point at which the hardness was reduced at the shortest-time holding was estimated as a pearlite nose transformation completion point. The pearlite nose transformation completion point of the semi-product steel material No. 1 was in the vicinity of a point at 750°C for 5 hours.
  • Measurement of a pearlite nose transformation completion point on the semi-product steel material (JIS steel SKT4) having the chemical component No. 2 was as follows. Test pieces were heated to a hot forging temperature (1150°C), thereafter were introduced into furnaces at temperatures set every 25°C steps in the temperature range from 600 to 750°C to be held for 2, 5, 10, 24 and 48 hours. After isothermal holding, the test pieces were taken out from the furnaces and cooled by air and the hardness was measured. A point at which the hardness was reduced at the shortest-time holding was estimated as a pearlite nose transformation completion point. The pearlite nose transformation completion point of the semi-product steel material No. 2 was in the vicinity of a point at 650°C for 10 hours.
  • Measurement of a pearlite nose transformation completion point on the semi-product steel material (JIS steel SKD11) having the chemical component No. 3 was as follows. Test pieces were heated to a hot forging temperature (1150°C), thereafter were introduced into furnaces at temperatures set every 25°C steps in the temperature range from 675 to 775°C to be held for 2, 5, 10 and 24 hours. After isothermal holding, the test pieces were taken out from the furnaces and cooled by air and the hardness was measured. A point at which the hardness was reduced at the shortest-time holding was estimated as a pearlite nose transformation completion point. The pearlite nose transformation completion point of the semi-product steel material No. 3 was in the vicinity of a point at 725°C for 2 hours.
  • process annealing was carried out by using the hot-forged semi-product steel materials having the chemical compositions Nos. 1 to 3.
  • the size of pieces of the hot-forged semi-product steel material A having the composition No. 1 was 430 mm (t) x 430 mm (w) x 3000 mm (1) x 2 pieces, and the weight thereof was about 8600 kg.
  • the size of the hot-forged semi-product steel material B having the composition No. 2 was 520 mm (t) x 830 mm (w) x 2400 mm (1) x 2 pieces, and the weight thereof was about 8000 kg.
  • the semi-product steel product No. A was subjected to hot forging at 1250°C (1 in Fig. 1 ), and then proceeded to the post-hot-working cooling step (2 in Fig. 1 ) in air.
  • Preparation for process annealing 3 was made during the post-hot-working cooling step by mounting the steel material 4 on heat insulation vessel base 5 as shown in Figs. 5A and 5B .
  • the maximum surface temperature of the semi-product steel was measured with a radiation thermometer and the steel material 4 was covered with insulation vessel upper lid 6 at 620°C, thereby completing introduction of the material 4 into the vessel 7.
  • the packing rate of the material in the vessel was 35.6%.
  • the temperature of the surface of the material was measured with a sheath thermocouple attached to the vessel. After heat recuperation to 800°C in the vessel (21 in Fig. 1 ), the semi-product steel material was held at the temperature within the pearlite nose transformation point plus/minus 20°C (730 to 770°C) for 5 hours to be transformed into pearlite (22 in Fig. 1 ). The material was then taken out from the vessel at 500°C (23 in Fig. 1 ) and cooled in air (24 in Fig. 1 ).
  • the semi-product steel product No. B was subjected to hot forging at 1250°C (1 in Fig. 1 ), and then proceeded to the post-hot-working cooling step (2 in Fig. 1 ) in air.
  • Preparation for process annealing 3 was made during the post-hot-working cooling step by mounting the semi-product steel material 4 on heat insulation vessel base 5 as shown in Figs. 5A and 5B .
  • the maximum surface temperature of the semi-product steel was measured with a radiation thermometer and the steel material 4 was covered with insulation vessel upper lid 6 at 600°C, thereby completing introduction of the material 4 into the vessel 7.
  • the packing rate of the material in the vessel was 33.2%.
  • the temperature of the surface of the material was measured with a sheath thermocouple attached to the vessel. After heat recuperation to 700°C in the vessel (21 in Fig. 1 ), the semi-product steel material was held at the temperature within the pearlite nose transformation point plus/minus 20°C (630 to 670°C) for 15 hours to be transformed into pearlite (22 in Fig. 1 ). The material was then taken out from the vessel at 500°C (23 in Fig. 1 ) and cooled in air (24 in Fig. 1 ).
  • the semi-product steel product No. C was subjected to hot forging at 1150°C (1 in Fig. 1 ), and then proceeded to the post-hot-working cooling step (2 in Fig. 1 ) in air.
  • Preparation for process annealing 3 was made during the post-hot-working cooling step by mounting the semi-product steel material 4 on heat insulation vessel base 5 as shown in Figs. 5A and 5B .
  • the maximum temperature of the semi-product steel surface was measured with a radiation thermometer and the steel material 4 was covered with insulation vessel upper lid 6 at 680°C, thereby completing introduction of the material 4 into the vessel 7.
  • the packing rate of the material in the vessel was 30.7%.
  • the temperature of the surface of the material was measured with a sheath thermocouple attached to the vessel. After heat recuperation to 850°C in the vessel (21 in Fig. 1 ), the semi-product steel material was held at the temperature within the pearlite nose transformation point plus/minus 20°C (705 to 745°C) for 4 hours to be transformed into pearlite (22 in Fig. 1 ). The material was then taken out from the vessel at 500°C (23 in Fig. 1 ) and cooled in air (24 in Fig. 1 ).
  • the semi-product steel materials used in the comparative examples had the same composition as those according to the invention, and the same hot forging conditions and the same sizes after hot forging as those according to the invention.
  • a conventional semi-product steel materials No. G is of a material according to JIS steel SKD61
  • No. H is of JIS steel SKT4
  • No. I is of JIS steel SKD11.
  • the conventional semi-product steel materials were subjected to the hot forging step 1, cooled by air (2 in Fig. 2 ), and introduced into a heating furnace (25 in Fig. 2 ), followed by the annealing step 3.
  • the steel material was heated to and held at a temperature not lower than the Ac3 point (26 in Fig. 2 ), completely transformed into austenite, and then slowly cooled to complete the process-annealing.
  • the dotted line in Fig. 2 indicates the Ac3 point.
  • the semi-product steel materials used in the comparative examples and those according to the examples of the invention had the same compositions, the same hot forging conditions and steel product sizes after hot forging.
  • the annealing temperature of not lower than the Ac3 point and the holding time for the semi-product steel material were 870°C x 5h for No. D, 750°C x 5h for No. E, and 870°C x 5h for No. F.
  • Table 2 shows the results of the metallographic structure and hardness of the semi-product steel materials of the examples according to the invention, the comparative examples and the examples of the conventional art after process annealing.
  • the holding times of the semi-product steel materials introduced into the heat insulation vessel at the temperature within the pearlite nose transformation completion point plus/minus 10°C were 2.5 hours for No. A, 7.5 hours for No. B, and 2 hours for No. C.
  • the semi-product steel materials Nos. D, E, and F according to the comparative example which are cooled at higher cooling rates and having passed on the shorter-time side of the pearlite nose transformation completion point have different metallographic structures from the semi-product steel materials Nos. A, B, and C to which the process annealing of the present invention was applied, and have higher hardnesses in comparison between corresponding materials.
  • process annealing can be performed without using a heating furnace.
  • a steel material of the present invention temperature is maintained by using pearlitic transformation latent heat from the steel material, thereby obtaining substantially the same effect as that of process annealing using a heating furnace, without making the metallographic structure a martensite. Therefore, according to the present invention, a steel material can be annealed, for example, by utilizing a time for transporting it on the sea or land, so that distribution of steel materials is facilitated and it contributes to energy saving.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)

Claims (6)

  1. Procédé de production d'un matériau en acier ayant un point d'achèvement de transformation de nez perlitique de pas moins de 30 minutes, le procédé comprenant :
    une première étape de déformation à chaud (1),
    une seconde étape de déformation à chaud, et
    un procédé de recuit (3) réalisé entre la première étape de déformation à chaud (1) et la seconde étape de déformation à chaud, le procédé de recuit (3) incluant les étapes :
    d'introduction d'un demi-produit de matériau en acier (4) dans un récipient d'isolation thermique (7) après la première étape de déformation à chaud (1),
    de récupération (21) de chaleur dans le matériau en acier (4), et
    de maintien (22) du demi-produit de matériau en acier (4) à une température dans une plage de point d'achèvement de transformation de nez perlitique plus/moins 20 °C avec une utilisation de chaleur latente de transformation provenant du demi-produit de matériau en acier (4) pour la transformation en perlite.
  2. Procédé selon la revendication 1, dans lequel la température du demi-produit de matériau en acier (4) introduit dans le récipient d'isolation thermique (7) est maintenue (22) à une température dans la plage du point d'achèvement de transformation de nez perlitique plus/moins 20 °C pendant pas moins de 2 heures.
  3. Procédé selon la revendication 1 ou 2, dans lequel la température du demi-produit de matériau en acier introduit dans le récipient d'isolation thermique (7) est maintenue (22) à une température dans une plage du point d'achèvement de transformation de nez perlitique plus/moins 10 °C pendant pas moins de 2 heures.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel une température de surface maximale du demi-produit de matériau en acier (4), lorsque le demi-produit de matériau en acier (4) est introduit dans le récipient d'isolation thermique (7), est dans une plage entre le point d'achèvement de transformation de nez perlitique plus 100 °C et le point d'achèvement de transformation de nez perlitique moins 200 °C.
  5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel le demi-produit de matériau en acier a un poids non inférieur à 500 kg.
  6. Procédé selon l'une quelconque des revendications 1 à 5, dans lequel le demi-produit de matériau en acier consiste en, en pourcentage en masse :
    0,10 à 2,0 % de C ;
    jusqu'à 2,0 % de Si ;
    jusqu'à 2,0 % de Mn ;
    1,0 à 15,0 % de Cr ;
    jusqu'à 10,0 % de Mo ;
    au moins l'un de jusqu'à 4,0 % de Ni ; jusqu'à 4,0 % de V, jusqu'à 20,0 % de W, et jusqu'à 10,0 % de Co ; et
    le reste étant sensiblement du Fe.
EP07741346.6A 2006-04-11 2007-04-10 Procédé de fabrication d'un acier Not-in-force EP2006398B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2006108174 2006-04-11
JP2006313747 2006-11-21
PCT/JP2007/057910 WO2007119722A1 (fr) 2006-04-11 2007-04-10 Procédé de fabrication d'un acier

Publications (3)

Publication Number Publication Date
EP2006398A1 EP2006398A1 (fr) 2008-12-24
EP2006398A4 EP2006398A4 (fr) 2013-06-19
EP2006398B1 true EP2006398B1 (fr) 2014-12-17

Family

ID=38609482

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07741346.6A Not-in-force EP2006398B1 (fr) 2006-04-11 2007-04-10 Procédé de fabrication d'un acier

Country Status (5)

Country Link
EP (1) EP2006398B1 (fr)
JP (1) JP5088633B2 (fr)
KR (1) KR101074297B1 (fr)
CN (1) CN101421424B (fr)
WO (1) WO2007119722A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009008285A1 (de) * 2009-02-10 2010-11-25 Gebr. Schmachtenberg Gmbh Stahllegierung
CN102560280A (zh) * 2011-12-30 2012-07-11 周子钦 一种耐高温高强度合金钢及其热处理工艺
US9758849B2 (en) * 2012-02-15 2017-09-12 Aktiebolaget Skf Bearing steel composition
DE102015113058A1 (de) * 2015-08-07 2017-02-09 Böhler Edelstahl GmbH & Co. KG Verfahren zum Herstellen eines Werkzeugstahles
CN108149151A (zh) * 2018-01-12 2018-06-12 安徽臣诺机器人科技有限公司 一种高强度工业机械臂合金铸件以及铸造工艺
JP6922759B2 (ja) * 2018-01-25 2021-08-18 トヨタ自動車株式会社 鋼部材の製造方法
US20200391288A1 (en) * 2018-02-23 2020-12-17 Hitachi Chemical Company, Ltd. Sintered valve guide and method for producing same

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57198209A (en) * 1981-05-27 1982-12-04 Daido Steel Co Ltd Annealing method of hot rolling material
JPH08260058A (ja) * 1995-03-27 1996-10-08 Daido Steel Co Ltd 鋼材の冷却方法
JPH11302725A (ja) * 1998-04-17 1999-11-02 Nippon Koshuha Steel Co Ltd 工具鋼の焼なまし方法
CN1169973C (zh) * 2001-06-11 2004-10-06 宝钢集团上海五钢有限公司 中合金铬系热作模具钢热处理方法
JP4277264B2 (ja) * 2003-05-13 2009-06-10 日立金属株式会社 高温強度特性に優れた工具部材およびその製造方法

Also Published As

Publication number Publication date
CN101421424B (zh) 2010-12-08
CN101421424A (zh) 2009-04-29
KR101074297B1 (ko) 2011-10-17
KR20080112287A (ko) 2008-12-24
WO2007119722A1 (fr) 2007-10-25
JP5088633B2 (ja) 2012-12-05
JPWO2007119722A1 (ja) 2009-08-27
EP2006398A4 (fr) 2013-06-19
EP2006398A1 (fr) 2008-12-24

Similar Documents

Publication Publication Date Title
US11001916B2 (en) Method for manufacturing a martensitic stainless steel part from a sheet
EP2824196B1 (fr) Procédé de fabrication d'un produit façonné à la presse et produit façonné à la presse
JP5423806B2 (ja) 高靱性耐摩耗鋼およびその製造方法
JP5458649B2 (ja) 高炭素熱延鋼板およびその製造方法
US20130160906A1 (en) Method for producing a motor vehicle component and motor vehicle component
EP3653736B1 (fr) Bande d'acier laminée à chaud et procédé de fabrication
JP4659142B2 (ja) 浸炭焼入れ性の優れた炭素鋼板およびその製造方法
EP2006398B1 (fr) Procédé de fabrication d'un acier
EP3222742A1 (fr) Barre en acier laminé ou matériau de fil laminé destiné à un composant forgé à froid
EP2801636A1 (fr) Tôle d'acier laminée à chaud à forte teneur en carbone et son procédé de production
CN108315637B (zh) 高碳热轧钢板及其制造方法
EP2801635B1 (fr) Tôle d'acier laminée à chaud à haute teneur en carbone avec une excellente trempabilité et une anisotropie minimale dans le plan et son procédé de production
EP3168319B1 (fr) Acier haute résistance faiblement allié pour formage à chaud de pièces de haute résistance et de limite élastique élevée
JPH09170017A (ja) 高強度高靭性鋼板の製造方法
KR102209555B1 (ko) 강도 편차가 적은 열연 소둔 강판, 부재 및 이들의 제조방법
EP3020841B1 (fr) Ressort hélicoïdal et procédé de fabrication de ce dernier
EP3298175B1 (fr) Acier raffiné en haute teneur de manganèse et haute résistance mécanique de troisième génération
KR102415764B1 (ko) 오스템퍼링 열처리 특성이 우수한 열연강판, 열연소둔강판, 부재 및 이들의 제조방법
JP7229827B2 (ja) 高炭素鋼板の製造方法
JPH08199309A (ja) 加工性の優れたステンレス鋼およびその製造方法
JPH08199310A (ja) 高強度マルテンサイト系ステンレス鋼部材の製造方法
WO2012172185A1 (fr) Procédé de fabrication d'un produit en acier à carbone moyen et produit en acier à carbone moyen laminé à chaud
EP3214189B1 (fr) Procédé de fabrication d'un tube sans soudure trempe et revenu pour ressort creux haute résistance
JP2016074951A (ja) 肌焼鋼の製造方法
KR100530068B1 (ko) 열처리특성이 우수한 자동차 보강재용 냉연강판과 그제조방법

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20081106

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE SI SK TR

RIN1 Information on inventor provided before grant (corrected)

Inventor name: EGUCHI, HIROTAKA

Inventor name: KATAOKA, HITOSHI C/O HITACHI METALS LTD

RIN1 Information on inventor provided before grant (corrected)

Inventor name: EGUCHI, HIROTAKA

Inventor name: KATAOKA, HITOSHI

DAX Request for extension of the european patent (deleted)
A4 Supplementary search report drawn up and despatched

Effective date: 20130522

RIC1 Information provided on ipc code assigned before grant

Ipc: C22C 38/00 20060101ALI20130515BHEP

Ipc: C21D 8/02 20060101ALI20130515BHEP

Ipc: C21D 6/00 20060101ALI20130515BHEP

Ipc: C21D 9/00 20060101AFI20130515BHEP

Ipc: C22C 38/58 20060101ALI20130515BHEP

Ipc: C21D 1/26 20060101ALI20130515BHEP

RIC1 Information provided on ipc code assigned before grant

Ipc: C22C 38/58 20060101ALI20140528BHEP

Ipc: C21D 8/02 20060101ALI20140528BHEP

Ipc: C21D 6/00 20060101ALI20140528BHEP

Ipc: C22C 38/00 20060101ALI20140528BHEP

Ipc: C22C 38/04 20060101ALI20140528BHEP

Ipc: C22C 38/02 20060101ALI20140528BHEP

Ipc: C22C 38/24 20060101ALI20140528BHEP

Ipc: C22C 38/22 20060101ALI20140528BHEP

Ipc: C21D 1/26 20060101ALI20140528BHEP

Ipc: C21D 9/00 20060101AFI20140528BHEP

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20140703

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE SI SK TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 701995

Country of ref document: AT

Kind code of ref document: T

Effective date: 20150115

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602007039699

Country of ref document: DE

Effective date: 20150219

REG Reference to a national code

Ref country code: SE

Ref legal event code: TRGR

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20150318

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20150417

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602007039699

Country of ref document: DE

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

26N No opposition filed

Effective date: 20150918

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20150410

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20150410

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150430

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150430

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150410

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 10

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150410

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: AT

Ref legal event code: UEP

Ref document number: 701995

Country of ref document: AT

Kind code of ref document: T

Effective date: 20141217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 11

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20070410

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20150417

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20141217

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 12

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20200312

Year of fee payment: 14

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20200331

Year of fee payment: 14

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20200415

Year of fee payment: 14

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20200325

Year of fee payment: 14

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 602007039699

Country of ref document: DE

REG Reference to a national code

Ref country code: SE

Ref legal event code: EUG

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 701995

Country of ref document: AT

Kind code of ref document: T

Effective date: 20210410

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210411

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211103

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210430

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210410