EP2430210A2 - Method for carbonitriding - Google Patents
Method for carbonitridingInfo
- Publication number
- EP2430210A2 EP2430210A2 EP10709725A EP10709725A EP2430210A2 EP 2430210 A2 EP2430210 A2 EP 2430210A2 EP 10709725 A EP10709725 A EP 10709725A EP 10709725 A EP10709725 A EP 10709725A EP 2430210 A2 EP2430210 A2 EP 2430210A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- phase
- carburizing
- nitriding
- nitrogen
- metal part
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/34—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in more than one step
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/20—Carburising
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/28—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in one step
- C23C8/30—Carbo-nitriding
Definitions
- the present invention relates to a process for carbonitriding at least one metal part.
- the document DE 199 09 694 A1 describes a carbonitriding process, in which the diffusion of nitrogen throughout the process or at
- Use of nitrogen as donor gas preferably takes place solely in the last process phase.
- DE 101 18 494 C2 describes a low-pressure carbonitriding process in which steel parts are first carburized and then with a
- Nitrogen donor gas to be embroidered Nitrogen donor gas to be embroidered.
- the document DE 103 22 255 A1 describes a method for carburizing steel parts in which nitrogen-emitting gas is added both during the heating phase and during the diffusion phase.
- the invention is therefore based on the object to provide a method for carbonitriding of metal parts, with which the tempering resistance and / or hardenability of a metal part can be improved and / or a depth of nitrogenation comparable to the carcass depth can be achieved.
- This object is achieved by the process according to the invention for carbonitriding at least one metal part in which the metal part is heated to a treatment temperature in a heating phase, embroidered with a nitrogen donor gas in at least one nitriding phase and carburized in at least one carburizing phase with a carbon donor gas and characterized in that the first nitriding phase begins after the completion of the heating phase and before the beginning of the first carburizing phase.
- the fact that the first nitriding phase begins only after the completion of the heating phase has the advantage that temperature gradients within the metal part or within a batch of several metal parts can be reduced and thus an inhomogeneous tempering resistance, hardness, strength and / or wear resistance within the metal part or within a batch of metal parts can be avoided.
- the fact that the first carburizing phase is started only after the start of the nitriding phase has the advantage that the nitrogen introduced into the surface of the metal part can diffuse into the metal part over the entire further treatment period and increase the tempering resistance, hardness, strength and Wear resistance in the edge zone contributes.
- the fact that the first carburizing phase starts only after the start of the nitridation phase involves nitrogen diffusion. accelerated carbon diffusion. This is because nitrogen atoms and carbon atoms can occupy the same interstices in the crystal lattice of the metal.
- a carburizing phase following a nitriding phase freed surface near-interstitial sites can be occupied by carbon atoms, thus making the effusion of nitrogen atoms and the associated nitrogen diffusion towards the surface more difficult.
- the nitrogen can be introduced by the early supply of nitrogen relatively, for example, up to 1, 5 mm or even up to 6 mm, deep into the surface layer of the metal part.
- an edge carbon concentration of ⁇ 0.3 mass% to ⁇ 0.7 mass% or even up to 1 mass%, and an edge nitrogen concentration of ⁇ 0.1 mass% to ⁇ 0.35 mass% or even from to to 0.5 mass percent can be achieved.
- the method according to the invention can be used for carbonitriding the edge layer of a metal part.
- the inventive method can also be used for carbonitriding of several metal parts.
- the method according to the invention can be used for carbonitriding one or more metallic workpieces.
- the metal of the metal part can be both a metal and a metal alloy, for example steel. - A -
- the first nitriding phase ends, in particular directly before the first carburizing phase or during the first carburizing phase or with the first carburizing phase or after the first carburizing phase.
- the nitrogen effusion can be reduced or prevented during further carburizing phases, further nitriding phases or diffusion phases.
- the method according to the invention can have at least one second nitriding phase. This can occur, for example, after the first carburization phase.
- the second nitriding phase may begin following the first carburizing phase.
- the method has a temperature equalization phase between the heating phase and the first nitriding phase, in which the treatment temperature for equalizing the temperature in the metal part or
- a constant atmosphere can be understood as meaning both a vacuum and a, preferably inert, gas atmosphere having a constant pressure and a constant composition.
- the temperature equalization phase subsequent to the heating phase may
- the first nitriding phase can in turn follow the
- Run off temperature equalization phase The temperature uniformity phase may, for example, last at least 5 minutes, in particular 30 minutes.
- a temperature equalization phase has the advantage that temperature gradients within the metal part or within a batch of several me-
- the treatment temperature can continue to be kept constant, in particular at the same treatment temperature as in the Temperatur fundamentalfahristspha- se. An increase or decrease in the temperature in a subsequent treatment phase is conceivable, however. 5
- the method is carried out in a, in particular evacuable, treatment chamber.
- the method has at least one diffusion phase in which the treatment chamber is evacuated and / or filled with an inert gas, for example argon.
- the first diffusion phase may, for example, be between the first nitriding phase and the first carburizing phase or between the first
- the method in addition to the first nitriding phase, has at least one further nitriding phase and / or at least one of the first carburizing phase
- a further carburizing phase and / or at least one further diffusion phase in addition to the first diffusion phase.
- the further nitriding phases and / or further carburization phases can take place both in particular directly, one behind the other, for example alternately, as well as partially or completely simultaneously.
- the carbon and nitrogen diffusion in the structure of the metal part can be advantageously increased.
- further diffusion phases can take place between the further nitriding phases and / or further carburizing phases.
- a further carburizing phase may take place during or subsequent to another nitriding phase.
- the nitrogen donor gas comprises a compound selected from the group consisting of ammonia, nitrogen and mixtures thereof, in particular amines. monia.
- the nitrogen donor gas may consist of a compound selected from the group consisting of ammonia, nitrogen and mixtures thereof, in particular ammonia.
- the carbon donor gas comprises a compound selected from the group consisting of acetylene, ethylene, propane, propene, methane and mixtures thereof.
- the carbon donor gas may be a compound selected from the group consisting of acetylene, ethylene, propane, propene, L-O methane, and mixtures thereof.
- the process is a low-pressure carbonitriding process.
- the treatment temperature is in a range of ⁇ 780 0 C to ⁇ 1050 0 C, in particular from ⁇ 780 0 C to ⁇ 950 0 C.
- a nitrogen donor gas partial pressure of less than 500 mbar for example less than 100 mbar, in particular less than or equal to 50 mbar, for example less than 20 mbar
- a carbon donor gas partial pressure of less than 300 mbar, in particular less than 20 mbar, for example less than 10 mbar may be present.
- nitriding the temperature for example, a
- the nitrogen concentration which is within a range of 850 0 C to 950 0 C adapted / increased; and / or the nitrogen supply, for example by increasing the nitrogen donor gas partial pressure, for example to 50 mbar or 30 mbar, and / or the nitrogen donor gas volume flow rate, for example to 3000 l / h, are increased.
- the nitrogen concentration for example to 50 mbar or 30 mbar, and / or the nitrogen donor gas volume flow rate, for example to 3000 l / h, are increased.
- the nitrogen concentration in a subsequent diffusion phase is now reduced due to nitrogen effusion and decreases, for example, to an edge nitrogen concentration of up to 0.5% by mass or, for example, 0.1% by mass to ⁇ 0.35% by mass, an increase in tempering resistance and Hardenability on the surface advantageously still be guaranteed.
- Another object of the present invention is a metal part, for example a metallic workpiece, in which the nitriding depth is greater than that
- Carburizing depth is.
- Such a metal part can be produced by a method according to the invention.
- the advantage here is that the component can have a deep-reaching support effect under mechanical stress at elevated operating temperatures.
- Another object of the present invention is a metal part, for example a metallic workpiece, produced by a method according to the invention.
- the nitriding depth may be greater than the carburizing depth.
- Fig. 1 shows a graph for schematically illustrating an embodiment of the method according to the invention.
- the method comprises a heating phase 1, a temperature equalization phase 4, four elevations. tion phases 2a, 2b, 2c, 2d, four carburization phases 3a, 3b, 3c, 3d and two diffusion phases 5a, 5b.
- FIG. 1 shows that, during the heating phase 1, the temperature is maintained continuously at a constant heating rate, up to a treatment temperature of approx
- the treatment temperature is kept constant at about 950 0 C.
- neither a nitrogen donor gas nor a carbon donor gas is supplied.
- a nitrogen donor gas for example ammonia
- a nitrogen donor gas partial pressure of about 50 mbar.
- the treatment temperature is kept constant at about 950 ° C., as in the following nitriding phases 2b, 2c, 2d, carburizing phases 3a, 3b, 3c, 3d and diffusion phases 5a, 5b.
- the first nitriding phase 2 a is followed by a first carburizing phase 3 a in which the nitrogen donor gas partial pressure is reduced again to 0 mbar and the carbon donor gas partial pressure is increased to about 10 mbar.
- the first carburization phase 3a is followed by a first diffusion phase 5a, in which the carbon donor gas partial pressure is lowered again to 0 mbar. This can be done, for example, by evacuating the treatment chamber or filling the treatment chamber with an inert gas.
- the first diffusion phase 5a is followed by a second carburizing phase 3b having a carbon donor gas partial pressure of about 10 mbar and a second nitriding phase 2b having a nitrogen donor gas partial pressure of about
- FIG. 1 shows that the second carburizing phase 3b and the second nitriding phase 2b start simultaneously. However, the second carburizing phase 3b is longer than the second nitriding phase 2b and thus ends only after the nitriding phase 2b. In the period in which both phases 2b, 3b proceed simultaneously, a carbon donor gas partial pressure of about 10 mbar and a
- Nitrogen donor gas partial pressure of about 50 mbar ago After completion of the second nitridation phase 2b, however, the nitrogen donor gas partial pressure is lowered to 0 mbar and the carbon donor gas partial pressure of about 10 mbar is maintained until the end of the second carburizing phase 3b.
- the second carburization phase 3b is followed by a second diffusion phase 5b in which the carburizing donor gas partial pressure is lowered again to 0 mbar.
- the second diffusion phase 5b in turn is followed by a third carburizing phase 3c with a carbon donor gas partial pressure of about 10 mbar.
- a carbon donor gas partial pressure of about 10 mbar Upon completion of the third carburizing phase 3c, the carbon donor gas
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102009002985A DE102009002985A1 (en) | 2009-05-11 | 2009-05-11 | Process for carbonitriding |
PCT/EP2010/053559 WO2010130484A2 (en) | 2009-05-11 | 2010-03-18 | Method for carbonitriding |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2430210A2 true EP2430210A2 (en) | 2012-03-21 |
EP2430210B1 EP2430210B1 (en) | 2018-01-24 |
Family
ID=42321146
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10709725.5A Active EP2430210B1 (en) | 2009-05-11 | 2010-03-18 | Method for carbonitriding |
Country Status (7)
Country | Link |
---|---|
US (1) | US20120103473A1 (en) |
EP (1) | EP2430210B1 (en) |
JP (1) | JP5930960B2 (en) |
CN (1) | CN102439194B (en) |
BR (1) | BRPI1014267A2 (en) |
DE (1) | DE102009002985A1 (en) |
WO (1) | WO2010130484A2 (en) |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102010028165A1 (en) * | 2010-04-23 | 2011-10-27 | Robert Bosch Gmbh | Process for the carbonitriding of metallic components |
CN102230151B (en) * | 2011-07-20 | 2015-10-21 | 新大洲本田摩托有限公司 | A kind of heat treatment process of metal workpiece |
FR2981948B1 (en) * | 2011-10-31 | 2014-01-03 | Peugeot Citroen Automobiles Sa | LOW PRESSURE CARBONITRURATION PROCESS WITH REDUCED GRADIENT TEMPERATURE IN AN INITIAL NITRIDATION PHASE |
FR2981947B1 (en) * | 2011-10-31 | 2014-01-03 | Peugeot Citroen Automobiles Sa | LOW PRESSURE CARBONITRURATION METHOD AT EXTENDED TEMPERATURE RANGE IN AN INITIAL NITRIDATION PHASE |
DE102013006589A1 (en) * | 2013-04-17 | 2014-10-23 | Ald Vacuum Technologies Gmbh | Method and device for the thermochemical hardening of workpieces |
FR3004731B1 (en) * | 2013-04-18 | 2016-05-13 | Peugeot Citroen Automobiles Sa | THERMO-CHEMICAL PROCESSING METHOD COMPRISING A SINGLE NITRIDING PHASE BEFORE CEMENTATION |
CN103361594A (en) * | 2013-08-07 | 2013-10-23 | 湖南特科能热处理有限公司 | Surface carburization and nitridation treatment method for steel workpiece |
FR3028530B1 (en) * | 2014-11-14 | 2020-10-23 | Peugeot Citroen Automobiles Sa | PROCESS AND PLANT FOR CARBONITRURING STEEL PART (S) UNDER LOW PRESSURE AND HIGH TEMPERATURE |
DE102015213068A1 (en) | 2015-07-13 | 2017-01-19 | Robert Bosch Gmbh | Process for nitriding a component |
CN105420663B (en) * | 2015-11-20 | 2018-07-10 | 贵州师范大学 | A kind of surface treatment method of titanium alloy compound carbonitriding |
JP6759842B2 (en) * | 2016-08-15 | 2020-09-23 | トヨタ自動車株式会社 | Steel manufacturing method |
DE102018222387A1 (en) | 2018-12-20 | 2020-06-25 | Robert Bosch Gmbh | Process for carbonitriding a metal part and metal part |
FR3132720A1 (en) | 2022-02-11 | 2023-08-18 | Skf Aerospace France | Method of strengthening a steel part by carbonitriding |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS60165370A (en) * | 1984-02-07 | 1985-08-28 | Ishikawajima Harima Heavy Ind Co Ltd | Nitriding treatment of stainless steel |
JPH0324258A (en) * | 1989-06-20 | 1991-02-01 | Koyo Seiko Co Ltd | Surface hardening treatment of carburized steel parts |
DE4208848C2 (en) * | 1991-12-04 | 2001-08-30 | Ald Vacuum Techn Ag | Process for the thermochemical after-treatment of steels and metals |
EP0707661B1 (en) * | 1994-04-22 | 2000-03-15 | Innovatique S.A. | Method of low pressure nitriding a metal workpiece and oven for carrying out said method |
JP3960697B2 (en) * | 1998-12-10 | 2007-08-15 | 株式会社日本テクノ | Carburizing and carbonitriding methods |
DE19909694A1 (en) | 1999-03-05 | 2000-09-14 | Stiftung Inst Fuer Werkstoffte | Production of carbonitrided edge layers in a low pressure carburization process comprises enriching the edge layers with nitrogen at the end of the process using molecular nitrogen as donor gas |
DE10118494C2 (en) | 2001-04-04 | 2003-12-11 | Aichelin Gesmbh Moedling | Process for low pressure carbonitriding of steel parts |
JP2003050321A (en) * | 2001-08-06 | 2003-02-21 | Mitsubishi Cable Ind Ltd | Optical fiber and method for manufacturing the same |
AU2002221138A1 (en) * | 2001-12-13 | 2003-06-23 | Koyo Thermo Systems Co., Ltd. | Vacuum carbo-nitriding method |
DE10322255B4 (en) | 2003-05-16 | 2013-07-11 | Ald Vacuum Technologies Ag | Process for high temperature carburizing of steel parts |
JP4255877B2 (en) * | 2004-04-30 | 2009-04-15 | 株式会社アライドマテリアル | High-strength and high recrystallization temperature refractory metal alloy material and its manufacturing method |
JP2007046088A (en) * | 2005-08-09 | 2007-02-22 | Yuki Koshuha:Kk | Nitrided quenched part, and method for producing the same |
JP2008106875A (en) * | 2006-10-26 | 2008-05-08 | Nsk Ltd | Large-sized rolling bearing |
CN101186992B (en) * | 2006-11-16 | 2010-11-17 | 有限会社结城高周波 | Nitrizing quenching product and its preparation method |
-
2009
- 2009-05-11 DE DE102009002985A patent/DE102009002985A1/en not_active Withdrawn
-
2010
- 2010-03-18 US US13/319,314 patent/US20120103473A1/en not_active Abandoned
- 2010-03-18 CN CN201080020682.2A patent/CN102439194B/en active Active
- 2010-03-18 BR BRPI1014267A patent/BRPI1014267A2/en not_active IP Right Cessation
- 2010-03-18 WO PCT/EP2010/053559 patent/WO2010130484A2/en active Application Filing
- 2010-03-18 JP JP2012510179A patent/JP5930960B2/en not_active Expired - Fee Related
- 2010-03-18 EP EP10709725.5A patent/EP2430210B1/en active Active
Non-Patent Citations (1)
Title |
---|
See references of WO2010130484A2 * |
Also Published As
Publication number | Publication date |
---|---|
BRPI1014267A2 (en) | 2016-04-12 |
CN102439194A (en) | 2012-05-02 |
CN102439194B (en) | 2014-07-23 |
US20120103473A1 (en) | 2012-05-03 |
JP2012526203A (en) | 2012-10-25 |
JP5930960B2 (en) | 2016-06-08 |
WO2010130484A3 (en) | 2011-01-13 |
DE102009002985A1 (en) | 2010-11-18 |
EP2430210B1 (en) | 2018-01-24 |
WO2010130484A2 (en) | 2010-11-18 |
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