WO2014016251A2 - Method for producing at least one component and open-loop and/or closed-loop control device - Google Patents
Method for producing at least one component and open-loop and/or closed-loop control device Download PDFInfo
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- WO2014016251A2 WO2014016251A2 PCT/EP2013/065420 EP2013065420W WO2014016251A2 WO 2014016251 A2 WO2014016251 A2 WO 2014016251A2 EP 2013065420 W EP2013065420 W EP 2013065420W WO 2014016251 A2 WO2014016251 A2 WO 2014016251A2
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- 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
-
- 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
-
- 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
- C23C8/02—Pretreatment of the material to be coated
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- 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
- C23C8/32—Carbo-nitriding of ferrous surfaces
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- 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
- C23C8/80—After-treatment
Definitions
- the present invention relates to a method for producing at least one component and a control and / or regulating device according to the preamble of the independent claims.
- Patent DE 199 09 694 A1 describes a carbonitriding process in which the diffusion of nitrogen takes place during the entire process or, when elemental nitrogen is used as the donor gas, preferably only in the last process phase.
- Nitrogen donors are in particular molecular nitrogen, ammonia and other nitrogen-containing compounds. Carbon donors are not specified.
- the document DE 101 18 494 C2 describes a low-pressure carbonitriding process in which steel parts are first carburized and then embroidered with a nitrogen donor gas.
- Carbon donors are acetylene, propane and ethylene.
- a nitrogen donor donor gas containing ammonia is called. Further information on the nitrogen donor will not be provided.
- the document DE 103 22 255 A1 describes a method for carburizing steel parts, in which nitrogen-releasing gas is added both during the heating phase and during the diffusion phase.
- Ammonia and nitrous oxide are indicated as nitrogen donors and acetylene, propane and ethylene as carbon donors.
- the cited references DE 101 18 494 C2 and DE 103 22 255 AI describe low-pressure carbonitriding in the pulse mode in which nitrogen compounds, such as.
- nitrogen compounds such as.
- ammonia or nitrous oxide can be used as nitrogen donor gas, which can be used in the bidding phases between the carburizing offers and / or during heating of the batch and / or during the final carbon diffusion phase. be introduced chamber to introduce the nitrogen in the component surface.
- Diethylamine and dibutylamine are used as carbon and nitrogen donors to simultaneously introduce carbon and nitrogen into the component surface.
- the problem with this carbonitriding process is the high treatment temperatures of 1100 to 1200 ° C and the atmospheric pressure. At these temperatures, the conversion of amine compounds in the gas phase and on the component surface is so high that more complex geometries with internal surfaces such. B. holes, or densely packed component batches are carbonitrided unevenly. In addition, the process gas pressure of 1 bar complicates the diffusion of the donor gases within the batch and / or within internal geometries, such. B. blind holes, considerably.
- this temperature range in conjunction with the high process gas pressure, is to be assessed as very maintenance-intensive.
- low cost metallic materials tend to coarse grain at these temperatures, which can adversely affect the fatigue strength of the component, requiring the use of more expensive materials and / or an additional heat treatment step for grain refining.
- Another essential aspect is that no control is provided for controlling the carbon and nitrogen uptake in all of the described low-pressure carbonitriding processes.
- the ratio between the carbon and nitrogen introduced in the boundary layer is crucial for the resulting material and component properties. Disclosure of the invention
- the inventive method for producing at least one component and the control and / or regulating device according to the invention with the features of the independent claims have the advantage that in at least one treatment phase, a carbon emitting gas and a nitrogen-releasing gas are introduced simultaneously into the treatment chamber, that Depending on a predetermined ratio between a carbon and nitrogen concentration to be absorbed by at least one component in its boundary layer, a setpoint for the temperature and / or pressure to be set in the treatment chamber is determined and adjusted for a predetermined time in the treatment chamber. In this way it is possible to ensure a continuous carbon and nitrogen uptake. Carbon and nitrogen are offered simultaneously and thus without process gas exchange or diffusion phases between alternating carbon and nitrogen supply phases. This shortens the process times.
- the low-pressure carbonization also allows homogeneous carburizing and nitriding even in densely packed batches or complex component geometries, such.
- an amine compound is selected as such gas, preferably aliphatic monoamine as both primary, secondary and tertiary compounds, or aliphatic diamine or a mixture of both.
- a further advantage results when the gas emitting carbon and nitrogen is selected as a gas which releases carbon and nitrogen in a ratio of less than or equal to three. In this way, the desired ratios in the case of adjust fuel and nitrogen profiles while reducing soot formation in the furnace.
- the same advantage also results if, when using different gases for the discharge of carbon and nitrogen in the treatment chamber, the amount, in particular the volume flow, of the treatment chamber supplied carbon emitting gas and the amount, in particular the volume flow, of the treatment chamber supplied nitrogen donating gas is selected in proportion to the discharge of carbon and nitrogen in the treatment chamber smaller than three.
- the control is also particularly simple and comfortable designed that the actual value for the temperature is tracked to the setpoint for the temperature via a control of a heater in the treatment chamber, wherein the temperature of the heater is increased when the actual value for the temperature is less than that Setpoint for the temperature is and the temperature of the heater is lowered, if the actual value for the temperature is greater than the setpoint for the temperature.
- the regulation becomes correspondingly simple and comfortable when the actual value for the pressure is tracked to the desired value for the pressure via a setting of a gas quantity, in particular a volume flow, carried out from the treatment chamber, the gas quantity being reduced when the actual value for the pressure is lower than is the desired value for the pressure and wherein the amount of gas is increased when the actual value for the pressure is greater than the setpoint for the pressure.
- the setpoint for the temperature in the treatment chamber is changed at least once. This makes it possible to set different ratios between the carbon and nitrogen concentrations used in different depth zones of the surface layer.
- a further advantage results if at least one heating phase or at least one cooling phase in the treatment chamber is followed by a temperature equalization phase. In this way, the setpoint for the temperature can be adjusted as accurately as possible for all components within a batch. It is advantageous that the desired value for the pressure in the treatment chamber is changed at least once. This makes it possible to set different ratios between the carbon and nitrogen concentrations used in different depth zones of the surface layer.
- the target pressure in the treatment chamber is less than or equal to 100 mbar, preferably between two and 30 mbar.
- 650 ° C to 1050 ° C preferably in a range of 650 ° C to 960 ° C, is located.
- a homogeneous carbonitriding densely packed component batches or complex geometries with internal surfaces such.
- precipitates such as carbides, nitrides and carbonitrides in the surface layer of the at least one component can form unintentionally and uncontrolled as a function of the temperature and the carbon and nitrogen depth profiles that arise. It is therefore particularly advantageous in the method according to the invention for a plurality of treatment phases to be provided, which are separated from each other by a respective diffusion phase. That way you can
- unwanted precipitates such as carbides, nitrides and carbonitrides are avoided in the surface layer of the at least one component and also set a desired or predetermined carbon and nitrogen depth profile in the surface layer of the at least one component.
- Such a predetermined carbon and nitrogen depth profile can be produced particularly simply by selecting the predetermined ratio between the carbon and nitrogen concentration to be absorbed by at least one component in at least two of the treatment phases, depending on the given carbon and nitrogen depth profile in FIG the boundary layer of the at least one component.
- FIG. 1 shows a schematic representation of a plant for low-pressure carbonitriding at least one component
- Figure 2 shows the influence of temperature on the set in the boundary layer of a component ratio between carbon and nitrogen
- Figure 3 schematically a process control of a low-pressure carbonitriding with controlled temperature
- FIG. 4 schematically shows the construction of the surface layer of the treated components achieved by the process control according to FIG. 3
- FIG. 5 shows a block diagram of a control and / or regulating device used for process control.
- FIG. 1 shows a schematic representation of a plant 1 for Niederdruckcarbonitr Schlieren one or more components 2.
- five components 2 are shown by way of example.
- the components 2 are arranged on a support 3 in a treatment chamber 4.
- the components 2 can be heated by means of a heater 5 shown in the lower part of the drawing.
- An inlet 6 with associated flow control valve 7 allows the introduction of a carbon and nitrogen donor gas 8.
- a temperature sensor 9 and a pressure sensor 10 are arranged in the upper region of the drawing of the treatment chamber 4.
- a control and / or regulating device 11 shown above receives the signals coming from the temperature sensor 9 and the pressure sensor 10.
- An outlet 12 of the treatment chamber 4 leads to the inlet of a pump 13, which may be formed for example as a vacuum pump. Upstream of the pump 13, a throttle valve 14 is arranged in particular for pressure control.
- the carbon and the nitrogen donor gas 8 is simultaneously introduced into the treatment chamber 4 in various process phases by means of the flow control valve 7.
- the control and / or regulating device 11 monitors and controls or regulates the process or the individual process phases, inter alia, by means of the temperature sensor 9 and the pressure sensor 10.
- the temperature detected by the temperature sensor 9, which is also referred to below as the treatment temperature is important.
- the treatment temperature results in the atmosphere of the treatment chamber 4, as will be explained to the following figures 2 and 3.
- the pump 13 acts at the outlet 12 together with the throttle valve 14 as a valve.
- the degree of opening of the throttle valve 14 is controlled by the control and / or regulating device 11, inter alia, depending on the pressure detected by the pressure sensor 10, which is also referred to below as the treatment pressure to adjust the required treatment pressure in the treatment chamber 4, the treatment chamber 4 to evacuate partially or omit or replace the gases contained therein.
- the Heating device 5 is controlled by the control and / or regulating device 11, inter alia, as a function of the treatment temperature detected by the temperature sensor 9.
- the flow control valve 7 is guided by the control and / or regulating device 11 in order to regulate the process-dependent throughputs of the process gas.
- the carbon donor gas also referred to as carbon donating gas
- the nitrogen donor gas also referred to as nitrogen donating gas
- Mixed ratio of the treatment chamber 4 are supplied.
- known gases can be selected.
- the carbon donor gas for example, acetylene, propane or ethylene.
- the nitrogen donor gas for example, ammonia or nitrous oxide.
- the process gas composition for the treatment chamber 4 is adjusted via the gas quantities of the carbon-emitting gas and the nitrogen-releasing gas.
- one and the same gas is selected for the carbon donor gas and for the nitrogen donor gas, for example an amine compound, preferably aliphatic monoamine as both primary, secondary and tertiary compounds, or aliphatic diamine or a mixture of both. This considerably facilitates the process management. A mixing chamber upstream of the flow control valve 7 or an additional flow control valve is not required in this case.
- Pressure base alternatively only on temperature or only on pressure basis, so that only one of the two sensors is required.
- FIG. 2 shows the influence of the treatment temperature on the introduced carbon and nitrogen in the edge zone of the components 2, at a distance from the component surface of 50 ⁇ m after a carbonitriding time of 20 minutes at a set treatment pressure of the dispenser gas dimethylamine (C2H 6 NH) of 10 mbar
- FIG. 2 shows, for the two temperatures 800 ° C. and 850 ° C., by way of example the experimentally determined influence of the treatment temperature on the ratio of carbon and nitrogen concentration set in the boundary zone of the components 2.
- the two temperatures were selected for presentation to illustrate the change in ratios of the amount of carbon and nitrogen taken up.
- the absorbed nitrogen quantity while more carbon is absorbed for the same process duration and a temperature of 850 ° C.
- FIG. 3 exemplarily shows a time course of treatment temperature and treatment pressure, also referred to as process gas pressure, during low-pressure carbonitriding.
- process control of a low-pressure carbonitriding with controlled temperature is shown schematically, which is used for example in the plant 1 shown in Figure 1 application.
- the process time t is shown on the abscissa of the diagram, the temperature T on the left ordinate, and the pressure p of the atmosphere in the treatment chamber 4 on the right ordinate.
- the low-pressure carbonitriding comprises a heating phase A, two temperature equalization phases Bl, B2, two carbonitriding phases Cl, C2, two diffusion phases Dl, D2, a temperature change E and a cooling phase F.
- An interruption on the abscissa indicates that the illustrated process phases are not each time must have drawn, but may also differ from the illustration of Figure 3.
- FIG. 3 shows that, during a heating phase A, the temperature is increased continuously with an approximately constant heating rate up to a treatment temperature of approximately 950 ° C. by means of the heating device 5.
- the heating device 5 is controlled accordingly by the control and / or regulating device 11 and the heating rate ⁇ / ⁇ regulated.
- the treatment temperature is constant to a first setpoint for the temperature of about 950 ° C by the control and / or regulating device 11 by comparing the temperature measured by means of temperature sensor 9 with the first setpoint for the temperature controlled by 950 ° C by appropriate control of the heating device 5.
- currency During the heating phase A and the first temperature equalization phase B, no carbon or nitrogen-emitting gas is supplied to the treatment chamber 4.
- first treatment phase Bl first treatment phase also referred to as the first carbonitriding phase Cl
- the treatment temperature remains adjusted to its first setpoint.
- a carbon and nitrogen donating gas also referred to as carbon and nitrogen donor gas, for example methylamine
- the treatment pressure is constant at a first setpoint value for the pressure of about 15 mbar by the control and / or regulating device 11 by comparing the pressure measured by pressure sensor 10 with the first setpoint value for the pressure of 15 mbar adjusted by appropriate control of the opening degree of the throttle valve 14.
- the first setpoint for the treatment temperature and the first setpoint for the treatment pressure is determined in the control and / or regulating device 11 depending on the experimentally determined relationships described above by means of corresponding stored maps to a first predetermined ratio between the absorbed carbon and nitrogen amount for To obtain the components 2 in the edge zone. Due to the selected first treatment time Atl of the first carbonitriding phase Cl, the amount or penetration depth of the carbon and nitrogen introduced into the components 2 is determined according to the first predetermined ratio.
- a first treatment time characteristic map is stored in the control and / or regulating device 11, which for the selected setpoint of the treatment temperature and the selected setpoint for the treatment pressure and the material composition of the components 2 - an experimentally or computationally determined relationship between the treatment time and describes the introduced into the components 2 carbon and / or nitrogen amount or penetration depth of the carbon and nitrogen in the boundary layer. All components 2 treated in the treatment chamber should have the same material composition in order to achieve the desired result with regard to the carbon and nitrogen concentration to be introduced.
- the first carbonitriding phase C1 is optionally followed by a first diffusion phase D1, in which the treatment chamber 4 is evacuated by the control and / or regulating unit 11 by means of the pump 13 with the flow control valve 7 closed by corresponding control of the throttle valve 14 and the flow control valve 7 with an inert gas, z. B. nitrogen or argon is purged, which then instead of the Carbon and nitrogen donor gas is supplied via the flow control valve 7 of the treatment chamber 4 and pumped out by the pump 13 again.
- a temperature change phase E for changing the treatment temperature to a second desired value of about 850 ° C. by corresponding activation of the heating device 5 in order to set the final ratio between carbon and nitrogen in the surface layer of the components 2 in this embodiment.
- the treatment temperature is constant to the second setpoint for the temperature of about 850 ° C by the control and / or regulating device 11 by comparing the measured temperature by means of temperature sensor 9 with the second setpoint for the temperature of 850 ° C by appropriate control of Heater 5 regulated.
- no carbon or nitrogen-emitting gas is supplied to the treatment chamber 4.
- the treatment temperature is further adjusted to its second setpoint.
- a gas emitting carbon and nitrogen for example methylamine, is supplied to the treatment chamber 4 via the flow control valve 7.
- the treatment pressure is constantly adjusted to a second desired value for the pressure of about 10 mbar by the control and / or regulating device 11 by comparing the pressure measured by pressure sensor 10 with the second desired value for the pressure of 10 mbar by appropriate control of the flow control valve 7 ,
- the second setpoint for the treatment temperature and the second setpoint for the treatment pressure is determined in the control and / or regulating device 11 depending on the experimentally determined relationships described above by means of corresponding stored maps to a second predetermined ratio between the absorbed carbon and nitrogen amount for To obtain the components 2 in the edge zone.
- the amount or penetration depth of the introduced into the components 2 carbon and nitrogen is determined according to the second predetermined ratio.
- a stored in the control and / or regulating device 11 second treatment duration map is used, depending on the selected setpoint treatment temperature and the selected setpoint for the treatment pressure and the material composition of the components 2 - - determined experimentally or computational relationship between the treat - duration and the addition of carbon and / or nitrogen in the components 2 or starting from the achieved in the first Carbonitrierpahse Cl penetration depth feasible additional penetration depth of the carbon and nitrogen into the boundary layer describes.
- the first treatment duration characteristic field can also be used instead of the second treatment duration characteristic diagram.
- the treatment chamber is adjusted to a temperature by the lowered second setpoint for the treatment temperature compared to the first carbonitriding phase Cl in the second carbonitriding C2, at which the nitrogen absorbed by the components 2 nitrogen content and the absorbed by the components 2 carbon content smaller becomes.
- the ratio between the amount of carbon and nitrogen taken up by the components 2 is also shifted in favor of the nitrogen due to the lower treatment pressure in the second carbonitriding phase C 1 shown in the exemplary embodiment in the second carbonitriding phase C 2.
- the second carbonitriding phase C2 may also be without a second one
- Temperature equalization phase B2 connect directly to the temperature change phase E.
- the amount of carbon and nitrogen taken up in the first carbonitriding phase Cl lies in a second zone 110 of the boundary layer 125 which is more widely spaced from the surface of the components 2 than the amount of carbon and nitrogen taken up during the second carbonitriding phase C2, which in one case reaches the second zone 110 adjacent and on the other hand by the surface 100 of the respective component 2 completed first zone 105 of the edge layer 125 is present, as Figure 4 can be seen.
- the second treatment duration ⁇ 2 has been selected to be shorter than the first treatment period Atl. Therefore, the second zone 110 in the edge layer 125 of the components 2 is made thicker than the first zone 105.
- the first zone 105 has a first thickness d1 which is smaller than a second thickness d2 of the second zone 110.
- To the second zone 110 then, facing away from the first zone 105, joins a core 115 of the respective component into which no carbon or nitrogen has been taken up by the treatment.
- the transition between the two zones 105, 110 is ideally jump-shaped in FIG. However, in reality, there will be a steady transition region between the ratios of the corresponding carbon and nitrogen concentrations of adjacent zones.
- a further diffusion phase D2 in which the treatment chamber 4 is evacuated or with an inert gas, for. As nitrogen or argon is purged. Finally, a cooling phase F.
- edge carbon concentration should be between 0.5 to 0.8 mass percent with an edge nitrogen concentration between 0.2 and 0.7 mass percent.
- one or more diffusion phases can optionally be inserted to avoid unwanted precipitations of carbides, nitrides and carbonitrides and / or to set a given carbon and nitrogen depth profile in the surface layer of the components 2 as described.
- the predetermined carbon and nitrogen depth profile indicates at what intervals from the surface of the components in the surface layer of the components which ratio should be present between the carbon and nitrogen concentration to be absorbed by the component in its boundary layer. For each of these zones of the boundary layer with individually predetermined ratio between carbon and nitrogen concentration, a corresponding carbonitriding phase is then provided as described above.
- the desired carbon and nitrogen concentration distribution in the surface layer of the components 2 is thus adjusted by a controlled temperature control and / or regulation of the dispensing gas pressure during the low-pressure carbonitriding and by a suitable choice of the times and the treatment periods of the carbonitriding phases.
- an advantage of the method according to the invention is that the process is carried out at low pressures of less than or equal to 100 mbar, advantageously between 2 and 30 mbar, whereby the accessibility of bore geometries for the uptake of carbon and nitrogen increases.
- the process gas pressure of the carbon and nitrogen donor gas is advantageously controlled within a deviation of + / ⁇ 8 mbar, even better within a deviation of +/- 3 mbar.
- Lower temperatures of less than or equal to 1050 ° C, advantageously less than or equal to 960 ° C and greater than or equal to 650 ° C, can be a homogeneous
- the maps described are developed from a simulation model that calculates the diffusion of nitrogen and carbon as a function of time, temperature, pressure and material composition.
- Figure 5 shows a block diagram of the control and / or regulating device 11 with the components which are provided for the control of the flow control valve 7, the opening degree of the throttle valve 14 and the heating device 5 for adjusting the carbonitriding phases.
- the degree of opening of the throttle valve 14, with the vacuum pump 13 running is adjusted in the manner by the control and / or regulating device 11, so that the treatment pressure in the treatment chamber 4 is regulated to the respective desired value.
- the control of the treatment pressure by means of appropriate adjustment of the opening degree of the throttle valve 14 takes place at the gas outlet from the treatment chamber 4 upstream of the pump 13 exceeds the measured by the pressure sensor 10 actual value of the treatment pressure the predetermined target value for the treatment pressure, then the throttle valve 14 by appropriate control on the part Control and / or regulating device 11 further open, so that the pump 13 can take a higher volume flow from the treatment chamber 4 and the actual value is lowered for the treatment pressure.
- the throttle valve 14 is closed further by corresponding control by the control and / or regulating device 11, whereby the volume flow which the pump 13 takes from the treatment chamber 4 is reduced and an increase in the actual value for the treatment pressure in the treatment chamber 4 is achieved.
- control and / or regulating device 11 as required, for example, for setting the heating phase A or the diffusion phases Dl, D2, are not shown for reasons of clarity and may be formed in a manner known to those skilled in the art.
- a user can enter several parameters for a desired treatment of the components 2 in the treatment chamber 4. Thus, it can predetermine one or more ratios between the carbon and nitrogen concentration to be absorbed by the components 2 in their boundary layer 125 by corresponding input.
- an assigned carbonitriding phase should be set in order to convert the predetermined ratio in the boundary layer 125.
- a carbonitriding phase is set for each ratio data record, in the chronological order of their input or numbering.
- a zone with the corresponding ratio of the carbon and nitrogen concentration in the boundary layer 125 is then formed for each ratio data set and therefore for each carbonitriding phase, the zones being assigned according to the chronological order of the input of the associated predetermined ratio and thus in the order of their numbering the surface 100 of the respective component 2 are formed.
- the first ratio data set sets the carbon and nitrogen concentrations with the greatest edge distance to the surface 100 of the respective component 2 and the last-applied data set the surface-closest carbon and nitrogen concentrations.
- the second zone 110 with the thickness d2 in the boundary layer of the component 2 was set with a first ratio data set and the first zone 105 with the thickness d1 with a second ratio data set.
- a desired amount or penetration depth should also be indicated, in other words an associated thickness of the associated zone.
- a first predetermined thickness data set in FIG. 5 is denoted by 225 and an nth predetermined thickness data set by 235.
- the totality of the thick data sets is marked 240.
- a temperature-pressure map 250 and the associated thickness data set the treatment duration map 255th supplied as input.
- the temperature-pressure characteristic field was determined experimentally and gives for each predetermined at its input ratio between the 2 to be absorbed by the components in their boundary layer 125 carbon and nitrogen concentration a target value ST for the associated treatment temperature and a target value SD for the associated treatment pressure his exit.
- the setpoint value ST for the treatment temperature and the setpoint value SD for the treatment pressure are also supplied as input variables to the treatment duration characteristic map 255.
- the setpoint value ST for the treatment temperature is also supplied as input to a first comparison element 265.
- the setpoint SD for the treatment pressure is also supplied as input to a second comparator 260.
- a material composition for example.
- the insert steel 20MnCr5 is further selected from a proposed amount, which characterizes the material composition of the components 2.
- a material composition data set 245 is generated, which is likewise fed to the treatment duration characteristic map 255 as an input variable.
- the treatment duration map 255 was also determined experimentally and indicates what treatment time is required to with a component of the selected material composition at the predetermined setpoint ST for the treatment temperature and the predetermined setpoint SD for the treatment pressure, the predetermined thickness of the zone to be formed with absorbed carbon and nitrogen according to the predetermined ratio of the carbon and the nitrogen concentration in the peripheral layer 125 of the respective component 2 to form.
- a corresponding release signal is sent to the flow control valve 7, so that it is open during the determined treatment time for the associated carbonitriding phase.
- the flow control valve 7 is closed or is only for possibly provided diffusion phases for purging with an inert gas, eg. For example, nitrogen or argon, opened in the skilled person known manner.
- the first comparison element 265 is supplied with an actual value IT for the treatment temperature, which is determined by the temperature sensor 9.
- the first comparison element 265 compares the setpoint value ST of the treatment temperature with the actual value IT of the treatment temperature and outputs a control signal to the heating device 5 as a function of the difference between the setpoint value ST for the treatment temperature and the actual value IT for the treatment temperature in order to minimize the control difference and the actual value IT for the treatment temperature to track the setpoint ST for the treatment temperature.
- the second comparison element 260 is supplied with an actual value ID for the treatment pressure, which is determined by the pressure sensor 10.
- the second comparator 260 compares the setpoint value SD of the treatment pressure with the actual value ID of the treatment pressure, and outputs a control signal to the throttle valve 14 depending on the difference between the setpoint value SD for the treatment pressure and the treatment pressure actual value ID, in order to minimize the control difference and the actual value Tracking the ID for the treatment pressure the setpoint SD for the treatment pressure.
- the respective predetermined ratio between the carbon concentration and the nitrogen concentration in the boundary layer 125 of the respective component 2 in the desired thickness in the corresponding zone is set for the determined treatment duration. If a plurality of such ratios are specified, a carbon and nitrogen depth profile in the boundary layer 125 predetermined by the ratio data sets 205,..., 215 and the thickness data sets 225,..., 235 is then determined by the assigned and optional carbonitriding phases separated by a respective diffusion phase set.
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- 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)
- Fuel-Injection Apparatus (AREA)
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/416,280 US20150176114A1 (en) | 2012-07-24 | 2013-07-22 | Method for Producing at least One Component and Open-Loop and/or Closed-Loop Control Device |
IN10406DEN2014 IN2014DN10406A (en) | 2012-07-24 | 2013-07-22 | |
BR112015000822A BR112015000822A2 (en) | 2012-07-24 | 2013-07-22 | method for manufacturing at least one element and one regulating and / or controlling device |
CN201380039402.6A CN104471100B (en) | 2012-07-24 | 2013-07-22 | Method and control and/or adjusting means for manufacturing at least one component |
JP2015522120A JP6101350B2 (en) | 2012-07-24 | 2013-07-22 | Method for manufacturing at least one component and open-loop control and / or closed-loop control device |
EP13741715.0A EP2877607B1 (en) | 2012-07-24 | 2013-07-22 | Method for producing at least one component and open-loop and/or closed-loop control device |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102012212918.9A DE102012212918A1 (en) | 2012-07-24 | 2012-07-24 | Method for producing at least one component and control and / or regulating device |
DE102012212918.9 | 2012-07-24 |
Publications (2)
Publication Number | Publication Date |
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WO2014016251A2 true WO2014016251A2 (en) | 2014-01-30 |
WO2014016251A3 WO2014016251A3 (en) | 2014-05-08 |
Family
ID=48875018
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2013/065420 WO2014016251A2 (en) | 2012-07-24 | 2013-07-22 | Method for producing at least one component and open-loop and/or closed-loop control device |
Country Status (8)
Country | Link |
---|---|
US (1) | US20150176114A1 (en) |
EP (1) | EP2877607B1 (en) |
JP (1) | JP6101350B2 (en) |
CN (1) | CN104471100B (en) |
BR (1) | BR112015000822A2 (en) |
DE (1) | DE102012212918A1 (en) |
IN (1) | IN2014DN10406A (en) |
WO (1) | WO2014016251A2 (en) |
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SU1680798A1 (en) | 1989-09-21 | 1991-09-30 | Нижегородское станкостроительное производственное объединение | Method of steel article nitrocarburizing |
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 |
DE10322255A1 (en) | 2003-05-16 | 2004-12-02 | Ald Vacuum Technologies Ag | Carburizing steel parts with a carbon dispenser gas within an evacuated chamber comprises feeding a nitrogen-releasing gas, e.g. ammonia, into the treatment chamber during the heating-up phase and during the diffusion phase |
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JPS5096436A (en) * | 1973-12-27 | 1975-07-31 | ||
CH593346A5 (en) * | 1974-02-07 | 1977-11-30 | Ciba Geigy Ag | |
US4196233A (en) * | 1974-02-07 | 1980-04-01 | Ciba-Geigy Corporation | Process for coating inorganic substrates with carbides, nitrides and/or carbonitrides |
JPH0254752A (en) * | 1988-08-16 | 1990-02-23 | Demutetsuku Kk | Method for nitriding structural steel and cast iron |
JP3548918B2 (en) * | 1995-05-16 | 2004-08-04 | Ntn株式会社 | Rolling bearing |
DE19719225C1 (en) * | 1997-05-07 | 1998-08-06 | Volker Dipl Ing Leverkus | Method and apparatus for controlling a nitriding or nitro-carburising atmosphere |
US6991687B2 (en) * | 2001-07-27 | 2006-01-31 | Surface Combustion, Inc. | Vacuum carburizing with napthene hydrocarbons |
AU2002218508A1 (en) * | 2001-11-30 | 2003-06-17 | Koyo Thermo Systems Co., Ltd. | Method and apparatus for vacuum heat treatment |
JP2005120404A (en) * | 2003-10-15 | 2005-05-12 | Nsk Ltd | Gas carburization method, gas carbonitriding method, and surface treatment device |
JP2005264270A (en) * | 2004-03-19 | 2005-09-29 | Honda Motor Co Ltd | Crankshaft |
JP4264082B2 (en) * | 2005-12-08 | 2009-05-13 | Ntn株式会社 | Carbonitriding method, machine part manufacturing method and machine part |
EP2360287B1 (en) * | 2005-12-08 | 2013-08-07 | NTN Corporation | Method of gas carbonitriding, process for producing machine part and machine part |
JP2007197812A (en) * | 2005-12-28 | 2007-08-09 | Honda Motor Co Ltd | Soft-nitrided non-heat-treated steel member |
JP4191745B2 (en) * | 2006-04-07 | 2008-12-03 | Ntn株式会社 | Carbonitriding method, machine part manufacturing method and machine part |
CN101698929B (en) * | 2009-11-06 | 2012-07-25 | 江南工业集团有限公司 | Pressurized gas nitrocarburizing method |
DE102010001936A1 (en) * | 2010-02-15 | 2011-08-18 | Robert Bosch GmbH, 70469 | Process for carbonitriding at least one component in a treatment chamber |
DE112010005929A5 (en) * | 2010-10-11 | 2014-01-02 | Ipsen International Gmbh | Method and device for carburizing and carbonitriding metallic materials |
-
2012
- 2012-07-24 DE DE102012212918.9A patent/DE102012212918A1/en not_active Withdrawn
-
2013
- 2013-07-22 US US14/416,280 patent/US20150176114A1/en not_active Abandoned
- 2013-07-22 EP EP13741715.0A patent/EP2877607B1/en active Active
- 2013-07-22 IN IN10406DEN2014 patent/IN2014DN10406A/en unknown
- 2013-07-22 BR BR112015000822A patent/BR112015000822A2/en not_active Application Discontinuation
- 2013-07-22 WO PCT/EP2013/065420 patent/WO2014016251A2/en active Application Filing
- 2013-07-22 CN CN201380039402.6A patent/CN104471100B/en active Active
- 2013-07-22 JP JP2015522120A patent/JP6101350B2/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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SU1680798A1 (en) | 1989-09-21 | 1991-09-30 | Нижегородское станкостроительное производственное объединение | Method of steel article nitrocarburizing |
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 |
DE10322255A1 (en) | 2003-05-16 | 2004-12-02 | Ald Vacuum Technologies Ag | Carburizing steel parts with a carbon dispenser gas within an evacuated chamber comprises feeding a nitrogen-releasing gas, e.g. ammonia, into the treatment chamber during the heating-up phase and during the diffusion phase |
Also Published As
Publication number | Publication date |
---|---|
CN104471100A (en) | 2015-03-25 |
EP2877607A2 (en) | 2015-06-03 |
JP6101350B2 (en) | 2017-03-22 |
IN2014DN10406A (en) | 2015-08-14 |
CN104471100B (en) | 2017-09-01 |
BR112015000822A2 (en) | 2017-06-27 |
DE102012212918A1 (en) | 2014-01-30 |
US20150176114A1 (en) | 2015-06-25 |
JP2015528061A (en) | 2015-09-24 |
WO2014016251A3 (en) | 2014-05-08 |
EP2877607B1 (en) | 2020-09-16 |
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