EP3322833B1 - Verfahren zum nitrieren eines bauteils - Google Patents

Verfahren zum nitrieren eines bauteils Download PDF

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Publication number
EP3322833B1
EP3322833B1 EP16733080.2A EP16733080A EP3322833B1 EP 3322833 B1 EP3322833 B1 EP 3322833B1 EP 16733080 A EP16733080 A EP 16733080A EP 3322833 B1 EP3322833 B1 EP 3322833B1
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EP
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Prior art keywords
component
nitrogen
phase
nitriding
process gas
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German (de)
English (en)
French (fr)
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EP3322833A1 (de
Inventor
Lothar Foerster
Thomas Krug
Jochen Schwarzer
Marcus Hansel
Thomas Waldenmaier
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Robert Bosch GmbH
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Robert Bosch GmbH
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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
    • C23C8/08—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
    • C23C8/26—Nitriding of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—Surface hardening
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02—Extraction of non-metals
    • C21D3/08—Extraction of nitrogen

Definitions

  • the present invention relates to a method for nitriding a component made of a metallic material.
  • nitriding inevitably creates a hard but brittle compound layer with a significantly higher nitrogen content in the areas closest to the surface. This layer can flake off, especially when there is notch loading, which can lead to failure of the component and consequential damage due to the particles released. To alleviate this problem, it is from the DE 102005049534 A1 known to subsequently remove the connecting layer electrochemically. This is not always possible with more complex component geometries.
  • the component is heated to at least 450 ° C. in a first nitriding phase, and a nitrogen-releasing process gas and / or process gas mixture is placed on its surface. This causes nitrogen to diffuse through the surface.
  • a nitrogen-releasing process gas and / or process gas mixture is placed on its surface. This causes nitrogen to diffuse through the surface.
  • an iron nitride-containing connecting layer is formed in the first nitriding phase.
  • the connecting layer is dissolved in a first breakdown phase by heat treatment.
  • the metallic material contains at least one further metallic element, and the nitrogen diffusing through the surface forms at least one special nitride with this further metallic element.
  • the method then has the additional advantage that the formation of these special nitrides is evened out.
  • the further metallic element can in particular be an alloy element of the metallic material.
  • the invention expressly relates not only to higher-alloyed materials, but also to low-alloyed and unalloyed materials.
  • the duration of the first nitriding phase, the temperature of the component during the first nitriding phase and / or the supply of nitrogen on the surface of the component during the first nitriding phase are advantageously chosen so that the connecting layer is at most 10 ⁇ m thick, preferably between 2 ⁇ m and 6 ⁇ m. This area is preferred in the sense that the actual nitriding is evened out, but no pore border is yet formed in the connecting layer due to the recombining of atomic to molecular nitrogen. These pores could not be subsequently removed by simply removing the iron nitride; they could only be removed by, for example mechanical or electrochemical, removal of the connecting layer.
  • the first breakdown phase is followed by a second nitration phase and a second breakdown phase.
  • the parameters of the second nitriding phase do not have to match the parameters of the first nitriding phase.
  • the parameters of the second breakdown phase do not have to match the parameters of the first breakdown phase.
  • Two (or more) nitriding phases with an intervening degradation phase have the advantage that overall a higher nitriding depth can be achieved without creating an excessively thick connecting layer at any point in time and thus, for example, forming a pore border.
  • the nitriding depth increases additively with each nitriding phase, while the thickness of the connection layer starts again at zero due to the previous degradation phase.
  • connecting layer about 100-200 nm thick, which can be detected under the X-ray microscope or by means of energy-dispersive X-ray spectroscopy (EDX), are correlated with early failures of the treated components.
  • the connecting layer initially formed is therefore advantageously so completely dissolved that it can no longer be seen at least in the light microscope. It is advantageously so completely resolved that its phase components through X-ray diffractometry (XRD) are no longer detectable. The dissolution can be observed in-situ by observing the phase proportions.
  • connection layer is completely dissolved.
  • the general functioning of the invention does not depend on how this is done in detail.
  • the connecting layer is dissolved by reducing the concentration of atomic nitrogen and / or a nitrogen-releasing process gas and / or by changing the composition of a nitrogen-releasing process gas mixture so that less nitrogen is offered for nitriding.
  • This measure can, for example, be carried out in one operation for a batch of a large number of different components which are in a disordered form as bulk material in a treatment chamber.
  • the process gas emitting nitrogen can in particular be ammonia.
  • a mixture of, for example, ammonia with nitrogen and / or hydrogen can also be used.
  • the nitrogen supply for the nitration can be changed without the pressure in the treatment chamber having to be changed.
  • the nitrogen supply on the component surface can also be reduced without changing the gas composition simply by further heating the component and / or the gas or gas mixture: the higher the temperature, the faster ammonia dissociates on the component surface and the faster atomic nitrogen diffuses from the component surface path.
  • the treatment chamber can advantageously be evacuated as an intermediate step in order to create defined conditions in the entire treatment chamber.
  • the component is advantageously further heated to no more than 1000 ° C., preferably to no more than 600 ° C., in order to dissolve the connecting layer. Above about 600 ° C, it is to be expected that the metallic material of the component will become austenitic due to the nitrogen placed on its surface. This is not desirable when nitriding because the component warps, its core too high tempered and / or its grid structure could be changed at the edge. Furthermore, many nitriding furnaces are limited to operating temperatures of up to approx. 700 ° C; At higher temperatures, the service life of the furnace materials can be greatly reduced, which can cause more warping. Niobium nitride and chromium nitride are examples of special nitrides that are temperature-resistant up to approx. 1000 ° C.
  • the inclusions from the special nitride which are responsible for the advantageous internal compressive stresses, are metastable.
  • the component temperature is therefore advantageously kept below the temperature at which inclusions from the special nitride spontaneously dissolve.
  • the residual compressive stresses then remain in the structure of the component.
  • the supply of atomic nitrogen on the component surface can in particular not only be reduced, but also completely reduced to zero, for example by evacuating the treatment chamber or simply placing an inert gas, such as molecular nitrogen or argon, on the component surface.
  • an inert gas such as molecular nitrogen or argon
  • the combination of the concentration of nitrogen and / or process gas or the composition of the process gas mixture on the one hand and the component temperature on the other hand is selected in a particularly advantageous embodiment of the invention from a map area in which diffusion of in Nitrogen bound to the connecting layer is driven out of the surface of the component.
  • the well-known teacher's diagram gives an example of the combinations of temperature, nitriding index and nitrogen supply at which an iron nitride layer forms or dissolves or whether the iron will transform into an austenitic structure.
  • the combination of the concentration of nitrogen and / or process gas or of the composition of the process gas mixture on the one hand and the component temperature on the other hand is advantageously selected from a characteristic map range in which the iron nitride of the connecting layer is thermodynamically is unstable.
  • the process that led to the formation of the connecting layer then preferably runs backwards.
  • the special nitride is thermodynamically stable in this map area. It is then retained in full.
  • the combination of the concentration of the nitrogen and / or process gas or the composition of the process gas mixture on the one hand and the component temperature on the other hand is selected from a map area in which the more strongly bound nitrogen in special nitrides remains in the surface of the component. Then the actual nitriding layer, which is decisive for the fatigue strength, is retained in its entirety, and only the connecting layer is formed back.
  • the component surface is oxidized in an additional oxidation phase before at least one nitriding phase and / or after at least one degradation phase.
  • This forms iron oxide, which improves the nitriding effect.
  • the degradation phase provided according to the invention is particularly advantageous in this embodiment with regard to the fatigue strength.
  • the process gases or process gas mixtures can, for example, be fed to the treatment chamber in a manner controlled by nitriding and / or oxidation and / or carbon. However, they can, for example, also be fed to the treatment chamber as a fixed amount of gas.
  • the general functioning of the invention does not depend on the process gases or process gas mixtures being supplied in a regulated manner.
  • the component can be nitrided and carburized at the same time thanks to the feed rate-controlled feed. This changes the structure of the connection layer.
  • the nitriding effect can be increased by feed controlled by the oxidation index.
  • Such a control is also advantageous if the component is made of steel that is highly alloyed with chromium.
  • the process is advantageously carried out under atmospheric pressure. Then the treatment chamber does not have to be pressure-resistant.
  • the method can also advantageously be used in low pressure, i.e. at a pressure lower than atmospheric pressure. Even with a small pressure difference, it is possible, for example, to prevent process gases from escaping from the treatment chamber in the event of a leak.
  • the mean free path for diffusion is greater at a lower pressure.
  • the process can, for example, also be carried out under plasma nitriding conditions with or without active screen support. This accelerates the nitration overall.
  • a process gas or process gas mixture that emits oxygen and / or carbon can also be added at any time in order to carry out nitrocarburization.
  • simulation models can be used that calculate the diffusion of nitrogen and the formation of special nitrides as a function of time, temperature and material composition. Otherwise, the process parameters can be fine-tuned in a known manner by making a series of test pieces and examining metallographic sections.
  • Whether a given component has been heat treated using the method according to the invention can show denitration at the nitriding temperature. Compared to a component that was nitrided from the outset without a compound layer, for example due to a reduced ammonia supply, less nitrogen will effuse from a component treated with the method according to the invention, since the concentration of unbound nitrogen atoms in the iron matrix already during nitriding due to effusion and diffusion in the Edge area is greatly lowered. How much nitrogen is effused can be determined, for example, by weighing the component by analyzing the Composition of the exhaust gas or by measuring the pressure increase in a temperature-controlled measuring chamber. In addition, the originally formed, later dissolved connecting layer can be demonstrated metallographically through a changed etching behavior.
  • Figure 1 shows an example of the process control for an embodiment of the method according to the invention.
  • the continuous curve denotes the course of temperature T over time t.
  • Sections A1 to F are defined along the time axis in which different activities take place.
  • the component 6 is first brought from room temperature to a temperature of 420 ° C.
  • the heating rate is constant.
  • the treatment chamber in which the process is carried out is filled with an inert gas, such as nitrogen or argon, at an overpressure of 20 to 100 mbar above atmospheric pressure.
  • the treatment temperature is kept constant at around 420 ° C.
  • no oxygen-containing process gas or nitrogen donor gas 7 is supplied.
  • the temperature equalization phase B1 is followed by a pre-oxidation phase C with an oxygen-containing process gas.
  • an oxygen-containing process gas For this purpose, air, nitrous oxide, synthetic air or a nitrogen-water vapor mixture is supplied isobarically to the treatment chamber.
  • an inert gas such as nitrogen or argon
  • the heating phase A2 is followed by the heating phase A2 at a constant heating rate until a treatment temperature of around 540 ° C. is reached.
  • the second temperature equalization phase B2 follows the heating phase A2.
  • the metallic components 6 contained in the treatment chamber are nitrided by a sufficiently high supply of ammonia, and a connecting layer V is formed.
  • the nitrogen supply is reduced by feeding an ammonia-nitrogen mixture or an ammonia-nitrogen-hydrogen mixture with a lower ammonia content isobarically to the treatment chamber.
  • This will bind the nitrogen in the Connection layer V thermodynamically unstable.
  • the nitrogen diffuses deeper into the component and forms special nitrides N there.
  • it also passes from the surface of the connecting layer into the atmosphere of the treatment chamber.
  • the connection layer is dissolved. The area of the component closest to the surface loses its hard, brittle character.
  • the nitrogen supply is increased again to the level of the nitration phase D1.
  • Further special nitrides are formed in the interior of the component, while a connection layer is formed again in the area closest to the surface. This is completely reduced in the subsequent breakdown phase E2, in which the nitrogen supply is again reduced to the level of the first breakdown phase E1.
  • an inert gas such as nitrogen or argon is fed to the treatment chamber to exchange the gas atmosphere isobarically. This ends the nitriding of the metallic components 6.
  • the treatment chamber and the metallic components 6 are then cooled to room temperature.
  • the division into two nitriding phases D1 and D2 with an interposed degradation phase E1 has the advantage that the connecting layer V does not reach an excessively great thickness in which it forms pores P. These would no longer have to be removed in the dismantling phase E1.
  • Figure 2 illustrates the comparison of a sample nitrided according to the state of the art ( Figure 2a ) with an according to the in Figure 1
  • the nitrogen donor gas 7 was presented in each case on the surface 8 of the component 6 made of the metallic material W.
  • the receding connection layer V shows a stronger etching behavior and therefore appears darker on microscopic photographs of metallographic sections.
  • the material of the in Figure 2 Outlined samples is X40CrMoV5-1, which, in addition to iron as the base metal, contains the following additional alloy elements in the following percentages by mass: carbon 0.39, silicon 1.10, manganese 0.4, chromium 5.20, molybdenum 1.40, vanadium 0.95.
  • Figure 3 shows a GDOES depth profile analysis of the in Figure 2 Components shown 6.
  • Curve a relates to the in Figure 2a sketched component 6.
  • Curve b relates to the in Figure 2b sketched component 6.
  • the nitrogen concentration n is shown in mass percent M% over the edge distance (depth) d in ⁇ m.
  • depth distance
  • the approximately 8 ⁇ m thick connecting layer is clearly closed detect.
  • the in Figure 2b sketched component 6 of the entire area near its surface 8 is nitrided very evenly. With increasing depth d, the nitrogen concentration n also converges in the component 6 according to FIG Figure 2a against the nitrogen concentration n in the component 6 according to FIG Figure 2b .
  • Figure 4 shows results of an endurance test of notched, cylindrical components 6 (tensile specimens) with regard to the fatigue strength. All components 6 were remunerated. Some of the components 6 were not further heat-treated, while the rest of the components 6 were nitrided. All components 6 in the clamping area were reworked before the tensile stresses. The notches were not reworked. Non-nitrided components 6, components 6 with an approximately 5 ⁇ m thick connecting layer V and components 6 with a less than 1 ⁇ m thick connecting layer V were tested.
  • the amplitude q of the stresses to which the components 6 were subjected is plotted in N / mm 2 over the number z of vibrations to which the components 6 were exposed.
  • the type of symbol indicates whether the component 6 passed the test (hollow symbol) or whether it failed (filled symbol).
  • the different symbol shapes indicate which sample the measurements relate to.
  • a square lying on its edge indicates a measured value that was obtained on a non-nitrided component 6.
  • a square standing on a point indicates a measurement point that was recorded on a component 6 with a 5 ⁇ m thick connecting layer V.
  • a circle identifies a measuring point that was obtained on a component 6 with a connecting layer less than 1 ⁇ m thick.
  • a compensation curve (1a, 2a, 3a) is laid through the measuring points, which indicates the combinations of voltage amplitudes q and repetition numbers z for which a failure probability of 50% is to be expected.
  • These compensation curves (1a, 2a, 3a) are each surrounded by dashed curves (1b, 2b, 3b) or (1c, 2c, 3c), which indicate the combinations of stress amplitudes q and number z of repetitions for which failure rates of 10% or 90% are to be expected.
  • Curves denoted by the number 1 relate to components 6 nitrided with a 5 ⁇ m thick connecting layer V.
  • Curves denoted by the number 2 relate to non-nitrided components 6.
  • Curves denoted by the number 3 relate to components 6 nitrided with a compound layer V which is less than 1 ⁇ m thick.
  • the letter a denotes the compensation curve that corresponds to a 50% failure probability.
  • the letter b denotes the curve that corresponds to the 90% probability of failure.
  • the letter c denotes the curve that corresponds to the 10% probability of failure.
  • the non-nitrided components 6 perform worst in relation to a failure probability of 50%.
  • the components 6 with a connecting layer V less than 1 ⁇ m thick show the highest stress amplitude that can be tolerated based on a failure probability of 50%.
  • the material of the in Figure 4 The samples examined is 50CrMo4, which, in addition to iron as the base metal, contains the following additional alloying elements in the following mass percentages: carbon 0.50, chromium 1.05, molybdenum 0.23.
  • Nitrided components 6 (circles as symbols, curves denoted by number 4) and other non-nitrided components 6 (squares as symbols, curves denoted by number 5) are compared with one another in an analogous manner using a method according to an exemplary embodiment of the invention.
  • the slope of curves 4a, 4b and 4c in the fatigue limit range is comparable to the slope of curves 5a, 5b and 5c.
  • curves 4a, 4b and 4c approximate curves 5a, 5b and 5c in the fatigue strength range. This means that one can speak of a comparable fatigue strength.
  • the voltage amplitude is increased by around 24% based on a failure probability of 50%.
  • the advantage of the method according to the invention manifests itself particularly in the fact that the scatter of the components 6 nitrided according to this method is similar in comparison with the non-nitrided components 6 and no early failures occur with small numbers z of load changes.
  • the material of the in Figure 5 The samples examined is 8CrMo16, which contains iron as the base metal and the following additional alloying elements in the following percentages by mass: carbon 0.09, chromium 3.90, molybdenum 0.50.

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  • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
EP16733080.2A 2015-07-13 2016-06-29 Verfahren zum nitrieren eines bauteils Active EP3322833B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015213068.1A DE102015213068A1 (de) 2015-07-13 2015-07-13 Verfahren zum Nitrieren eines Bauteils
PCT/EP2016/065124 WO2017009044A1 (de) 2015-07-13 2016-06-29 Verfahren zum nitrieren eines bauteils

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EP3322833A1 EP3322833A1 (de) 2018-05-23
EP3322833B1 true EP3322833B1 (de) 2020-08-12

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EP (1) EP3322833B1 (pt)
CN (1) CN107849678A (pt)
BR (1) BR112017028323A2 (pt)
DE (1) DE102015213068A1 (pt)
WO (1) WO2017009044A1 (pt)

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CN109338090B (zh) * 2018-11-30 2020-04-21 武汉钢铁有限公司 连续式退火炉脱碳渗氮装置
CN114182196B (zh) * 2021-12-02 2024-01-19 贵州师范大学 钛合金真空气体阶梯渗氮方法

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JP3495590B2 (ja) * 1997-06-30 2004-02-09 アイシン・エィ・ダブリュ株式会社 軟窒化処理を施した歯車並びにその製造方法
JP3303741B2 (ja) * 1997-09-25 2002-07-22 トヨタ自動車株式会社 ガス軟窒化処理方法
DE102005049534A1 (de) 2005-10-17 2007-04-19 Robert Bosch Gmbh Verfahren und Vorrichtung zur Bearbeitung eines Düsenkörpers für ein Kraftstoffeinspritzventil
DE102009002985A1 (de) 2009-05-11 2010-11-18 Robert Bosch Gmbh Verfahren zur Carbonitrierung
DE102009045878A1 (de) 2009-10-21 2011-04-28 Robert Bosch Gmbh Verfahren zum Steigern der Beanspruchbarkeit von Bauteilen aus Stahl unter zyklischer Belastung
JP2011235318A (ja) * 2010-05-11 2011-11-24 Daido Steel Co Ltd ダイカスト金型の表面処理方法
JP5656908B2 (ja) * 2012-04-18 2015-01-21 Ｄｏｗａサーモテック株式会社 窒化鋼部材およびその製造方法
JP6115140B2 (ja) * 2013-01-15 2017-04-19 株式会社ジェイテクト 摺動部材の製造方法およびクラッチプレートの製造方法

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BR112017028323A2 (pt) 2018-09-11
CN107849678A (zh) 2018-03-27
EP3322833A1 (de) 2018-05-23
DE102015213068A1 (de) 2017-01-19
WO2017009044A1 (de) 2017-01-19

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