Nitration of machine parts with production of nanostructured surface ply and ply composition

FIELD: process engineering.

SUBSTANCE: invention relates to metallurgy. Parts are processed by quenching at 920-940°C, subjected to negative hardening with heating to 600-650°C for 2-10 hours and removal of decarbonised ply. Then, ion-plasma nitration is performed at 500-570°C, cathode voltage of 300-320 V, and current density of 0.20-0.23 mA/cm2. Ammonia with dissociation of 0-80% is used as a gas medium. Ammonia flow rate makes up to 20 dm3/h. Pressure in the chamber at cathode spraying makes 1.3-1.35 Pa and, at saturation, 5-8 GPa. This nitration is performed at cyclic temperature and ammonia dissociation variation. Note here that at the first half of described cycle temperature makes 570°C at maximum nitrogen potential. During second half, temperature decreases to 500°C while nitrogen potential is decreased owing to increase in ammonia dissociation to 40-80%. Note also that the number of said cycles should make at least 10. Nitrated part has surface ply containing diffusion ply with α-phase with nanosized incoherent alloying element nitrides that makes soft matrix. Besides, it has surface ply with hard inclusions composed by nanoparticles of ε-phase iron nitrides formed by local phase recrystallisation of iron nitride lattices. This results from cyclic temperature and ammonia dissociation variation.

EFFECT: higher wear resistance, longer life of kinetic friction parts made from above described material.

2 cl, 1 tbl, 2 dwg

 

The technical field

The invention relates to mechanical engineering, in particular to a method of nitriding of machine parts with obtaining nanostructured surface layer, the nanostructure state diffusion layers used to improve wear resistance of parts sliding friction units of alloys based on iron.

The level of technology

Known methods of chemical-heat treatment that can improve the wear resistance of steel parts and contains the operations of preliminary heat treatment and subsequent nitriding. Thus, the technical solution contained in (RF Patent No. 2291227, IPC C23F 17/00, C23C 8/26, C21D 1/72, publ. 10.01.2007), calls for before nitriding pretreatment, consisting of the following operations: normalizing, tempering, hardening, tempering, machining, stabilizing vacation, and then nitriding at a temperature of 530°C for 1.5 to 30 h and diazotoluene within 0,4 1,5 hours...This method allows to increase wear resistance and reduce the fragility of the near-surface layers of steel, however, the mechanical properties of the surface have a fairly large scatter (according to the description of the patent it is not less than 15%), and the process of nanostructuring in the diffusion zone does not occur. As a result, the improvement of wear resistance remains within the Ah, defined through the wear rate of the Ihnot more than Ih≈10-9.

There is also known a method of processing steel products in gaseous environment (Patent RF №2367716, IPC C23C 8/34, C23C 8/26, publ. 20.09.2009), including heating products to the saturation temperature of 450...780°C in an atmosphere of ammonia, followed by exposure to saturating gaseous environment, where as saturating the environment with a shutter speed using the air and ammonia, which are served separately, and the exposure of the products are performed alternately in air and then in an atmosphere of ammonia with the formation on the surface of a multilayer structure consisting of alternating between the layers of oxide and nitride phases of iron and the respective alloying elements.

However, the oxide layer has a low mechanical properties and low wear resistance, it reduces the overall effect of improving wear resistance.

The closest technical solution is a method of chemical-heat treatment described in (Patent RF №2367715, IPC C23C 8/34, C23C 8/26, publ. 20.09.2009). The main difference of this method is the use of air atmosphere for forming on the surface of the steel before nitriding layer of oxides. The sequence of operations in this way is as follows: heating in an inert atmosphere, the exposure at the attained temperature is ur in air atmosphere, exposure to saturating nitrogen-containing atmosphere to obtain a diffusion layer in the form of nanoparticles of nitrides of alloying elements.

The main disadvantage of this method is the presence of the oxide layer, which according to the authors of the present invention, the analog promotes the penetration of nitrogen into the steel and the formation of nanoparticles of special nitrides.

This way, nano-sized particles of nitrides. However, the resulting composite oxide-nitride layer is not effective - insufficient wear - improving the wear resistance is negligible within - the order of tens of percent.

Disclosure of inventions

The task of the invention is a significant improvement of wear resistance of the surface layers formed in the nitriding parts sliding friction units, and a corresponding increase in the durability of sliding friction units with the same composition of the surface layer.

The technical effect is achieved in that in the method of nitriding parts sliding friction units with obtaining nanostructured surface layer part is subjected to a preliminary heat treatment and subsequent nitriding. At the same time as the preliminary heat treatment using a tempering at a temperature of 920...940°C, subsequent high the vacation up to 600...650°C for 2...10 hours and removal of de-carbonized layer, and then spend a plasma nitriding process with the following parameters in the temperature range of 500 to 570°With: - the voltage at the cathode 300...320V; - current density of 0.20...0,23 mA/cm2; - the composition of the gas medium, the ammonia with the degree of dissociation from zero to 80%; - the consumption of ammonia to 20 DM3/h; - the pressure in the chamber at the cathode sputtering - 1,3 1,35...PA, at saturation - 5...8 GPA. Moreover, the nitriding is carried out in the mode of cyclic changes of temperature and degree of dissociation of ammonia in the first half of the cycle the temperature is 570°C at maximum nitrogen potential, but in the second half of the cycle, the temperature was lowered to 500°C, while the nitrogen potential is reduced by increasing the degree of dissociation of ammonia (40...80%), while the number of such cycles must be at least 10.

Detail of the friction slip with nanostructured surface layer includes a diffusion zone with nanoscale nitride inclusions, while considered nanostructured surface layer obtained by the proposed method contains a diffusion layer with an α-phase with nanoscale non-coherent nitrides of alloying elements, which forms a soft matrix, and the surface layer containing solid particles constituting the nanoparticles of iron nitrides : ε-phase generated by the phase of the local recrystallization p is setok nitrides of iron, which is provided by cyclic change of temperature nitriding and the degree of dissociation of ammonia.

List of drawings

Figure 1 shows the microstructure of the ε-phase in the upper part of the nitrided layer steel MOI: - svetlopoli image microdiffraction pattern. (d) dark-field image of the ε-phase in the reflex (110);

figure 2 - change in the wear rate nitrided steel MOA at sliding friction.

The implementation of the invention

The main difference of the proposed method of treatment is that there is a formation of a diffusion zone with nitrides of alloying elements having a non-coherent link with the matrix and the size 10...15 nm, and the surface layer, consisting of nanoparticles ε-phase of iron nitrides of Fe2-3N) of size 20...50 nm.

The nitriding is carried out in conditions of cyclic changes of temperature nitriding and supply of ammonia with different (from 0 to 80%) degree of dissociation, which allows the process to change the nitrogen potential of the gas environment.

As a result of this process of reception (Cycling) in the proposed solution the conditions for phase recrystallization of the nitrided zone and its formation in nanostructured state. On the first active stage of the cycle at a temperature of 570°C in flowing ammonia in the conditions is x high nitrogen capacity created a fairly thick (20...30 µm) nitride layer of the ε - and γ'-phases, phases of nitrides of iron and alloying elements formed by direct recrystallization of the α↔γ'↔ε. The second passive stage of the cycle, the temperature was lowered to 500°C. and for a time served dissociatively ammonia (degree of dissociation from 40 to 80%). A sharp decrease in nitrogen capacity caused the development of reverse transformation ε↔γ'. When the alternation of cycles, consisting of active and passive stages, grinding patterns nitride zone and the formation of surface nitriding steels surface layer of ε-phase in the nanostructured state.

The layer thickness of the ε-phase, the size of the crystals in it, and their hardness is substantially influenced by the temperature of the preliminary (before nitriding) high holidays. At one and the same mode of nitriding layer thickness ε-phase increases in proportion to the increase in the tempering temperature of 500 to 650°C. in Addition, the reduced nano-sized nitrides in this phase, increases their hardness and, consequently, increases its durability.

Plasma nitriding process, giving the possibility to adjust the parameters of the technological process, carried out under the following parameters in the temperature range of 500 to 570°C:

the voltage at the cathode 300 320...;

the current density of 0.20...0,23 mA/cm2;

the composition of the gas environment - ammonia varying degrees of dissoc the purpose (range from 0 to 80%;

the flow rate of the gas mixture to 20 DM3/h;

- pressure in the chamber at the cathode sputtering - 1,3 1,35...PA at saturation - 5...8 GPA.

Modes nitriding and parameters of the surface layer are shown in table 1.

Table 1
Modes of ion-plasma nitriding and parameters of the near-surface layer (surface and diffusion layers) were MOI.
The degree of dissociation of ammonia (number of cycles)Mode nitridingThickness
The temperature of vacation before nitriding, °CLong
ness, h
effective mmoverall, mmlayer ε-phase, mcm
0↔60% (10)650300,23-0,260,40-0,4526-28
0↔80% (5)600150,21-0,240,36-0,406-8
0↔80% (10)300,27-0,290,44-0,468-12
0↔80% (16)480,32-0,340,52-0,5415-17
0↔80% (5)65015of 0.25 to 0.270,41-0,438-10
0↔80% (10)300,31-0,330,46-0,4812-15
0↔80% (16)480,36-0,380,61-0,6516-18

The rationale for the number of cycles contained in the table, where it is shown that the thickness of the nanostructured layer (layer ε-phase) may be not less than 10 μm when the number of cycles of at least 10, and provides the necessary wear resistance of the surface layer.

The nitrided layer has a layered and multi-phase structure. It is accepted that the work surface should have a structure which Assenova nitrogen solid solution with particles of nitrides of alloying elements. Surface nitride zone nitrided layer in the form of the ε-phase is traditionally removed by grinding details. Meanwhile, the results of the studies indicate that when certain established authors modes of ion-plasma nitriding layer ε-phase is formed in the form of nanocrystalline particles.

The formation of the ε-phase in the nanostructured state is confirmed by x-ray diffraction and electron microscopic studies. Used a special technique of moving the x-ray beam. Shooting at a small angle to the analyzed surface was provided information about the structure of the thin layer of ε-phase. Physical broadening of x-ray lines clearly demonstrated that the ε-phase is nanocrystalline with crystals size from 20 to 50 nm, which is confirmed by the results of transmission electron microscopy (figure 1).

First it is shown that the basis for the creation of nanoscale structures is phase recrystallization: ε↔γ'↔α phase nitrided layer, a driving force which is changing during the process, the nitrogen capacity of the gas environment.

The mechanism of recrystallization causes the formation of nuclei of crystals of the new phase within the existing (old) phase. Solid-phase local recrystallization of lattices nitri the s iron based on the simultaneous nucleation and growth of five "doubles" on stable nitrogen atom icosahedral clusters. In conditions of cyclic change the value of the nitrogen potential of developing multiple phase recrystallization and the surface is formed nanostructured nitride layer with a crystal size of 50 nm.

It is important that the nanostructured layer is formed directly on the surface of the hardened parts during the nitriding process. This is a significant advantage of the phase recrystallization as a way of intensive grinding of grain and increase the wear resistance of sliding friction units.

Experience of experimental research shows that in the diffusion zone formed a special nitride (nitride alloying elements). Depending on the technology parameters of these nitrides have a coherent, poluchennuyu and incoherent communication with the matrix, their size has a nanometer scale. They provide a strengthening effect and correspondingly increased durability.

The authors found that the greatest effect of improving wear resistance of material couples the sliding friction provide nitrides, no coherent or polutoraletnej connection with the matrix, i.e. incoherent nitrides of alloying elements. This effect is the effect of nanocrystalline surface layer (ε-phase), which represents an increase of wear resistance n is 2 orders of magnitude (100 times). When this diffusion zone with incoherent particles plays the role of a soft substrate for solid particles ε-phase, which creates favorable conditions for the process of deformation by friction with a minimum level of destruction.

Conducted long-term tests of pairs of sliding friction. Set that layer ε-nitride, located in the nanocrystalline state, has the practical effect of bezsennosc. Weight loss of the samples with a layer of ε-phase is at the limit of sensitivity of the recording equipment. As an example, figure 2 shows the kinetic curves of wear diffusion zone with non-coherent nitrides of alloying elements and the surface layer, consisting of ε-phase, when the sliding friction with the average relative sliding speed v=0,19 m/s and pressure in contact with p=10 MPa (line 1 - wear diffusion zone containing a special nitride (nitride alloying elements), incoherent with the matrix, line 2 - the wear of the surface layer above the diffusion zone and consisting of ε-nitride (Fe2-3N) in the nanocrystalline state.

It is seen that the wear layer of nanocrystalline ε-phase two orders of magnitude lower. Calculations show that even durability only this layer is sufficient to ensure the endurance of many of sliding friction units, including cervical shafts, to lucky camshafts, plunger pairs, injector of diesel engines.

Thus, the technical result of the proposed solutions reduce the wear rate of parts sliding friction units two orders of magnitude (100 times). The method can be used in the composition of the set of processing operations in the manufacture of machine parts involved in the sliding friction and prone to wear.

Therefore, the combination of a number of known characteristics, namely the conduct of the pre-nitriding heat treatment (high holidays), and then ion-plasma nitriding with the cyclic change of the mode, temperature and nitrogen potential of the gas environment allows you to get a new synergetic effect, consisting in the formation of a diffusion zone with non-coherent nitride and the surface layer with particles of ε-phase (Fe2-3N) in the nanocrystalline state and multiple (2) improving the wear resistance of the parts being processed.

1. Method of nitriding parts sliding friction units with obtaining nanostructured surface layer comprising a pre-heat treatment and subsequent nitriding parts, characterized in that as a preliminary heat treatment using a tempering at a temperature of 920-940°C, the subsequent high-temperature tempering up to 600-650°C during the course the e 2-10 hours and removal of de-carbonized layer, then spend a plasma nitriding process in the temperature range 500-570°C when the voltage at the cathode 300-320 B, current density of 0.20-0.23mm mA/cm2when used as a gas environment of ammonia with the degree of dissociation from zero to 80%, the flow rate of ammonia to 20 DM3/h, the pressure in the chamber at the cathode sputtering 1,3-1,35 PA, at saturation 5-8 GPA, while the nitriding is carried out in the mode of cyclic changes of temperature and degree of dissociation of ammonia in the first half of the cycle the temperature is 570°C at maximum nitrogen potential, but in the second half of the cycle, the temperature was lowered to 500°C, with nitrogen capacity reduced by increasing the degree of dissociation of ammonia up to 40-80%, while the number of cycles mentioned should not be less than 10.

2. Detail of the friction slip with nanostructured surface layer containing a diffusion zone with nanoscale nitride inclusions, characterized in that the surface layer obtained by the method according to claim 1, in fact the nanostructured surface layer includes a diffusion layer with an α-phase with nanoscale non-coherent nitrides of alloying elements, which forms a soft matrix, and the surface layer containing solid particles constituting the nanoparticles of iron nitrides : ε-phase generated by the phase the th local recrystallization gratings of iron nitrides, which is provided by cyclic change of temperature nitriding and the degree of dissociation of ammonia.



 

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