squirts and details from polyvinylchloride.

Data about plasma nitriding of RAMAX S steel are not found [1, 2, 3 , 4, 5, 6, 7]. The aim of the present work is to investigate the influence of the process of nitriding in low-temperature plasma over the total thickness of the nitrided layer, the thickness of the combined zone, the surface hardness, heat resistance and impact strength of RAMAX S tool steel.

RAMAX S - STEEL NITRIDING IN LOWTEMPERATURE PLASMA

Angel Petrov ZUMBILEV

2. METHODOLOGY OF THE INVESTIGATIONS 2.1. Materials under Investigation and Modes of Thermal Treatment and Ion Nitriding
RAMAX S steel was used for the investigations. The chemical

Abstract: The aim of the present work is to investigate the influence of the process of nitriding in low-temperature plasma over the total thickness of the nitrided layer, the thickness of the combined zone, the surface hardness, the heat resistance and the impact strength of RAMAX S (420 F, modified AISI ) tool steel. Several modes of ion nitriding are considered at constant pressure of the ammonia and at varying the time of treatment as well as the temperature of nitriding. The results show that after ion nitriding of RAMAX S steel at temperature of nitriding 500 0, pressure of ammonia in the chamber 400 and time of treatment 8h, the highest level of micro hardness HV0,1= 12000 Ma is obtained . It is also established that after nitriding in lowtemperature plasma the heat resistance increases, while the impact strength of the steel reduces by 12%. Key word: plasma, nitriding, RAMAX S tool steel

composition of the steel was studied by means of equipment for automatic analysis Spectrotest and the results are given in table 1. Test samples from the steel with sizes 20 20 10 mm and surface roughness of Ra = 0.63 m were produced. The test samples were thermally treated in a chamber furnace in air medium according to the modes, given in table 2. The samples were ion nitrided afterwards in the installation ION 20 according to the modes presented in table 3.

2.2. Metallographic Investigations

In order to establish the morphological characteristics of the nitrided layers metallographic analysis was carried out. For clearing out the structure and the thickness of the nitrided layers a microscope "Axioskop" was used and metallographic pictures were taken by means of it. The thickness of the nitrided layer was defined through the depth at which hardness equal to the core plus 500 MPa was obtained. Measuring the micro hardness of the nitrided samples was carried out by means of a micro-hardness meter "Shimadzu" with a load of 0.98N following the Vikers method. During the process of defining the heat resistance of the nitrided layer, the level of hardness of the additionally tempered samples was measured by the Vikers method with a load of 49.05N. The impact strength of the thermally treated and ion nitrided steel was defined by using standard samples with sizes of 55 5510 mm and a V-shaped opening. The test on impact threepoint sagging was done with a fly hammer 5003 with maximum energy of 150 J. 449

1. INTRODUCTION
The tools for material processing (prints, press moulds, nozzles, squirts, swages etc.) work under very heavy conditions and therefore the requirements towards the choice of the material for a particular tool are very high and they can be only satisfied by choosing steels with heightened content of carbide forming elements. One of these steels is RAMAX S (420 F, modified AISI), which is with heightened content of chromium (17%) and this fact determines this type of steel as corrossion-resistant. In most cases steel is delivered in thermally treated condition of hardness 32-35 HRC. In this condition it can be very well mechanically processed because of the heightened content of sulphur in its chemical composition. It is chiefly used for producing

Table 1. Chemical composition of the steel Chemical elements, weight percentage Steel RAMAX S 4 20 F - AISI Si Ni S V Mn

0,34 0,35

17,1

0,55

0,12

0,02

0,47

1,37

0,17

Table 2. Modes of preliminary thermal treatment Steel RAMAX S Hardening t ,0 1030 Cooling medium Oil Tempering t , 0 620 Cooling medium Air

Table 3. Modes of ion nitriding Tempersature of nitriding of the mode t nitrogen., 1 2 3 4 550 550 500 500

Ammonia pressure - NH3, 400 400 400 400

Time of treatment - , h 4 8 4 8

3. EXPERIMENTAL RESULTS AND DISCUSSION 3.1. Thermal Treatment of the Test Samples
The results from measuring the hardness of the test samples after hardening and tempering are given in table 4. Table 4. Hardness after preliminary thermal treatment Hardness , HRC Steel Hardening RAMAX S 52 Tempering 35

3.2. Ion Nitrided Test Samples

The maximum surface hardness HV0.1 and the total thickness of the nitrided layer - tot were defined through the in-depth measured micro hardness of the thermally treated and nitrided samples. The in-depth measured micro hardness remains nearly constant and sharply changes at the moment of transition into the main material (fig. 2a) The results from the investigation of the nitrided steel are given in table 5. Table 5. Results from the ion nitriding of the test samples of the tot t nitr NH3 HV0.1 mode from MPa h m table 3 60 10000 4 400 550 1 100 10100 8 400 550 2 50 9500 4 400 500 3 70 12000 8 400 500 4 On the basis of the results (table 3) and the metallographic analysis it becomes clear that under the first mode of nitriding of RX S steel (temperature of nitriding 5500, ammonia pressure 400 and time of treatment

The micro structure of RAMAX S steel after hardening and high temperature tempering is given by fig. 1 a. From the figure it can be seen that the structure of the bettered steel is fine-grained with grain rating 10-11, which ensures uniform distribution of nitrogen in depth and favorable flowing of the process of diffusion. 450

4h) a layer with thickness tot = 60 m and maximum micro hardness HV0.1 = 10000 MPa is obtained. It can be noted that at the same temperature of treatment and ammonia pressure but at prolonged time of detention 8h (the second mode, table 3), the total thickness of the layer increases tot = 100m and the micro hardness also increases a bit HV0.1 = 10100 MPa. The combined zone of the nitrided layer is probably very thin, since it cannot be seen by means of the metallographic microscope fig.1.b. After ion nitriding of RX S steel following the third mode (temperature of nitriding 5000, gas pressure 400 and time of treatment 4 h) the thickness of the nitrided layer is tot = 50m and the maximum micro hardness is HV0,1= 9500 Ma. Under this mode of treatment the total thickness of the layer is smaller than the one, obtained under the first mode of nitriding. This is due to the lower temperature of saturation of the steel with nitrogen (smaller coefficient of diffusion of the ammonia into the steel), as well as to the heightened content of alloying constituents (>19%) in the steel. Together with the increase in the time of treatment to 8h (the fourth mode, table 5) a nitrided layer with a higher total thickness tot = 70m and the highest maximum micro hardness HV0,1 = 12000 Ma than in all the other modes of nitriding is obtained. The high micro hardness is due to the lower temperature of saturation (5000), at which the process of diffusion of nitrogen in depth is impeded. This leads to satiating of the steel surface with nitrogen and forming thin lamellar nitrides (carbonitrides) of the alloying constituents (r, Mo, V) which are coherently connected to the matrix. At the higher temperatures (5500) of saturation with nitrogen this coherence is broken and hardness decreases. Under these two modes of nitriding (the third and the fourth) a very thin, broken and hardly noticeable white zone is observed fig. 1 b, c. The metallographic analysis of the test samples shows that for the chosen modes of ion nitriding the distribution of micro hardness at a definite distance from the surface remains approximately the same and suddenly drops in depth. This type of distribution of the micro hardness of the nitrided layer leads to an increase in the wear resistance and contact load resistance of the layer fig. 2a. In the nitrided layer of the steel rN is formed (Fig.4 ), which leads to reducing the corrosion resistance of the steel . From the results and the metallographic analysis it could be noticed that RX S steel can be well nitrided in low temperature plasma. Depending on the particular mode of treatment a nitrided layer with high level of hardness HV= 9500 - 12000 P, small total thickness tot = 60 -100m and not formed combined zone is obtained.

3.2.1. Heat resistance of the nitrided layer The heat resistance of the nitrided layer was defined after measuring the hardness (HV5) of the additionally tempered at different temperatures (5500, 6000, 6500, 7000, 7500) nitrided test samples. The four modes of additional tempering of the nitrided steel were with 4h duration of detention period. The heat resistance was found through the limiting temperature of additional tempering, at which within the period of 4h the same hardness of 5500 HV5 was retained. On the basis of the obtained results curves were drawn up in order to define the heat resistance of the nitrided layer through the hardness of the test samples (measured at room temperature) in dependence on the temperature of additional tempering fig. 2b. The results for the heat resistance of the nitrided test samples are given in table 6. From table 6 it can be seen that under the first and second modes of nitriding, conducted at the higher temperature of treatment, better results for the heat resistance of the nitrided layer are obtained. The highest heat resistance is observed at: Tnitr = 5500, = 400 , = 8 hours. This is due to the heightened content of alloying constituents (r, V, Mo) in the steel, which increase the solvability of the nitrogen in the hard solution and form at the higher temperature of nitriding a bigger amount of special nitrides with higher temperature of dissociation. It can be noted that the positive influence of the process of ion nitriding on the heat resistance of RAMAX S steel is related to the considerable amount of alloying constituents in the hard solution, the heightened resistance of the solution containing nitrogen, and the slow coagulation of the nitride and carbide particles, containing vanadium, molybdenum, chromium or manganese. It slows down the processes of softening the nitrided layer and determines the high value of its heat resistance. 3.2.2. Impact strength of ion nitrided samples The results obtained from testing the thermally treated and ion nitrided test samples to impact three-point sagging are given in table 7. From table 7 it can be noticed that after ion nitriding of RAMAX S steel, the impact strength of the nitrided samples reduces to 12%. It shows that the nitrided layer with its parameters (micro hardness, total thickness, thickness of the combined zone) formed this way, does not influence significantly the impact strength. A bigger reduction of the impact strength (12%) is observed 451

under the mode 2 (temperature of nitriding 550 0, ammonia pressure 400 and time of treatment 8h), which is due to the bigger thickness of the nitrided layer tot = 100m. The nitrided layer formed on the surface is with higher brittleness and higher module of elasticity than the basic

material [2,3,8]. The nitride (carbon nitride) precipitations in the diffusion zone of the nitrided layer are the concentrator of the pressures, which influences favorably on the formation and the propagation of the crack.

Table 6. Results for the heat resistance of the nitrided samples of the mode from table 3 1 2 3 4 Tnitr,

, 400 400 400 400

, h 4 8 4 8

HV0,1* Ma 10000 10100 9500 12000

tot * m 60 100 50 70

Heat resistance at 5500 HV5/ 4 h 715 730 650 720

550 550 500 500

Note: * - hardness and thickness of the layer before additional tempering Table 7. Results for the impact strength of nitrided of the mode from table 3 1. 2. 3. 4. Not nitrided sample tnitr, 550 550 500 500 , 400 400 400 400 , h 4 8 4 8 HV0,1 Ma 10018 10097 9460 12006 35HRC tot m 60 100 50 70 KCV, MJ/m2 0.28 0.26 0.29 0.28 0.30

Fig.1 Microstructure of RAMAX S steel after hardening and tempering - and after ion nitriding at: b - t = 5000, NH3 = 400 , = 4h; c- t = 5500, NH3 = 400 , = 8h 452

1200 1100 1000

Microhardness 10V 0,1, RAM AX S t = 550 0 = 400 t = 8h

1200 1000 800 600 400 200 0 RAMAX S t = 550 = 400 = 8h

800 700 600 500 400 300 200 100 0 0 15 30 45 60 75 90 105 120 135
Distance from the surface, m

Hardness x10 - HV5,Pa

900

550

650

730

750
o

Temperature of additional tempering,

Fig.2. Distribution of hardness in depth of the nitrided layer - , b Dependence between hardness and temperature of additional tempering

Fig.3. XRD analysis of nitriding steel 420F

4. CONCLUSIONS
4.1. It is proved that RX S steel can be nitrided in low-temperature plasma. Depending on the mode of treatment a nitrided layer with high micro hardness HV0,1= 9500 - 12000 P, low total thickness tot = 60 100m and not formed combined zone is obtained. 4.2. It is established that after ion nitriding of RAMAX S steel at temperature of nitriding 500 0, ammonia pressure 400 and time of treatment 8h, the highest micro hardness HV0,1= 12000 Ma is obtained. 4.4. It is established that after nitriding of RAMAX S steel in low-temperature plasma the impact strength reduces and, depending on the mode of treatment, it can reach 12%. 453 4.3. It is proved that the highest heat resistance of the nitrided layer (7300) is obtained at temperature of nitriding 550 0, ammonia pressure 400 and time of treatment 8h.

REFERENCES:
1. RAMAX S, Prehardened stainless holder steel, Tool Steel Facts, Uddeholm, 2001. 2. Buchkov D, Toshkov V., Ion nitriding, S., Technique, 1990. 3.Toshkov V., Theoretical and practical aspects of the process of nitriding iron and iron-carbon alloys in low temperature plasma, Thesis, Sofia, 1997. 4. Toshkov V., Nitriding in low temperature plasma, King, 2004. 5. Fisher-ChatterjeeP.,W.Eysell,u.a.,Nitrieren und Nitrocarburieren, Sindeifingen, Expert Verbag, 1994 6. Hocman R.F., Effects of Nitrogen in Metal Surfaces, Proceeding of an International Conference on Ion Nitriding, Cleveland, Ohio, USA 15-17, September 1989, pp 23-30. 7. Nitriding and Nitrocarburising, Contract Heat Treatment Association,Aston University, Birmingham, 1996. 8. Lozev M.,A.Zyumbyulev, V.Toshkov and L.Boev, Fracture mechanic of ion-nitrided steel. MaterialsScience, Volume 28, Number 2 \ March ,1993, pp116-119.

CORRESPONDENCE
Angel ZUMBILEV, Assoc. prof. Ph.D. Technical University of Sofia Plovdiv Branch, Tzanko Dustabanov Str. 25, Plovdiv, Bulgaria zumbilev@mail.bg

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