SLOVAK UNIVERSITY OF TECHNOLOGY IN BRATISLAVA

FACULTY OF MATERIALS SCIENCE AND TECHNOLOGY IN TRNAVA

Institute of Materials Science

Report to dissertation thesis

SURFACE TREATMENT OF HIGH ALLOY TOOL STEEL

USING LASER TECHNOLOGY

for achieving academic title doctor

(philosophiae doctor, Ph.D.)

Ing. Mária ŠTEFÁNIKOVÁ

Study programme: materials engineering

Number and name of study branch: 5.2.26 materials

Trnava, June 2012

Dissertation thesis was compiled during day form of doctoral study at Institute of Materials
Science, Faculty of Materials Science and Technology in Trnava, Slovak University of
Technology in Bratislava (Slovakia) and at Department of Materials Technology, Faculty of
Mechanical Engineering in Ljubljana, University of Ljubljana (Slovenia)

Submitter: Ing. Mária ŠTEFÁNIKOVÁ

Institute of Materials, Department of Materials Engineering
Faculty of Materials Science and Technology in Trnava
J. Bottu 25, 917 24 Trnava (Slovakia)

Supervisor: A/Prof. Roman MORAVČÍK, PhD.

Institute of Materials, Department of Materials Engineering
Faculty of Materials Science and Technology in Trnava
J. Bottu 25, 917 24 Trnava (Slovakia)

Consultant: A/Prof. Roman ŠTURM, PhD.

Department of Materials Technology
Faculty of Mechanical Engineering in Ljubljana
Aškerčeva 6, 1000 Ljubljana (Slovenia)

Reviewers: Prof. Otakar BOKŮVKA, PhD.

University of Žilina, SjF, Univerzitná 1, 010 26 Žilina, SK

A/Prof. Martin KUSÝ, PhD.

STU MTF, J. Bottu 25, 917 24 Trnava, SK

Report was sent on: .........................................

Defence of dissertation thesis takes place on: ..................................................

in seminar room T-202 (Bottova campus), J. Bottu 25, 917 24 Trnava, Slovakia

Prof. Dr. Ing. Oliver MORAVČÍK

Dean of MTF STU in Trnava
LAYOUT

1 INTRODUCTION .............................................................................................................. 4
2 AIMS OF THE DISSERTATION THESIS ....................................................................... 5
3 EXPERIMENTAL RESULTS ............................................................................................ 6
3.1 Quasi-equilibrium phase transformations in K390 high alloy cold work tool steel ......... 6
3.2 Influence of HIP parameters on laser remelted surface ................................................... 7
3.3 Analysis of LSR K390 Microclean tool steel after various heat treatments .................. 10
4 CONCLUSION ................................................................................................................. 14
BIBLIOGRAPHY .................................................................................................................... 16
WORKS PUBLISHED ........................................................................................................ 17
ABSTRACT ......................................................................................................................... 19
SÚHRN ................................................................................................................................ 20

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1 INTRODUCTION

Continuous development, improvement of metallurgical processes, wide range of

production assortment and optimal solution for each part of industrial steel production
characterizes nowadays engineering practice.
Tools are manufactured from varying materials, however, tool steel occupies still
very important place among materials. Tool steels cover a wide range of composition
depending on type of tool and work technique. Also various mechanical, physical and
technological properties are demanded.
More and more, higher requirements for performance, lifetime and quality of tool
reflect in high demands for cleanness and uniformity of initial material. It can be achieved
only due to special technological procedure of steel production mainly represented by
powder metallurgy process. This production technique yields high-performance tool steels
with homogeneous carbide structure, high wear resistance, capacity to withstand high
pressure load while maintaining good grindability and polishability.
Except of suitably selected material and also technological procedure of production,
in particular heat treatment has influence for tool quality which makes possible to change
and modify properties of steel according to requirements of tool. However, attention
should be devoted also to a surface treatment of tools. One of this surface treatment is laser
remelting process which makes possible to improve material properties due to formation of
hard, homogeneous and ultrafine microstructure of the surface layer (due to dissolution
and/or redistribution of large carbides), without changing its chemical composition. The
properties of the modified layer depend on the microstructure prior to heat treatment and
on the amount of energy input transferred to the surface layer of the specimen. After that
the laser treated tool steels have generally a high level of hardness and wear, corrosive,
erosive and fatigue resistance. Laser remelting can harden alloys that cannot be hardened
as effectively by laser hardening. The laser remelting process attracts also commercial
interest because of its ability to alter with accuracy the properties of localized surface
regions without reprocessing the material as a whole. A big advantage of laser heat
treatment is that the desired microstructural changes can be achieved without the use of
cooling agents, thus allowing the workpiece surface to be kept clean. Other advantages for
practice include flexibility of treating small areas, leaving the other parts unaffected. Laser
processing is considered as one of the practical approaches to improve the damaged region.
This is because laser processing can simultaneously remove the cracks or defects and carry
out heat treatment.

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2 AIMS OF THE DISSERTATION THESIS

The dissertation thesis is focused on a laser surface remelting and its influence on
microstructure and phase composition. Based on literature survey and achieved
experimental results following aims of the dissertation thesis are defined.
First goal is to determine a phase transformations in K390 Microclean high alloy tool
steel during the quasi-equilibrium state. For fulfilment of this aim is needed to implement
the following partial experiments:
1. Differential thermal analysis measurements of phase transformations during slow
heating and cooling.
2. For more detail analysis of the phase transformations in solid state the dilatometry
and thermogravimetry devices are needed to use.
3. Sample obtained from differential thermal analysis must be analysed by light
microscopy and scanning electron microscopy. The chemical composition and
elements distribution will be measured using the energy dispersive X-ray
spectroscopy.
4. X-ray diffraction analysis will be used for determining the phase composition on
quasi-equilibrium samples.
Second main goal of dissertation thesis is comparison of the influence of different
laser parameters and various parameters of hot isostatic pressing on microstructure and
hardness measurements. This part is aimed at determination of optimal parameters of laser
surface remelting. For achieving this aim the following methods and analysis will be
carried out:
1. Sample preparation by hot isostatic pressing using various parameters.
2. Sample preparation using laser surface remelting at various parameters.
3. Light and scanning electron microscopical analysis of cross-sectioned samples.
4. Hardness measurements of different areas after laser surface remelting.
5. X-ray diffraction analysis of treated samples.
Third main aim of thesis is analysis of influence of heat treatment of samples before
surface laser remelting. Fulfilment of this goal needs to carry out following experimental
procedures:
1. Heat treatment of bulk samples: hardening (1150 °C), tempering at 200 °C or 200
and subsequent at 500 °C.
2. Laser surface remelting with equal parameters, however, in different conditions
(with and/or without pre-heating, post laser remelting heat treatment).
3. Microscopical analysis using the light and scanning electron microscopy.
4. Hardness measurements of significant areas of remelted surface.
5. X-ray diffraction analysis of the change of phase composition and phase amount
and determining lattice parameters using phase analyse.
Results of this dissertation thesis are the determination of suitability this material for
improving the surface layer of K390 Microclean cold work tool steel by means of laser
surface remelting.

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3 EXPERIMENTAL RESULTS

The investigated steel K390 Microclean is high alloy cold work tool steel produced
by powder metallurgy process. It is tool material with high wear resistant and toughness.
The microstructure of K390, in compare with the conventional technology production,
characterised uniform carbide distribution, small carbide size, uniform chemical
composition over the entire cross section and length and virtually isotropic behaviour due
to improved homogeneity and the segregation absence of harmful elements. This material
is used for various applications as blanking and punching tools, cold forming tools and
knives [1].
The chemical composition of K390 Microclean high alloy tool steel (Table 1) was
determined by means of SPECTRUMA GDA 750 glow discharge optical emission
spectrometer (GDOES) after calibration. The used parameters were following: voltage
1000 V, current 20 mA and Ar protective gas with 99.999 % purity.

Table 1 Chemical composition of K390 Microclean cold work tool steel in wt. %

C Si Cr Mo V W Co

2.34 ±0.03 0.53 ±0.01 4.01 ±0.05 3.84 ±0.01 8.66 ±0.07 0.82 ±0.01 1.30 ±0.01

3.1 Quasi-equilibrium phase transformations in K390 high alloy cold work tool steel

Aim of this experimental work is to describe the phase transformations in high

alloy cold work tool steel during slow heating and cooling. These conditions are different
compared to those used in production of the alloy steels, but they enable to describe the
solidification and phase transitions in quasi-equilibrium conditions. Some aspects
solidification of the high alloyed tool steels are describe in [2-6] The analysed high alloy
cold work tool steel shows the transition from ferromagnetic to paramagnetic state during
heating at temperature of 781 °C, Fig. 1. Then the transformation of ferrite to austenite at
temperature of 856 °C occurs. This temperature is higher than the temperature of ferrite to
austenite transition determined by dilatometry (832 °C), probably due to higher heating
rate at DTA measurements. Melting process of tool steel begins at temperature of 1209 °C
and continues in three steps. First step is probably the melting of molybdenum carbide
eutectics at temperature of 1209 °C. They are localised on the boundary of eutectic
colonies Melting of the material continues with vanadium carbide eutectic colonies and
melting is finished when the last amount of austenite is dissolved in the melt at temperature
of 1389 °C.
Also solidification of the material proceeded in three steps. In undercooled melt the
austenite grains grow at temperature of 1340 °C. Next, solidification continues by the
evolution of eutectic colonies based on the vanadium carbide (starts at 1327 °C).
Molybdenum is diffusing to the melt and in the last step of solidification the molybdenum
carbide eutectics at the boundaries are formed.

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 Fig. 1 DTA curve of the investigated high alloy tool steel during heating

The cooling in solid state shows only two transitions in thermogravimetry curve,
Fig. 2. The first change is the transition from paramagnetic to ferromagnetic state at
temperature of 780 °C and second one is the formation of the secondary carbides in the
matrix at temperature of 500 °C.

Fig. 2 Thermogravimetry curves

The knowledge about the phase transformations in high alloy cold work tool steel
can help in better understanding of processes occuring in material during the heat
treatment. The results can be useful for the next thermodynamic analysis of phase
transitions using the Thermocalc and Dictra software.

3.2 Influence of HIP parameters on laser remelted surface

The aim of this part thesis is analysis of HIP parameters and pre-heating
temperature before LSR of K390 Microclean high alloy cold work tool steel on
microstructure, hardness and roughness evaluation. The HIP process play important role in
the production process of cold work tool steel. The HIP parameters, and also size of
rapidly solidified powder particles, significantly influence the microstructure of the final
material thereby also mechanical properties. After HIP process using various parameters

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big particles keep their own original microstructure although slightly thermally modified.
Therefore on the base of obtained results and previous works which have shown that laser
surface remelting can be used to obtain chemically homogeneous structure in tool steels
and to eliminate the residual porosity of materials produced by powder metallurgy were
carried out laser surface remelting on samples after various HIP parameters process. In this
part of dissertation thesis are analysed two factors influencing of HIP parameters on
microstructure and hardness of laser remelted layer: 1. effect of pressure during constant
time and temperature and 2. effect of pressing time during constant press and temperature.
LSR was carried out on samples which were pre-heated at 200 and 350 °C in chamber
furnace, laser pre-heated and without pre-heating.
On the base of macro-pictures in all samples the change of HIP parameters (the
change of pressure and time) has not any visible influence on the LR surface. During the
LSR 50 % overlapping of laser spots was used. By means of macroscopy analysis micro-
cracks were observed on the LR surface of sample without pre-heating. Some of other
samples contain holes vaporisation by influence of too high temperature in the spot centre
due to pre-heating. The measured roughness does not show any considerable differences
among individual samples too. In some cases of sample areas insufficient overlapping was
observed which causes the change of roughness on the LSR.
By microscopical analysis following base zones were observed in cross-section
after LSR of each sample: laser remelted zone, heat affected zone and base material. In LR
zone Marangoni effect is visible. Regarding HAZ no noticeable changes were observed.
The microstructure of base material appears as heterogeneous, therefore bigger particles
keep approximately their origin shape and small particles fill interparticle space. The
matrix is formed homogeneous distribution of carbides based on V, Cr, W and Mo. The
LSR layer in so called mix area has spherulite microstructure which is formed by primary
carbides (probably MC) causing as nucleus centre. Generally, it can be stated that it is
apparently hypereutectic alloy. By comparison of microstructures of all samples it can be
express that HIP parameters and the high of pre-heat temperature have no significant
influence on microstructure of base material, mix area and “white” area. However, it has a
small influence on depth of LR layer.
The comparison of LSR depth indicates that the pre-heating temperature at 200 and
350 °C does not determine any differences. The divergence is just relatively several
negligible micrometres. Also, sample without pre-heating has comparable depth of LSR
with other samples. The measured depth of HAZ is relatively adequate to LSR depth.
Probably the distinctive change in LSR depth would be observed if laser processing
parameters are changing.
The microhardness measurement which was done in various areas of microstructure
shows differences in hardness values among all kind of samples. The highest hardness
values after LSR was measured in mix area. The maximal hardness value was measured up
to ~898 HV0.025 (mix area), however, the average hardness value can be stated at about
750 HV0.025. The results have shown some difference in dependence on pre-heating
temperature before LSR where higher values were measured on samples treated at 350 °C.
The remarkable results were obtained after laser pre-heating and following LSR where
measured hardness was in all areas comparable and achieved hardness higher than
800 HV0.025. Generally, microhardness changes in dependence of selected area in
analysed material as is given in Fig. 2 for sample p10t09 (pre-heating at 350 °C) and
p15t09 (without pre-heating).

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 900
p10t09_350
p15t09_Ta

Hardness HV0.025
850

800

750

700
white area mix area top area bottom area HAZ

Fig. 2 Hardness measurements of investigated p10t09_350°C and p15t09_TA samples in various areas

By the evaluation of the diffraction pattern from X-ray analysis the following
phases were identified: martensite, α-phase, austenite and MC carbide based on vanadium.
The identified α-phase is basically martensite, however with small tetragonality and it is
said cubic martensite which has small dimension difference between lattice parameters “a”
and “c” (Maud programme cannot calculate it). The measured phase amount of individual
phases in investigated samples using X-ray analysis is documented in Fig. 3. In all samples
high portion of retained austenite about 44 vol. % was measured in LSR layer. The
vanadium carbide collimates around 31 vol. % and martensite and/or α-phase (blue light
colour in column diagram, Fig. 3) is around 25 vol. %. The portion of phases is comparable
in all analysed samples. The change of measured lattice parameters is relatively negligible
among individual samples. From X-ray diffraction analysis it can be stated that HIP
parameters and varying pre-heating processes have no influence on evaluated phases and
their portion in LSR material. The used pre-heating temperatures at 200 and 350 °C have
small differences among results of phase portion.
MC Austenite Martensite/ α-phase

100%
phase amount [vol. %]

80%

60%

40%

20%

0%

Fig. 3 Phase amount of analysed samples using X-ray analysis

As conclusion it can be stated that production parameters of semifinish product by

HIP can influence resulting properties of LR surface (various value of metastability of
presented phases in material), as well LSR process, however the changes were small after
using the laser source.

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 3.3 Analysis of LSR K390 Microclean tool steel after various heat treatments

The aim of this chapter is analysis of previous heat treatment influence (tempering
temperatures 500 and 200 °C) on the laser surface remelted material. Some samples were
also pre-heated at 350 °C before laser surface remelting. Additional, various post-heat
treatments after LSR were used (500, 550 and 600 °C) to analyse its influence on
macrostructure, microstructure and hardness of investigated K390 material. By Pleterski
[7], a significant decrease of hardness of cold work tool steel after LSR can be caused by
high amount of retained austenite. Therefore, the solution of that problem can be
subsequent post-heat treatment, as also Jurči suggests [8]. Besides that the process of laser
surface remelting induces residual stresses in the modified surface layer [9].
Samples 5PhLr were used for detailed analysis in experimental part of thesis. Their
schematical treatment procedure is shown in Fig. 4.

Fig. 4 The treatment procedure of selected 5PhLr samples

The analysed samples which treatment consists of pre-heating at 350 °C prove the
better results, specifically samples which were after quenching tempered at 500 °C. It is
confirmed also by macroanalysis where on the surface of laser remelted samples (Fig. 5)
were observed no cracks and pores in compare with samples prepared without pre-heating.
In case of sample without pre-heating, cracking of surface was observed during laser
remelting. The cause of this negative influence can be large thermal difference between
cold substrate and high flow power beam of laser.
Results obtained from the roughness measurements on the LR surface do not show
distinctive difference among all samples.
From microscopical point of view, 3 different zones were observed (Fig. 6): laser
remelted zone, heat effected zone and base material. The differences in microstructure
observed by the light microscopy are minimal in individual samples. The change of heat
treatment conditions before LSR as well the change of post-heat treatment have no
significant influence on the microstructure formation. The main subject of investigation
was laser remelted layer where Marangoni effect was affecting during laser pulse remelting
on the surface of material. The microstructure of LSR layer is much finer than base
material. Regarding microstructure of base material homogenous distribution of primary
carbide particles is observed and also small amount of secondary carbides. The matrix
except carbides is formed by martensite and retained austenite. The presented carbides are
probably based on vanadium and molybdenum. From cause too fine microstructure it was
not possible analyse material by using energy dispersive X-ray analysis exactly identifying
of carbide types, therefore it influences wide surroundings and would not be unambiguous
the interpretation. However, from chemical composition it can be stated that to the carbide
formation mainly V, Mo, Cr and W contribute. The microstructure of LSR layer is formed

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mix area and so called “white” area. The mix area has character of spherulite
microstructure which represents hypereutectic alloy type therefore apparently at first
carbide particles originate from the undercooled melt around whose consequently dual-
phase carbide eutectic formed. The eutectic spherulites are based on vanadium carbides.
The surrounding eutectic areas around spherulite can be interspherulitic eutectics probably
based on molybdenum carbides alloyed with other carbide formation elements. The matrix
of ”white” area is enriched about carbon and alloying elements due to partial dissolution of
carbide particles. In that matrix also secondary carbides form which arrange into lines after
post-heat treatment of LSR at temperature 550 and 600 °C. Fig. 7 shows “white” area
between laser remelted layer and base material of selected 5PhLr55 sample. It is possible
to see advancing the dissolution of carbides (lighter strip) in base material and spherulitic
microstructure (bottom part of image) in remelted area. This phenomena is observed in all
analysed samples.

Fig. 5 Macro of 5PhLr55 sample Fig. 6 Microstructure of 5PhLr55 sample

Fig. 7 Microstructure of transition zone of 5PhLr55 sample

The hardness measurements confirmed that various treatment procedures of

samples have a large influence for final quality and properties of material. If samples
temper at 500 °C after quenching, the hardness increases considerably after laser surface
remelting. Particularly, if material is pre-heated before LSR also no cracking occur. The
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highest hardness value 65 HRC was measured for 5PhLrNO sample which was tempered
at 500 °C after quenching, then pre-heated at 350 °C and subsequently laser remelted
without next treatment. Post-heat treatment at 550 °C after LSR in all samples comes
through probably by secondary hardness. Samples quenched and tempered at 200 °C with
subsequently LSR have mostly lower hardness what is influenced a large amount of
retained austenite. The post-heat treatment at 600 °C causes noticeable the drop of
hardness.
66

65
Hardness HRC

64

63

62

61

60

Fig. 7 Changes in surface hardness in dependence on treatment procedure

The obtained results from microhardness measurements show the highest hardness
values over 840 HV0.025 in all areas in LR layer for 5PhLr sample with post-heat
treatment at 550 °C. Regarding HAZ it was not same therefore the highest hardness was
achieved on sample without post heat treatment. Post-heat treatment at 600 °C in compare
with 550 °C causes decreasing of hardness as it is confirmed also by Rockwell hardness
measurements. Samples without, and pos-heat treatment at 500 °C, have relatively
comparable hardness in LR layer except ”white” area where is the different in hardness
~67 HV0.025. In all samples it has seen that hardness is changing in dependence on
treatment temperature. The comparison of results of 5PhLr and 2PhLr samples shows same
behaviour of hardness in “white” area and HAZ. In “white” area hardness values increase,
opposite to HAZ where measured hardness decrease.
By means of X-ray diffraction analysis α-phase, austenite, MC (vanadium carbide
type) were identified in all laser surface remelted layer. Besides mentioned phases also
small portion of Fe2O3 oxide was measured. From obtained X-ray diffraction results it is
clear that initial heat treatment has strong influence on the portion of evaluated phases in
laser surface remelted layer. The comparison of samples has showed that with increasing
post-heat treated temperature the portion of retained austenite decreases. After post-heat
treatment at 600 °C (without pre-heating before LSR) no retained austenite or small
amount of austenite 5.72 vol. % (with pre-heating) was measured in LSR layer with the
difference of samples without post-heat treatment where the highest portion of retained
austenite was measured around 40 vol. %. In matrix of base material tempered at 500 °C as
well as no retained austenite was detected. The amount of vanadium carbides is relatively
stable in all investigated samples. The distinctive changes in lattice parameters among
individual identified phases are not notable.

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 100%
phase amount [vol. %]
80%
MC
60% Austenite
α-phase
40%

20%

0%

Fig. 8 Phase amount of analysed in 5Lr samples from X-ray analysis

Based on achieved results it is possible to state that the most advantageous

treatment method of analysed K390 Microclean high alloy cold work tool steel is
hardening and tempering at 500 °C, pre-heating before laser surface remelting and
subsequent post-heat treatment at 550 °C.

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4 CONCLUSION

The cold work tool steel K390 Microclean is tool material with high wear resistant
and toughness. This material has used for different applications. This dissertation thesis
deals with the laser surface remelting of cold work tool steel which was produced by
powder metallurgy process.
The influence of laser surface remelting of high alloy tool steels is presented in
some works [10-15], however, it was carried out in different applications of laser using,
such as laser cladding [13], laser surface alloying [10,12], laser repair-welding and surface
treatment [11] or laser modified of surface layer [14]. These works determine some
problems caused by laser treatment.
The main aim of thesis is to find optimal parameters for surface laser remelting process
with specific laser device. This process can be used for improvement of surface properties
the tools, or for repairing of damaged surface during its exploitation.
The first analysis was focused to phase evolution and transformation in quasi-
equilibrium state during slow heating and cooling. The microstructure of high alloy cold
work tool steel has a dendritic morphology; however, dendrites are created by eutectic
based on the vanadium carbides. On the boundaries are formed molybdenum carbide
eutectics. Transformation of austenite to ferrite occurs around the temperature of 830 °C.
The transition from ferromagnetic to paramagnetic state is around the temperature 780 °C.
The crucial aim was analysis of laser surface remelted layer of K390 high alloy tool
steel. Therefore, from the detailed characterization and examining of the laser surface
remelted samples, the following conclusions may be summarised:
1. The pre-heating process prevented crack formation and pores on the surface due to
decreasing thermal difference between cold substrate and laser beam which
influences LR layer on surface. For LSR 50 % overlapping laser spots was used.
The crack formation do not depend probably from phase amount in LSR layer,
therefore, it was identified in higher/ lower amount of martensite in microstructure
of samples which were without pre-heating before LSR.
2. The results from roughness measurements and topography are relatively
comparable in all type of samples.
3. HIP parameters have no influence on formation of microstructure in LSR layer. In
sample cross-section after LSR three zones were observed: laser remelted zone,
heat affected zone and base material. The microstructure of LR layer is much finer
than microstructure of base material which is heterogeneous. The distribution of
carbides in matrix is homogeneous. In case of heat treated samples secondary
carbide particles were observed after post heat treatment of LSR layer. The LSR
layer in so called mix area has spherulite microstructure which is formed by
primary carbides (probably MC) causing as nucleus centre. From the morphology
type of microstructure this tool steel is as hypereutectic alloy. The lighter area
surrounding around eutectic spherulite is rich on molybdenum.
4. The hardness measured on HIP samples after LR do not show distinct differences.
In case of heat treated samples hardness measurements on the LSR has shown the
best results on samples which were tempered at 500 °C after hardenning and pre-
heated at 350 °C before LSR. The highest hardness value (65 HRC) was measured
on sample which was tempered at 500 °C, pre-heated at 350 °C with following
laser remelting without subsequent post-heat treatment. As well as, samples treated
various procedures; however alike post-heat treatment at 550 °C shows the optimal
hardness results which can be achieved due to treatment after LSR. The

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 temperature of post-heat treatment at 600 °C causes noticeable the drop of
hardness.
The Rockwell hardness measurements confirmed the highest measured hardness in
LR layer for 5PhLr55 sample and decreasing hardness of 5PhLr60 (tempered at
500 °C and pre-heated at 350 °C before LSR with following post-heat treatment at
550 °C and 600 °C respectively) as microhardness measurements. The results of
microhardness measurements have shown the change of hardness in dependence on
treatment manner what it depends with achieving equilibrium state of individual
presented phases in LSR layer. The values of microhardness depend on chemical
composition change of presented phases.
5. By means of X-ray analysis martensite and/or α-phase, austenite and MC carbide
based on vanadium were identified. In all samples after HIP process with following
pre-heating large portion of retained austenite ~ 44 vol. % was measured in LSR
layer, therefore it is needed to carry out post-heat treatment after LSR. Samples
which were heat treated and consequently post-heat treated after LSR shows
decreasing tendency of retained austenite amount with increasing post-heat
treatment temperature. Post heat-treatment at 600 °C ensured the transformation
retained austenite into α-phase. As well as in base material tempered at 500 °C no
retained austenite was detected.

The all obtained results indicate that the best treatment manner of investigated
K390 Microclean high alloy cold work tool steel is hardening and tempering at
temperatures 200 °C and 500 °C, pre-heating at 350 °C immediately before LSR and post-
heat treatment at 550 °C.
The dissertation thesis is a new groundwork for using laser surface remelting of
high alloy and high carbon tool steel. The analysed steel contains cobalt content which has
an influence on diffusion process during laser remelting and conventional heat treatment.
Such high complex alloy tool steel with high carbon content has not been analysed after
laser surface remelting in big extent. The results indicate that for optimal treatment is
needed pre-heating before LSR and tempering the created layer for achieving optimal
properties.

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of a cold work tool steel after pulsed laser remelting. In Metalurgija, vol. 51 (1), 2012,
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[8] JURČI, P., CEJP, JIRI, BRAJER, J. Metallurgical aspects of laser surface processing of
PM Cr-V ledeburitic steel. In Advances in Materials Science and Engineering 2011
(2011) 8.
[9] GRUM, J., ŠTURM, R. Residual stress state after the laser surface remelting process.
In Materials Engineering and Performance 10 (3) (2001) 270-281.
[10] BONEK, M., DOBRZANSKI, L.A., HAJDUCZEK, E., KLIMPEL, A. Laser
modification of surface layer properties of a hot-work tool steel. In Journal of
Achievements in Materials and Manufacturing Engineering 14 (1-2) (2006) 152-156.
[11] VEDANI, M., PREVITALI, B. VIMERCATI, G.M., SANVITO, A., SOMASCHINI, G.
Problems in laser repair-welding a surface-treated tool steel. In Surface and Coatings
Technology 201 (2007) 4518-4525.
[12] BONEK, M., DOBRZANSKI, L.A., HAJDUCZEK, E., KLIMPEL, A. Structure and
properties of laser alloyed surface layers on the hot-work tool steel. In Journal of
Materials Processing Technology 175 (2006) 45-54.
[13] PLETERSKI, M., TUŠEK, J., MUHIČ, T., KOSEC, L. Laser cladding of cold-work tool
steel by pulse shaping. In Journal of Material Science and Technology 27(8) (2011) pp.
707-713.
[14] DOBRZANSKI, L.A., BONEK, M., HAJDUCZEK, E., KLIMPEL, A., LISIECKI, A.
Comparison of the structures of the hot-work tool steels laser modified surface. In
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[15] GRUM, J., ŠTURM, R. Influence of laser beam guiding and overlapping on residual
stress in remelting process. In Surface Engineering 21 (1) (2005) 27-34.

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WORKS PUBLISHED

ADF Scientific works in Slovak non-current journals

Number of accounts: 2
ADF1 Štefániková, Mária - Moravčík, Roman - Kocúrová, Karin: The analysis of causes
of lorry piston combustion engine damage.
In: Materials Engineering. Materiálové inžinierstvo. - ISSN 1335-0803. - Vol. 19
(2012), p. 47-51
ADF2 Kocúrová, Karin - Hazlinger, Marián - Štefániková, Mária: Microstructure and
fractographic analysis of damage reasons of cogwheel.
In: Materials Engineering. Materiálové inžinierstvo. - ISSN 1335-0803. - Vol. 19
(2012), p. 82-87

AFD Published contributions in Slovak scientific conferences

Number of accounts: 4
AFD1 Štefániková, Mária - Moravčík, Roman - Kocúrová, Karin: Analýza príčin
poškodenia piestu spaľovacieho motora nákladného automobilu. - ITMS
26220120014.
In: Degradácia konštrukčných materiálov 2011 : XII. vedecká konferencia so
zahraničnou účasťou, Terchová - Biely Potok, 12. - 14.9.2011. - Žilina : Žilinská
univerzita, 2011. - ISBN 978-80-554-0416-5. - s. 147-151
AFD2 Kocúrová, Karin - Hazlinger, Marián - Štefániková, Mária: Analýza príčin
poškodenia ozubeného kolesa.
In: Degradácia konštrukčných materiálov 2011 : XII. vedecká konferencia so
zahraničnou účasťou, Terchová - Biely Potok, 12. - 14.9.2011. - Žilina : Žilinská
univerzita, 2011. - ISBN 978-80-554-0416-5. - s. 70-74
AFD3 Štefániková, Mária - Moravčík, Roman: Influence of the powder particle size on the
microstructure of Cr-Mo-V tool steel compacts produced by hot isostatic pressing.
In: International Doctoral Seminar 2010 : Proceeding. Smolenice, 16-19 May 2010.
- Trnava : AlumniPress, 2010. - ISBN 978-80-8096-118-3. - p. 502-511
AFD4 Štefániková, Mária: Vplyv parametrov izostatického lisovania za tepla na kompakty
z vysokolegovanej nástrojovej ocele.
In: SEMDOK 2010 : 15th International of PhD. students´ seminar. Žilina -
Terchová, Slovakia, 27-29 January, 2010. - Žilina : Žilinská univerzita, 2010. -
ISBN 978-80-554-157-7. - s. 221-225

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Scientific works in foreign journals (sent for publishing)
Number of accounts: 2
1 Moravčík, Roman – Štefániková, Mária – Čička, Roman – Čaplovič, Ľubomír –
Šturm, Roman – Kocúrová, Karin: Phase transformations in high alloy cold work
tool steel. In: Strojniški vestnik. Journal of Mechanical Engineering. - ISSN xxxx-
xxxx. - Vol. xx (2012), p. xx-xx
2 Čička, Roman, Bakajová, Jana – Štefániková, Mária – Dománková, Mária –
Janovec, Jozef: Evolution of secondary phases in 0.17C-16Cr-11Mn-0.43N
austenitic stainless steel at 800 and 850°C. Thermodynamic modeling of phase
equilibria and experimental kinetic studies. In: Journal of Mining and Metallurgy,
Section B: Metallurgy - ISSN xxxx-xxxx. - Vol. xx (2012), p. xx-xx

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ABSTRACT

Key words: High alloy tool steel; Powder metallurgy; Phase transformation; Heat
treatment; Laser remelting; X-ray diffraction analysis

The dissertation thesis deals with the solidification in quasi-equilibrium conditions

during cooling in K390 Microclean high alloy cold work tool steel produced by powder
metallurgy. The microstructural analysis, differential thermal analysis, thermogravimetry
and electron microprobe analysis established that microstructure is formed by two
morphologically different types of eutectics based on vanadium and molybdenum reach
phases. Phase transformation from austenite to ferrite is observed to take place at
temperature ~830 °C. Solidification of analysed material begins at 1340 °C and it is
finished at 1208 °C. The Curie temperature of this steel is approximately at 780 °C.
The aim is analysis of influence of laser remelting on surface layer of K390 high alloy tool
steel. In the laser surface remelted layer three various areas are observed. The mix area in
laser surface remelted layer is formed by eutectic spherulites based on vanadium reach
carbide phase. The best results are obtained on samples which were conventionally treated
by hardening and tempered at temperature 500 °C and with following pre-heat treatment at
350 °C before laser remelting process. The hardness measurements of samples with
subsequent post-heat treatment at 550 °C after laser remelting have proved optimal results.
The process of pre-heating at 350 °C shows very important effect to prevent of potential
crack and pores formation, respectively. Following phases are identified using X-ray
analysis on the laser remelted surface: martensite and/or α-phase, austenite and MC carbide
based on vanadium. It has been found out that varying hot isostatic pressing parameters
and just pre-heating without post-heat treatment has no significant influence on resulting
phases evolved in laser surface remelted microstructure. The material without post-heat
treatment after laser surface remelting is distinguished by higher portion of retained
austenite in laser remelted layer. It is confirmed that with increasing post-heat treatment
temperature after LSR portion of retained austenite decreases and at temperature 600 °C
austenite already is not identified.

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SÚHRN

Kľúčové slová: Vysokolegovaná nástrojová oceľ; Prášková metalurgia; Fázová premena;

Tepelné spracovanie; Laserové pretavovanie; RTG difrakčná analýza

Dizertačná práca sa zaoberá analýzou solidifikácie v kvázi rovnovážnych

podmienkach počas pomalého ohrevu a ochladzovania vo vysokolegovanej nástrojovej
oceli na prácu za studena K390 Microclean vyrobenou práškovou metalurgiou. Analýzou
mikroštruktúry, DTA záznamu, záznamu z termogravimetrie a mikroanalýzou sa stanovilo,
že mikroštruktúra je tvorená dvoma morfologicky odlišnými typmi eutektík na báze
vanádu a molybdénu. Bola určená teplota fázovej premeny austenitu na -fázu pri teplote
~830 °C. Solidifikácia nástrojovj ocele začína na teplote 1340 °C a je ukončená pri teplote
1208 °C. Curieho teplota tejto ocele je približne v okolí teploty 780 °C.
Cieľom bola analýza vplyvu laserového pretavovania na povrchovú vrstvu
vysokolegovanej nástrojovej ocele K390. V laserom pretavenej vrstve boli pozorované
rôzne oblasti. Premiešaná oblasť v laserom pretavenej povrchovej vrstve je mikroštruktúra
tvorená eutektickými sforolitmy na báze karbidu vanádu. Najlepšie výsledky boli získané
na vzorkách, ktoré boli tepelne spracované kalením a popustením pri teplote 500 °C
a následným predohrevom na 350 °C pred procesom laserového pretavovania. Meranie
tvrdosti dodatočného spracovania po laserovom pretavení pri teplote 550 °C preukázali
optimálne výsledky. Predohrev na 350 °C pre laserovým pretavovaním povrchu má
výrazný vplyv na zamedzenie potenciálnych povrchových trhlín alebo pórov. Na základe
RTG difrakčnej analýzy boli v laserom pretavenom povrchu identifikované fázy: martenzit
resp. α-fáza, austenit a MC karbid na báze vanádu. Rôzne parametre HIP a samotný
predohrev pred laserovým pretavovaním bez následného popustenia nemajú zásadný vplyv
na výsledné fázy v mikroštruktúre laserom pretavenej vrstvy. Materiál bez následného
popustenia po pretavení sa vyznačuje vyšším podielom zvyškového austenitu v pretavenej
vrstve. Tiež sa potvrdilo, že so zvyšujúcou sa teplotou popúšťania po pretavení povrchu sa
podiel zvyškového austenitu znižuje, a po popúšťaní pri teplote 600 °C nebol
identifikovaný.

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