Effect of nitrogen on supersolidus sintering of
modified M35M high speed steel
I. Aguirre, S. Gimenez, S. Talacchia, T. Go ´ mez-Acebo, and I. Iturriza
atmosphere, 90N
2
–9H
2
–1CH
4
. The diminution of the
optimum sintering temperature and the widening of the
Water atomised high vanadium M35M high speed
sintering gate were proved. It was also demonstrated
steel powders with different carbon contents were cold
that sintering to full density of modified high carbon–high
compacted at 700 MPa and sintered under an N
2
rich
vanadium T42, T15, and M35M HSSs under 1150°C is
atmosphere. Full density specimens were obtained at
possible.10–12 This marks a historical milestone because
temperatures between 1140 and 1105°C for carbon
continuous mesh belt furnaces could now be used to
contents between 1·8 and 2·5 wt-% respectively. The
sinter HSS.
sintering behaviour of these powder mixtures was cor-
However, the interpretation of how nitrogen affects
related with dilatometric curves and phase diagram
sinterability was only made in a descriptive way. The aim
calculations made by Thermo-Calc software. It is
of this paper is to show the correlation between supersolidus
demonstrated that densification takes place above the
sintering behaviour and the nitrogen effect. The effect of
solidus temperature, within the austenite +carbide +
nitrogen has been studied through the sintering behaviour
liquid phase field, and that nitrogen widens this
of modified M35 HSS. Experimental results have been
region, which is responsible for increased sinterability
explained under the basis of the supersolidus theory and
with regards to vacuum sintered high speed steel.
the phase diagrams obtained by Thermo-Calc software
PM/0836
and the SSOL databank. Calculations of phase diagrams
where the effect of sintering atmosphere can be taken into
The authors are at CEIT and Faculty of Engineering,
account would be a powerful tool for designing powder
University of Navarra, Po Manuel de Lardizabal
compositions and processes in order to obtain more
15, Bo de Ibaeta, 20018 San Sebastia ´n, Guipuzcoa,
competitive HSS components.
Basque Country, Spain. Manuscript received 2 March
1999; accepted 11 June 1999.
EXPERIMENTAL PROCEDURE
© 1999 IoM Communications Ltd.
Vacuum annealed water atomised M35MHV HSS powders
were produced at Powdrex Ltd (UK). The chemical analysis
of the powders provided by the manufacturer is Fe–1·80C–
INTRODUCTION
4·0Cr–5·4Mo–5·5Co–0·035N–4·2V–6·0W–0·06O. Additions
After three decades of study, two commercial PM routes
of 0·2, 0·5, and 0·7 wt-% of elemental carbon (graphite)
are now employed in the production of fully dense
were made and dry mixing in a Turbula mixer was carried
high speed steel (HSS) components; one is hipping of gas
out for 3 h. Powders were cold compacted uniaxially at
atomised powders and the other is vacuum sintering of
700 MPa and then sintered in a flowing atmosphere of
water atomised powders.1 The latter allows HSS powders
90N
2
–9H
2
–1CH
4
. Specimens were heated at the sintering
to be cold pressed and sintered to near net shape. It is well
temperature, soaked for 60 min, and oil quenched. Densities
established that direct sintering is one of the few commercial
were measured using the Archimedes’ method. Transverse
applications of the supersolidus processes.2,3 The presence
sections were mechanically polished, etched with 3% nital,
of a liquid phase associated with a narrow sintering window
and observed by optical microscopy. As polished specimens
(region of temperature where full density specimens with
were observed by a Philips XL30 SEM fitted with an
acceptable microstructures are obtained) makes an accurate
energy dispersive X-ray system. Dilatometric curves were
determination of the sintering gate necessary. This avoids
obtained with a Netzsch Dil 402 E/7 dilatometer. Specimens
distortion owing to an excessive volume fraction of liquid
were heated at 20 K min-1 under a N
2
flowing atmosphere.
or, on the contrary, a lack of densification because of an
Specimens without carbon addition and those mixed with
insufficient liquid phase. Both situations would produce
0·2 and 0·5 wt-%C were heated to 1250°C, while the
undesirable mechanical properties. Commercial grade HSSs
specimens with additions of 0·7 wt-%C were heated to
exhibit a narrow sintering window (less than 3 K for M2
1230°C.
and 10 K for T1) and thus vacuum sintering needs to
After taking into account the carbon and nitrogen
control accurately the temperature inside the furnace,
contents after sintering, several phase diagrams were
making the sintering of cold compacted near net shape
calculated using the Thermo-Calc software.13 The thermo-
components expensive.
dynamic parameters in the calculations were taken from
As a consequence, it is clear that a good understanding
the SSOL database produced by the Scientific Group
of how the sintering gate is affected by compositional and
Thermodata Europe.14 In this software, each phase is processing variables will enhance the production routes
modelled considering all the possible contributions to the for HSS parts, in order to make them cheaper and more
Gibbs energy, including the magnetic contributions. The flexible. The effect of carbon, cobalt, and molybdenum
effect of composition is taken into account by means of additions on the sinterability of different T and M grades
different binary interaction parameters and, in some cases, (BT42, BT1, BM2) has been studied by several authors.4–6
ternary or even higher order interaction parameters. The They found that controlled additions of these elements not
correlation between calculated phase diagrams (isopleths) only lowers the solidus temperature but also extends the
and dilatometric curves was analysed in order to establish sintering gate.
solidus lines and sintering windows for different compos- Since 1980, work has been carried out by Urcola and
co-workers7–9 on sintering of HSS under a nitrogen rich itions.
Powder Metallurgy 1999 Vol. 42 No. 4 353 ISSN 0032–5899