Beruflich Dokumente
Kultur Dokumente
2130–2138
The main focus of the present study was the influence of liquid metal properties on the particle size
during water atomisation. Experiments for liquid iron showed that alloy additions of carbon and sulphur
decreased the particle size. Moreover, it was indicated that the reduced d50 value at increased %C and
%S contents may be related to a decreased viscosity and surface tension respectively. An alternative
mechanism could be that raised superheats at increased carbon contents increased the total available
time for atomisation. This may also have decreased the particle size. The influence of surface tension and
viscosity on the d50 value was further analysed with a theoretical d50 model proposed in a previous work.
A reduced viscosity from 6.8 to 4.3 mPa s decreased the d50 value with 33%. In addition, the particle size
was estimated to decrease with 27% by decreasing the surface tension from 1 850 to 900 mN m–1.
KEY WORDS: water atomisation; surface tension; viscosity; metal powders; particle size; superheat.
Table 2. DOE study, parameters and results for test 1–6, see
“Nomenclature” for parameter definitions.
Test 1 2 3 4 5 6
Heat D1959 D1951 D1961 D1952 D1957 D1956
Fig. 1. Experimental set-up for V-jet water atomisation trials. Parameters
Atomising time (s) 251 222 222 244 136 54
sequence. Nitrogen gas was purged through the lid, to mM (kg s ) –1
0.96 0.95 0.95 0.82 1.62 1.39
decrease the degree of oxidation of the melt. The liquid steel
mW (kg s–1) 4.99 6.51 4.16 5.27 4.99 6.51
temperature was measured with an expendable temperature
Temperature furnace
sensor, which was immersed with a steel lance in the liquid (°C)
1 626 1 624 1 617 1 617 1 620 1 630
steel. When the target steel temperature of 1 620°C was
Temperature tundish
reached, the furnace was tilted and the liquid metal was (°C)
1 560 1 552 1 547 1 530 1 580 -
poured into a tundish with an alumina refractory lining. A
Liquidus temperature
Liquefied petroleum gas burner was used to preheat the 1 236 1 520 1 519 1 167 1 241 1 513
(°C)
tundish, which was red hot before the atomisation was started. μM (m Pa s) 5.03 6.27 6.76 4.34 4.93 6.49
The steel temperature was measured in the furnace just before
γM (mN m–1) 926 1 680 901 1 849 1 712 920
atomisation and after 1–2 minutes of atomisation in the
WeL/ReL (Eq. (13)) 0.59 0.61 0.82 0.38 0.31 1.15
tundish. The liquid iron was poured through a tundish nozzle
into the V-jet water atomising system. The V-jet has in total As atomised powder
eight symmetrically arranged water nozzles. These include LECO (wt %)
two pairs of main and side jets respectively and four support- C 3.38 0.22 0.04 4.22 3.53 0.13
ing jets. The jet angle between the water jet and the metal N 0.002 0.005 0.008 0.001 0.002 0.008
stream was 26.5° for the main jets. Nitrogen was used to flush O 0.41 0.39 0.48 0.29 0.32 0.96
the atomising tank, to avoid the risk for hydrogen explosions.
S 0.513 0.006 0.503 0.004 0.008 0.443
The steel level in the tundish was regulated manually to
around 20 cm during the atomisation. The steel flow rate to ICP-OES
the atomizer was stopped immediately when the furnace was Al 0.004 0.002 0.001 0.000 0.002 0.002
empty, by pressing a steel rod through the melt to block the Cr 0.007 0.009 0.001 0.009 0.003 0.017
tundish nozzle. The powder slurry was dewatered after atom- Cu 0.002 0.004 0.001 0.002 0.002 0.004
isation. The wet iron powder cake was finally dried at 180°C Mn 0.028 0.022 0.012 0.041 0.032 0.023
by using warm compressed air. The drying was interrupted
Mo 0.000 0.001 0.000 0.000 0.000 0.001
when the temperature of the iron powder reached 95°C.
Ni 0.015 0.018 0.014 0.015 0.015 0.018
2.2. Experimental Programme and Procedure P 0.003 0.002 0.002 0.003 0.002 0.003
The experimental programme was planned and evaluated Si 0.025 0.014 0.000 0.076 0.051 0.028
with the software Modde 9 developed by Umetrics AB.9) A Ti 0.019 0.000 0.000 0.106 0.038 0.002
26–3 fractional factorial design with resolution III and four V 0.071 0.063 0.040 0.091 0.079 0.043
centre points was chosen for the study, Table 1. Investigated Particle size
factors were pW (water pressure), J (configuration of the
d50 (μ m) 80.5 59.3 103.6 48.4 131.8 57.6
water jet), DM/D0 (relative melt stream diameter), H/H0 (rel-
σLN 2.16 2.34 2.46 2.12 2.00 2.47
ative water level in the atomising tank), %C (carbon content
in the liquid steel) and %S (sulphur content in the liquid AD (g cm–3) 3.42 2.94 3.38 3.38 3.20 3.27
Table 3. DOE study, parameters and results for test 7–12, see Table 4. Influence of melt stream diameter, parameters and results
“Nomenclature” for parameter definitions. for test 13–16, see “Nomenclature” for parameter defini-
tions.
Test 7 8 9 10 11 12
Test 13 14 15 16
Heat D1954 D2134 D1974 D1960 D1953 D1958
Parameters Heat D1981 D1982 D1983 D1984
Atomising time (s) 134 140 178 113 136 114 Parameters
mM (kg s–1) 1.60 1.60 1.26 1.24 1.14 1.18 Atomising pressure (MPa) 15 15 15 15
mW (kg s–1) 4.16 5.27 5.68 5.68 4.77 4.77 Atomising time (s) 195 132 112 70
γM (mN m ) –1
1 596 965 1 016 1 000 1 015 1 048 γM (mN m–1) 1 639 1 629 1 662 1 649
WeL/ReL (Eq. (13)) 0.44 0.80 0.79 0.81 0.79 0.77 WeL/ReL (Eq. (13)) 0.62 0.62 0.61 0.62
C 0.12 4.17 1.92 1.83 2.11 1.92 C 0.918 1.059 1.181 1.022
N 0.006 0.001 0.004 0.005 0.005 0.004 N 0.007 0.004 0.004 0.003
O 0.44 0.85 0.28 0.21 0.70 0.38 O 0.19 0.35 0.30 0.36
S 0.011 0.46 0.258 0.276 0.268 0.218 S 0.006 0.007 0.006 0.006
ICP-OES ICP-OES
Al 0.002 <0.001 0.002 0.002 0.002 0.001 Al 0.000 0.000 0.001 0.001
Cr 0.007 0.65 0.110 0.002 0.003 0.002 Cr 0.567 0.141 0.081 0.266
Cu 0.003 0.002 0.001 0.002 0.003 0.002 Cu 0.001 0.001 0.001 0.001
Mn 0.018 0.023 0.020 0.022 0.027 0.023 Mn 0.031 0.025 0.027 0.029
Mo 0.001 0.007 0.000 0.000 0.001 0.000 Mo 0.002 0.000 0.000 0.002
Ni 0.019 0.044 0.016 0.015 0.017 0.014 Ni 0.015 0.014 0.014 0.016
P 0.002 0.003 0.002 0.002 0.002 0.002 P 0.001 0.002 0.002 0.003
Si 0.007 0.011 0.053 0.030 0.019 0.034 Si 0.025 0.022 0.028 0.029
Ti 0.000 0.002 0.003 0.006 0.008 0.007 Ti 0.003 0.001 0.002 0.002
V 0.049 0.095 0.074 0.071 0.070 0.069 V 0.061 0.068 0.075 0.076
d50 (μ m) 176.4 35.4 67.4 82.5 79.2 82.7 d50 (μ m) 78.5 83.1 85.0 91.7
σLN 2.69 2.80 2.41 2.57 2.53 2.48 σLN 2.47 2.33 2.57 2.48
AD (g cm ) –3
3.34 3.12 3.71 3.56 3.49 3.74 AD (g cm–3) 3.10 3.20 3.10 3.08
steel). Two different setups of water nozzles were investi- slowly feeding all atomised powders through a powder sam-
gated in the study, jet A and B. The water flow rate in jet A pler. A spinning riffler was finally used to split the powder
was 20–24% higher than in jet B, depending on the level of to the specific amount needed for each analysis. Carbon,
the water pressure, Tables 2 and 3. The water level during sulphur, oxygen and nitrogen were determined by a LECO
atomisation was defined as the distance from the tank top to analysis, according to the standards ISO 15350 (percentag-
the water surface in the atomising tank. The water level in es of C and S) and ISO 15351 (percentages of O and N).
the atomising tank (H) and the melt stream diameter (DM) Inductively plasma atomic emission spectroscopy was used
were related to a reference value, Table 1. The parameters to determine trace elements, according to ISO 13898 1-4.
H0 and D0 represent the lowest water level and the largest The as-atomised powder particle size was determined by a
melt stream diameter, respectively. sieve analysis (EN ISO 24497). The apparent density was
The experiments were carried out in a random order, to determined with a Hall flow meter (ISO 3923-1). In addi-
minimize that time dependent trends influenced the experi- tion, scanning electron microscopy (SEM) was used to study
mental values. Four additional trials were finally carried out, the particle shape and morphology.
to further investigate how the particle size was influenced
by an increased melt stream diameter, Table 4. The heat size
3. Results
during these four trials was 150 kg.
A powder sample of 5 kg was taken from each heat, by As mentioned previously, the main purpose of this paper
is to study how the physical properties of the liquid metal heat is here defined as the difference between the steel tem-
influence the particle size for water atomised metal pow- perature in the induction furnace just before atomisation and
ders. Carbon and sulphur was alloyed to liquid iron, to spe- the liquidus temperature. The software Thermocalc10) was
cifically investigate how the d50 value was influenced by the used to calculate the liquidus temperature for all test heats
viscosity and surface tension of the liquid metal. The target in this work. The d50 values for the experiments were calcu-
tapping temperature of the furnace was constant at 1 620°C lated by curve fitting of data from a sieve analysis against
for all test heats, to be able to select as consistent data as the log normal distribution. The correlation between the
possible for these properties. The superheat during the cumulative particle size distribution obtained from sieve
experiments varied from around 100 to 450°C, depending analysis and the log normal distribution was very good for
on the carbon and sulphur contents, Tables 2–4. The super- all experiments in the present study, Fig. 2. Atomised pow-
ders contained a mixture of irregular and rounded particles.
Figures 3 and 4 show the particle morphology for a 0.22%C
and a 4.22%C content, respectively. It is clear that the par-
ticle shape was generally more irregular for powders atom-
ised at low carbon contents.
Fig. 4. Scanning electron microscope investigation, test 4, heat Fig. 6. Histogram plot of d50 data after logarithmic transformation
D1952, 4.22%C, particle size of 75–106 μ m. (base 10), factorial experiments.
( Y − Yl )
2
i i
PRESS = Σ ........................ (3)
(1 − hi )
i 2
Fig. 10. Estimated viscosity values at 1 550°C versus carbon con- Fig. 11. Influence of water pressure, surface tension and viscosity
tent for all test heats in the present study. on the d50 value, for tests 1–16.
frictionless flow and ρw is the water density. °K–1, T is the temperature of the liquid metal in °K, and
The coefficient φ was estimated to have a value of 0.86 Tsteam is the steam temperature in the atomizing zone in °K.
for the nozzles in the current study, based on water flow The cooling time was calculated for test 2 and 4 which
rates and pressure values from the nozzle supplier. The were atomised at carbon contents of 0.22 and 4.22% respec-
water temperature was assumed to be 20°C in the calcula- tively, Tables 1 and 2. The steel temperature T was estimated
tions, which gives a water density of 0.998 g cm–3. Data with the measured temperature in the tundish. Values for h
from all experiments in this work (Tables 1–4) were finally were taken from a study by Sanin and Nichiporenko.22) The
used to estimate the ratio between the viscous energy dissi- heat transfer coefficient at 18 MPa was estimated to decrease
pation and the surface energy according to Eq. (13). A value from 8.9×105 to 1.4×105 W m–2 °K–1, when the metal droplet
of WeL/ReL = 1 would mean that the surface tension and vis- size increased from 10 to 500 μ m. Values for ρM and cM were
cous forces are of similar importance during the atomisation equal to 7 030 kg m–3 and 717 J kg–1 °K–1 respectively.13) The
process. WeL/ReL was estimated to have values between 0.3 steam temperature was estimated to 900°C.21)
and 1.2 for the tests in the present study, Tables 2–4. This Figure 12 shows calculated cooling times at 5 different
indicates that both the viscosity and the surface tension of metal droplet diameters. The cooling time increased with an
the liquid metal may have influenced the atomisation of the increased metal droplet size. It was determined to be 17
liquid metal in this work. times longer at a 4.22%C content compared to a 0.22%C
content. The rounder particle shape for test 4 compared to
4.2. Influence of Superheat test 2 further indicated that the cooling time was significantly
The influence of the liquid metal properties can be dis- longer at high carbon contents, Figs. 3 and 4. It can be spec-
cussed further by evaluating how the superheat affects the ulated that the available time for atomisation was increased at
particle size. As mentioned earlier, it was estimated using higher carbon contents in the present study, since the superheat
Eq. (4) that the d50 value decreased by 28% when the carbon was raised at increased carbon contents. This may improve
content in the liquid steel increased from 0.05 to 4%. This the secondary atomisation of primary atomised ligaments,
increased carbon content also corresponds to a raised super- which could contribute to a reduction of the particle size.
heat from around 90 to 430°C, Tables 2–4. Summarized, this
corresponds to a reduction of the d50 value by 8% per 100°C 4.3. d50 Model
of superheat. This is in agreement with previous investiga- The experimental results in this work were further evalu-
tions by Ankus et al.3) and Dunkley et al.,6) who noticed a ated with an empirical d50 model proposed in a previous
reduction of the d50 value by 7–9% and 5–10% respectively work.23) This model is presented in Eq. (13), with calculated
per 100°C of superheat. exponents relevant for the present study
The calculated influence of the superheat on the particle
−0.39
size in this work may be explained by a decreased viscosity γ 0.45 μ 0.90 D 0.20 ⎛ m ⎞
d50 = k M 0.72M M ⎜ W ⎟ ............. (13)
at increased carbon contents, Fig. 10. However, a second pW sin α ⎝ mM ⎠
possible mechanism could be that the total available time for
atomisation increases at increased superheats. This can be where k is a model constant, α is the jet angle between the
illustrated by evaluating the cooling time down to the liqui- axis of the water jet and axis of the metal stream, DM is the
dus temperature for an atomised steel droplet. The cooling melt stream diameter in m, mW and mM is the mass flow rate
time tC can be estimated with Eq. (12):21) of water and metal respectively in kg s–1.
ρ M cM (T − TSteam ) All experimental heats in this work were used to deter-
tC = d d ln ................ (12) mine the k value and exponents in Eq. (13), Tables 1–4. The
6h (Tm − TSteam ) parameter units defined in ‘Nomenclature’ were used to cal-
where dd is the metal droplet diameter in m, ρM is the liquid culate the k value. The least-square method was used to min-
metal density in kg m–3, cM is the specific heat for the liquid imize the error between experimental and calculated d50
metal in J kg–1 °K–1, h is the heat transfer coefficient between values. The k value in Eq. (13) for this study was estimated
the metal droplet and the surrounding atmosphere in W m–2 to 1.85×109. The superheat was not directly considered in
this model. The influence of liquid metal properties was
Fig. 12. Calculated cooling time for liquid metal droplets from the
tundish temperature down to the liquidus temperature, Fig. 13. Experimental data from the present study versus calcu-
tests 2 and 4. lated d50 values for Eq. (13).
Table 5. Calculated exponents for Eq. (13) compared with previous investigations, see “Nomenclature” for parameter
definitions.
Alloy additions of 4%C and 0.5%S to liquid iron KS : adsorption coefficient for sulphur
decreased the d50 value with 28 and 31%, respectively. It is mM : mass flow rate of liquid metal/kg s–1
indicated that the reduction of the particle size at increased mW : mass flow rate of water/kg s–1
carbon and sulphur contents may be related to a decreased pW : water pressure/Pa
viscosity and surface tension of the liquid metal, respectively. ReL: Liquid phase Reynolds number
The relation between investigated parameters and the par- T: temperature of liquid metal/°K
ticle size was further analyzed with an empirical d50 model T m: liquidus temperature of metal/°K
proposed in a previous work.23) The influence on the d50 val- Tsteam: water steam temperature in the atomising zone/
ue was estimated as follows for investigated parameters: °K
i) water pressure: large effect, a 44% decrease for pres- vW : velocity of atomising water/m s–1
sures from 8 to 18 MPa. WeL: Liquid phase Weber number
ii) viscosity: medium effect, a 33% decrease for viscosities α: jet angle, between the axis of the water jet and
from 6.8 to 4.3 mPa s. the melt stream/°
iii) surface tension: medium effect, a 27% decrease for sur- γM : surface tension of liquid metal/N m–1
face tensions from 1 850 to 900 mN m–1. μM : viscosity of liquid metal/Pa s
iv) melt stream diameter, small effect, a 10% decrease for ρM : density of liquid metal/kg m–3
relative diameters (DM/D0) from 1 to 0.57. ρW : density of atomising water/kg m–3
The influence of the surface tension and viscosity should σLN : standard deviation of the log normal distribution
be seen as provisional, since there is a relatively large scatter
between experimental data in the literature14,28) REFERENCES
It may also be possible that the reduced particle size at 1) J. Dunkley: Met. Powder Rep., 57 (2002), No. 11, 18.
2) E. Klar: Met. Powder Rep., 40 (1985), No. 1, 7.
increased carbon contents in this work was caused by an 3) A. T. Ankus and R. D. Venter: Powder Technol., 73 (1992), No. 2,
increased available time for atomisation. Alloy additions of 169.
4%C to liquid iron increased the superheat in the furnace 4) Y. Kato: Int. Conf. on Powder Metallurgy for Automotive Components,
Science Publisher, Enfield, USA, (1997), 295.
from around 90 to 430°C. Model calculations indicated that 5) J. J. Dunkley: Powder Metall. Int., 10 (1978), No. 1, 38.
this raised superheat resulted in around 17 times longer 6) J. J. Dunkley and J. D. Palmer: Powder Metall., 29 (1986), No. 4,
287.
cooling times for atomised droplets, from the tundish tem- 7) E. Klar and W. M. Shafer: Int. J. Powder Metall., 11 (1975), No. 4,
peratures down to the liquidus temperature. It can be spec- 241.
ulated that the significantly longer cooling time at large 8) B. Bergquist: Powder Metall., 42 (1999), No. 4, 331.
9) L. Eriksson, E. Johansson, N. Kettaneh-Wold, C. Wikström and S.
superheats may improve the secondary atomisation of pri- Wold: Design of Experiments, Principles and Applications, Umetrics
mary atomised ligaments. This could contribute to a reduc- AB, Umeå, (2008), 75, 417.
10) J. O. Andersson, T. Helander, L. Höglund, P. F. Shi and B. Sundman:
tion of the particle size. Calphad, 26 (2002), 273.
11) Y. Chung and A. W. Cramb: Metall. Trans. B, 31B (2000), 957.
12) T. A. Engh: Principles of Metal Refining, Oxford University Press,
Acknowledgements New York, (1992), 62.
Special thanks are given to H. Gadmar, L. Boo, M. 13) R. I. L. Guthrie: Engineering in Process Metallurgy, Oxford University
Augustsson and M. Olsson for all their help and support dur- Press, New York, (1992), 483
14) M. J. Assael, K. Kakosimos, R. M. Banish, J. Brillo, I. Egry, R.
ing the pilot scale tests. M. Cengiz is also gratefully Brooks, P. N. Quested, K. C. Mills, A. Nagashima, Y. Sato and W.
acknowledged for all his input and help during this study. A. Wakeham: J. Phys. Chem. Ref. Data, 35 (2006), 286.
15) R. N. Barfield and J. A. Kitchener: J. Iron Steel Inst., 180 (1955),
Many thanks are also given to O. Litström, M. Berntsson, 324.
H. Grosser, A. Heinrich and O. Bergman, for their assistance 16) N. V. Vatolin, A. A. Vostryakov and O. A. Yesin: Fizika Met., 15
during the design and evaluation of the experiments. (1963), 222.
17) J. Lee and K. Morita: Steel Res., 73 (2002), No. 9, 367.
18) M. G. Frohberg and T. Cakici: Arch. Eisenhuttenwes., 49 (1978), No.
Nomenclature 5, 229.
19) A. J. Yule and J. J. Dunkley: Atomisation of Melts, Oxford University
AD: apparent density/g cm–3 Press, New York, (1994), 26.
aO: oxygen activity in the steel 20) R. J. Grandzol and J. A. Tallmadge: Int. J. Powder Metall., 11 (1975),
aS: sulphur activity in the steel No. 1, 103.
21) O. S. Nichiporenko: Sov. Powder Metall. Met. Ceram., 15 (1976),
cM: specific heat of liquid metal/J kg–1 °K–1 No. 9, 665.
d50: mass median particle size of as atomised powders/ 22) A. F. Sanin and O. S. Nichiporenko: Sov. Powder Metall. Met.
Ceram., 27 (1988), No. 9, 677.
μm 23) F. Persson, A. Eliasson and P. Jönsson: Powder Metall., 55 (2012),
dd: metal droplet diameter/m No. 1, 45.
24) Y. F. Ternovoi and O. S. Nichiporenko: Powder Metall. Met. Ceram.,
DM/D0: relative melt stream diameter 32 (1993), No. 1, 1.
H/H0: relative water level in atomising tank 25) Y. F. Ternovoi, O. S. Nichiporenko, V. N. Makogan and V. I. Bilan:
h: heat transfer coefficient, metal droplet to atmo- Powder Metall. Met. Ceram., 32 (1993), No. 2, 99.
26) H. Kishidaka: Proc. Multidisciplinary Meeting on Sintered Metals
sphere/W m–2 °K–1 and Magnetic Properties, Japan Society for Powder and Powder
J: water jet configuration/A = –1, B = 1 Metallurgy, Kyoto, (1972), 19.
27) T. H. Wang, W. H. Lee and W. C. Liu: China Steel Tech. Rep., 7
k: model constant (1993), No. 7, 98.
KO: adsorption coefficient for oxygen 28) B. J. Keene: Int. Mater. Rev., 33 (1988), No. 1, 1.