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Materials Science and Engineering A 383 (2004) 1–6

Atomization process for metal powder


Stanislav Lagutkin b,∗ , Lydia Achelis a , Sheikhali Sheikhaliev b ,
Volker Uhlenwinkel a , Vikas Srivastava a
a University Bremen, SFB372, Badgasteiner Str. 3, 28359 Bremen, Germany
b NPI MIFI Uralnetramm, Lenin Str. 85, Novouralsk, Sverdlovsk Region 624133, Russia

Received 27 January 2004

Abstract

A new atomization process has been developed, which combines pressure and gas atomization. The melt leaves the pressure nozzle as
a hollow thin film cone. After the pre-filming step, the melt is atomized by a gas stream delivered by a ring nozzle. The objectives of this
investigation are to achieve a narrow size distribution and low specific gas consumption compared to conventional gas atomization techniques.
Both lead to a higher efficiency and low costs. Tin and some alloys have been atomized successfully with this technique. The mass median
diameters from different experiments are between 20 and 100 ␮m. Sieving analysis of the tin powder shows close particle size distributions.
© 2004 Elsevier B.V. All rights reserved.

Keywords: Melt atomization; Conical film; Tin powder

1. Introduction Recent developmental attempts [5] have been focused on


overcoming the problem of wide size distribution for the
Challenges in the growing metal powder market are to close-coupled atomization. It was observed that the melt film
improve conventional atomization techniques and to de- at the nozzle tip was not stable. Hence, a slotted nozzle was
velop new atomization processes with better productivity introduced, since slots at the nozzle tip maintain the thin film
and economy. Water atomization [1] is one of the eco- of the melt more stable and lead to enhanced the particle
nomical processes, but this technique is not suitable for size distribution.
the production of spherical and clean powders. For this This paper presents a new atomization technique [6],
purpose, different techniques, such as ultrasonic capillary which combines the centrifugal hydraulic atomization
wave atomization [2], rotating disk atomization [3], and gas (CHA) [7] with gas atomization. Here, a conical molten
atomization, and in particular, close-coupled atomization metal film is atomized by high velocity gas jets. In the
[4] are used. The close-coupled gas atomization technique absence of atomizing gas, melt atomization will produce
is characterized by its high mass flow rate, and therefore, it larger mean particle sizes (d50 > 200 ␮m). Smaller mean
is frequently used for production of metal powders with a particle sizes with a narrow size distribution and low spe-
mass median diameter ranging from 10 to 100 ␮m. How- cific gas consumption are the main goals of this technique.
ever, the particle size distribution is quite wide and the A comparison with other atomization techniques would be
specific gas consumption is high. In addition, generally, desirable, but this has to be done very carefully. Data from
only a fraction of the raw metal powder can be used as a literature cannot be used for comparison purposes because
product. Larger and smaller particle size ranges must be the raw powder has to be analyzed with the same equip-
separated, and this reduces the productivity of the process. ment. This problem will be discussed in light of the results
A wide particle size distribution of the raw metal powder from this investigation.
means a low productivity.

2. Principle of the new atomization technique


∗ Corresponding author.
E-mail addresses: sheichali@npi.novouralsk.ru (S. Sheikhaliev), The new atomization technique uses a conventional pres-
uhl@iwt.uni-bremen.de (V. Uhlenwinkel). sure nozzle [7]. A pressure difference of up to 1.0 MPa

0921-5093/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2004.02.059
2 S. Lagutkin et al. / Materials Science and Engineering A 383 (2004) 1–6

Fig. 1. Schematic of CHA. (a) Cross-section of the conical film; (b) photograph of CHA with tin alloy; and (c) schematic representation of the new
atomization technique.

pushes the molten metal into a swirl chamber where it flows the gas nozzle, and design of the gas nozzle). Fig. 2 shows a
in until it is pressurized enough to leave the pressure noz- few examples of laser light sheet pictures. The bright zones
zle through a small cylindrical hole. At the exit, a conical mark the water film and the atomized particles. The water
thin film is generated due to the centrifugal force (Fig. 1(a)). film leaves the nozzle at the top of the pictures and builds
The film thickness decreases in the flow direction. Fig. 1(b) a conical film, which is atomized by the gas stream (white
shows a photograph of the CHA process, when the melt arrows are used to mark the exit of the gas stream and the
leaves the pressure nozzle. After 10–15 mm travel at the cone initial flow direction). Generally, discrete jet nozzles (ax-
surface, the continuous thin film starts breaking up forming ial array of cylindrical holes) were used at different axial
small holes. This leads to detachment of large ligaments. The impingement angles (−15◦ , 0◦ , +15◦ ). It can be seen how
thin film offers an ideal surface for efficient disintegration different gas flow directions affect the apical angle of the
into small droplets by high velocity gas jets. A schematic conical water film. In addition, a ring-slit nozzle was used.
representation of this process is shown in Fig. 1(c). The laser light sheet picture shows that the water film is
The details of the atomization process are unknown and even more affected (Fig. 2(d)). It was observed that many
have not been investigated. To develop this process, initial droplets hit the gas nozzle, and this can cause serious prob-
experiments were carried out with water, instead of molten lems in the case of molten metal.
metal and air, instead of nitrogen. The goal of these experi- Measurements of the static pressure in the absence of
ments was to study the interaction between gas flow and liq- water flow give a better understanding of the gas flow. In
uid film. During this investigation, several parameters have Fig. 3, the static pressure relative to atmosphere (pa ) is
been varied (water flow rate, gas flow rate or gas pressure in plotted versus the axial distance z from the atomizer. The

Fig. 2. Laser light sheet pictures of water atomization with the new atomization technique, different gas nozzle designs, constant gas flow of 45 kg/h,
constant water flow of approximately 50 kg/h.
S. Lagutkin et al. / Materials Science and Engineering A 383 (2004) 1–6 3

300
CC +15
250 CC 0
CC -15
200
CC rgn
150
p-pa [kPa]

100

50

-50

-100

-150
0 5 10 15 20 25 30 35 40
z [mm]

Fig. 3. Static pressure minus ambient pressure versus distance z along the axis of the atomizer, for different gas nozzle designs exhibited in Fig. 2. (For
interpretation of the references to colour in this figure legend, the reader is referred to the web version of the article.)

pressure differences are very strong for the ring-slit nozzle, the atomizing medium. After atomization, the powder was
which indicates a strong effect on the water film. There is separated in several samples and analyzed with different
a subpressure of about −10 kPa in the vicinity of the melt methods (dry sieving, laser diffraction with wet dispersion:
nozzle (z = 0 mm) and an overpressure of about 25 kPa at BSM).
the stagnation point of the gas flow.

4. Results and discussion


3. Experimental procedure
Table 1 shows strong dependence of median particle di-
Table 1 summarizes the experimental parameters of the ameter on gas flow rate. Fig. 4 shows the particle size distri-
molten pure tin experiments. Different alloys (Sn61Pb39; bution (cumulative mass Q3 ) at different gas pressures. The
Sn62Pb36Ag2; CuSn15P5Ni4) were successfully atomized powder was wet-dispersed and the measurements were car-
with this technique, but will not be analyzed in this paper. A ried out with a laser light diffraction instrument (Coulter LS
static overpressure of 0.7 MPa on top of the melt forced the Particle Size Analyzer LS 130). Essentially, the particles are
melt through the pressure nozzle and led to a melt flow rate spherical, as shown in the SEM micrographs for two of the
of 185 ± 15 kg/h. Due to the investigations with water, the raw powders. However, there was a big difference between
gas nozzle with an angle of 0◦ was adopted for all experi- the mass median diameter measured by laser light diffrac-
ments. The atomization gas supply pressure, which directly tion and the sieving analysis of the dry powder. Fig. 5 com-
varies with gas flow rate, was the only parameter varied. The pares both measurements and shows that the mass median
gas flow rate varied in the range from 21 to 98 m3 /h. The diameter obtained from the sieving analysis is approximately
spray chamber was evacuated (2 kPa) and refilled with nitro- 15 ␮m larger in size. Further measurements are necessary
gen, reducing the oxygen content to between 10 and 50 ppm to find the reason for this difference in the mass median di-
before initiation of atomization. Nitrogen was also used as ameter. The following correlation between the mass median

Table 1
Experimental parameters and results
Number Run time, Pressure on Mass flow Gas pressure, Volume gas Gas-to-metal Mass median Mass median
t (s) top of the melt, ṀL pG −pa (MPa) flow rate V̇G ratio, GMR diameter diameter
melt, PL (kg/h) (m3 /h) (m3 /kg) (sieving), (BSM), d50,3
(MPa) d50,3 (␮m) (␮m)
5 181 0.7 199 0.2 27 0.14 150 –
6 187 0.7 193 0.4 45 0.23 98 85
3 188 0.7 191 0.6 62 0.33 61 47
8 209 0.7 172 0.6 62 0.36 67 49
7 192 0.7 188 0.8 80 0.43 54 39
2 206 0.7 175 1.0 97 0.56 – 23
4 S. Lagutkin et al. / Materials Science and Engineering A 383 (2004) 1–6

Fig. 4. Cumulative mass distribution Q3 for different gas pressures (pg −pa varied between 0.4 and 1.0 MPa) with SEM micrographs of the finest and
coarsest raw powder. Measurements conducted by laser light diffraction (wet dispersion). (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of the article.)

120,0

105,0

90,0
BSM d50,3

75,0

60,0

45,0

30,0
30,0 45,0 60,0 75,0 90,0 105,0 120,0
Sieving d50,3

Fig. 5. Comparison of size measuring techniques. Laser light diffraction (BSM) vs. sieving. (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of the article.)

size and the gas-to-metal ratio (GMR) was established:

d50,3 = C1 GMR−C2 (1)


180

where C1 and C2 are constants. 160

Fig. 6 shows the variation of mass median diameter with 140

gas-to-metal ratio for both methods of measurement (laser 120


d50,3 [µm]

light diffraction and sieving). Two correlation functions are 100


shown as well, using the same exponent C2 = 1.0. This 80
indicates that the exponent does not depend on the measuring 60 Sieving

method. Further experiments with increased gas flows will 40 BSM


show how much the particle size can be reduced. 20
Even more important than the mass median diameter is 0
the standard deviation of the particle size distribution. In 0,0 0,1 0,2 0,3 0,4 0,5 0,6

this investigation, the diameter ratio between d84 and d50 GMR [m³/kg]
was used to characterize the width of the particle size distri-
Fig. 6. Mass median diameter vs. GMR for two measuring techniques
bution. Again, the results of both measuring techniques are (sieving, BSM: laser light diffraction). (For interpretation of the references
presented versus the gas-to-metal ratio (Fig. 7). A correla- to colour in this figure legend, the reader is referred to the web version
tion between the diameter ratio and the gas-to-metal ratio of the article.)
S. Lagutkin et al. / Materials Science and Engineering A 383 (2004) 1–6 5

3,0 200
= 1.5
/%

Sieving = 1.75
180
2,5 BSM = 2.0
d84,3 / d 50,3 [-]

160 = 2.25
= 2.5
productivity / productivity

2,0 140

120
1,5
100

1,0 80
0,1 0,2 0,3 0,4 0,5 0,6
GMR [m³/kg] 60
20 25 30 35 40 45 50
Fig. 7. Diameter ratio d84 /d50 vs. gas-to-metal ratio GMR for sieving d50 / µm
analysis method and laser light diffraction method (BSM). (For inter-
pretation of the references to colour in this figure legend, the reader is
Fig. 9. Relative productivity vs. mass median diameter for different geo-
referred to the web version of the article.)
metric standard deviations (σ).

can be neglected for the sieving and diffraction measurement


as well. But, the mean values are quite different. While the The calculation has been done for a size range of 25
diameter ratio for the laser diffraction measurement (BSM) to 45 ␮m, which is typical for “type 3” solder powders.
is approximately 2.0, the sieving analysis gives a value of Fig. 8 shows the yield versus the mass median diameter
approximately 1.6. A narrow size distribution is interesting for different geometric standard deviations (σ). Each curve
because this also implies a higher productivity. Due to rea- shows an optimum when the median diameter is approxi-
sonable differences in the results (sieving and laser diffrac- mately 35 ␮m. This optimum is not very distinct for high
tion) a comparison with published results achieved by other standard deviations, however, it becomes more important
atomization methods is not helpful. A comparison will only when the standard deviation decreases. Low standard devi-
be useful if the powders were analyzed by the same tech- ations are very important for the yield. Standard deviations
nique. of 2.25 are typical for gas atomization. The yield will in-
crease if it is possible to achieve a standard deviation below
1.75.
5. Effect of mass median diameter and geometric Exactly similar curves are obtained for the relative pro-
standard deviation on productivity ductivity (Fig. 9). Starting with a standard deviation of 2.25
the productivity will increase approximately 40 or 80%, if
The relation between productivity, mass median diame- the standard deviation can be reduced to 1.75 or 1.5. Again,
ter and geometric standard deviation can be calculated. For this example shows how important it is to find atomization
this calculation a log-normal particle size distribution is as- techniques with high production rates and narrow particle
sumed, which means that d84 /d50 = d50 /d16 [8]. size distributions.

60
55
= 1.5
= 1.75
50
= 2.0
45 = 2.25
Yield / %

40 = 2.5

35

30

25
20
20 25 30 35 40 45 50
d50 / µm

Fig. 8. Yield of the size range 25–45 ␮m vs. mass median diameter for different geometric standard deviations (σ).
6 S. Lagutkin et al. / Materials Science and Engineering A 383 (2004) 1–6

6. Summary References

A new atomization technique combining a pressure noz- [1] E. Klar, J.W. Fesko, Gas and water atomization, in: E. Klar (Ed.),
zle (centrifugal hydraulic atomization) and a gas nozzle was Metals Handbook, vol. 7, ninth ed., Powder Metallurgy, American
developed. This technique was refined by observations of Society for Metals, Metals Park, OH, USA, 1984, pp. 25–39.
[2] R. Ruthardt, E.G. Lierke, A new ultrasonic atomization technique for
flow patterns by laser light illumination and measurement the production of metal powder, in: H.H. Hausner, H.W. Antes, G.D.
of the static pressure in the vicinity of the melt exit. For the Smith (Eds.), Modern Developments in Powder Metallurgy, vol. 12,
first time, molten metals (pure tin and some alloys) were MPIF, Princeton, NJ, USA, 1981, pp. 105–111.
atomized successfully with this new method, using differ- [3] R. Anderson, Int. J. Powder Metall. 26 (2) (1990) 171–178.
ent gas flow rates. The tin powder was analyzed by sieving [4] A. Lawley, Atomization: The Production of Metal Powders, MPIF,
Princeton, NJ, USA, 1992.
and laser light diffraction. Both measuring techniques de- [5] I.E. Anderson, R.L. Terpstra, S. Rau, Progress toward understanding of
liver different results for the mass median diameter (d50 ) and gas atomisation processing physics, in: K. Bauckhage, V. Uhlenwinkel
the characteristic size distribution (d84 /d50 ) as well. The de- (Eds.), Spray Forming, Kolloquium Band 5, Books on Demand GmbH
crease in median particle size with increasing gas flow rate (ISBN 3-88722-508-2), Norderstedt, 2001, pp. 1–16.
[6] S. Lagutkin, S. Sheikhaliev, V. Uhlenwinkel, L. Achelis, S. Evers,
can be described by a negative exponential law. For compar-
Verfahren und Vorrichtung zum Herstellen von Metallpulvern und
ison with other atomization techniques it is necessary to use Keramischen Pulvern, Patent application no. DE 102 37 213.6, B 22
the same methods to analyze the metal powder. The siev- F 09/08, 14 August 2002.
ing analysis shows a larger median particle diameter which [7] J.J. Dunkley, S.M. Sheikhaliev, Single fluid atomization of liquid
is approximately 15 ␮m larger than that measured by laser metals, in: Proceedings of the International Conference on Pow-
der Metallurgy & Particulate Materials, Seattle, USA, 14–17 May
light diffraction and a much better diameter ratio (d84 /d50 )
1995.
of about 1.6. A narrow particle size distribution is the key [8] A. Yule, J. Dunkley, Atomization of Melts for Powder Production
parameter for high yield and productivity. These initial re- and Spray Deposition. Oxford Series on Advanced Manufacturing,
sults on the new atomization technique are encouraging, but Clarendon Press, 1994.
several developmental steps are necessary for the future.

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