POWDER-METALLURGY INDUSTRY, ECONOMICS AND ORGANIZATION

OF PRODUCTION

PRODUCTION OF COPPER POWDER AT THE ALAVERDY MINING

AND METALLURGICAL INTEGRATED WORKS

N. S. Sarkisyan, O. S. Nichiporenko, M. Z. Kol'chinskii,

E. P. Pokotilo, B. I. Bondarenko, and A. N. Karibyan UDC 621.762

The technology of producing copper powders by the method of atomizing the melt by water under high pressure, worked
out at the Institute of Materials Science of the Academy of Sciences of the UkrSSR and introduced at the Alaverdy Mining and
Metallurgical Integrated Works, makes it possible to obtain powders with specified chemical composition with particles of
certain size and shape, which upon compaction ensures good quality of the finished product.
Dispersion of the liquid metal is attained by impact of a water stream under high pressure. Although considerable
energy dissipation reduces the efficiency of the process to 1-2%, this method plays an important role in the industrial production
of powders, both from the technical and the economic point of view. Powders obtMned by water atomization consist, as a rule,
of particles with irregular shape and with a rough oxidized surface. It was shown in [1] that between the mean particle size of the
powder dp and the speed of the water stream W w there exists the empirical correlation:

ep = A / % . (1)
It was established by further investigations that in the control of the particle size the dominating factor is the normal component
of the velocity vector of the water stream, i.e., W w sin a, where a is the angle between the jet of the melt and the jet of water [2]:

dp = A/(Ww sin sO. (2)

In the process of atomization the melt interacts with the water so that oxide of the metal forms. The intensity of the
interaction depends on the conditions of atomization and on the properties of the metal. When products for electrotechnical
purposes [3] are to be obtained, the oxygen content of the copper powder must not exceed 0.08-0.1%.
At the Alaverdy Mining and Metallurgical Integrated Works the production technology of copper powders by water
atomization of the melt with subsequent reducing annealing was introduced. At the stage of industrial trial runs the decisive
parameters of the process and their effect on the properties of the powders were discovered. A basic technological flow chart of
the process is presented in Fig. 1.
Let' us consider the main parts of the technological cycle, viz., atomization and annealing because they, in particular,
determine the eventual properties of the powder. Atomization is effected by water under high pressure (12-14 MPa) with a flow
rate of up to 20 m3/h. The melt flows out through a hole with 8-9 mm diameter at a speed of 2-3 m/sec. The speed of the water
is 150-170 m/sec. As a result of numerous experiments we obtained the most important correlations between the process
parameters and the properties of the powder (Table 1).
The most important characteristics are the strength of the raw compact, formability, particle size of the powder, and also
its oxygen content, which determine the suitability of the powder for making products from it. Under industrial conditions three
alternatives of the production technology of the powders were tested: atomization of the melt (batch I), atomization of the melt
with subsequent reduction annealing of the raw powder (batch II); atomization of the melt with intermediate oxidation and
subsequent reduction of the powder (batch III). The aim of the experiment was to work out and master the production technolo-
gy of high-quality powder with minimal oxygen content, good strength characteristics of the raw compact, and formability.

Institute of Materials Science, Academy of Sciences of the Ukrainian SSR. Translated from Poroshkovaya Metallurgiya,
No. 5(341), pp. 91-95, May, 1991. Original article submitted July 11, 1989.

432 0038-5735/91/3005-0432512.50 9 Plenum Publishing Corporation

 i Recycledproduct l i Charcoal I
i. I I
JWeighing andl~ ' J Weigh~n~ J
icomposition J J J . . . . ~---= |
J of charge_J I ~
+ ' Jl, . , I IMixingwithfreshi~
, ,
[~ Melt ,High-pres:ure water I r Dust'-~
J~
"~ jI 'I Slag+ . ~ j latomization, of copperI ~
~l ' J Dehydration ~ - - ~ ~
jDrying with~oxidationJ
! Classification J bccumulatio

*
+
l T
I Grinding I *
+ IFraction+~f] +~g77]--~0711
J Passivation
+ ~ccumulationacc.to fractions I
I Classification + r

1 J Batching acc. to fractions 1

j Fraction +0.16 J J Mixingof fractions I
I Pelleting 1 J Batching
l w evacuation
iandt packing
h
j Recycled product J J Finishedproduct '1

Fig. I. Basic technologicalflow chart of the production of copper powders by high-pressure

water of melts.

TABLE 1. Effect of the Process Parameters on the Principal Properties of

Powders

Parameter Particle S hericity ulk densit Oxygen

size P content

Water pressure ~ ~
Water flow rate # ~
Outflow speed of water ~ ~ ~
Flow rate of melt ~
Diameter of jet of melt
Temp. of melt ~ ~ ~
Surface tension ~ ~ ~
Angle of attack ~ ~

The process of atomization was described in sufficient detail in [4, 5]. The powder is oxidized at the time of drying in a
tubular dryer in an ascending stream of a mixture of air and the combustion products of natural gas. The temperature of the
powder at the outlet from the tubular dryer is 1500C, and its oxygen content is approximately 0.5%. At the Alaverdy Mining and
Metallurgical Integrated Works the copper powder is annealed in a pusher furnace STN-2,5 that was substantially reconstructed.*
The furnace is provided with a hermetic stainless-steel muffle, tubular nichrome spiral heaters, a loading chamber with gas
protection in analogy with the discharge chamber. Layers of powder 30-40 cm high are annealed in stainless-steel trays. The
reducing agent is endogas obtained on an installation I~N-60 which is operated at the ratio O/C = 1.5-1.6, which is the upper

*Reconstruction of the furnace STN-2,5 and its adjustment were carried out by staff members of the Gas Institute of the
Academy of Sciences of the UkrSSR.

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 Fig. 2. Particles of raw copper powder (a, b), atomized after annealing (c), oxidized after
atomization (d, e), and reduced after oxidation (f). Magnification: a, d, f) 300; b, c, e) 750.

limit of normal operation of the catalyst GIAP-8. With a higher ratio O/C the catalyst becomes overheated in the combustion
zone of the gas--air mixture and loses its activity. Excess moisture of the endogas condenses in the cooler of the gas-preparation
plant and is continuously removed through a water seal. Before being fed into the furnace the endogas had the following
composition, vol.%: 3.2-4.0 CO2; 14.5-15.8 CO; 24-26 H2; 1.2-1.5 H20; _<0.1 CH4; remainder N 2. We did not manage to com-
pletely prevent liberation of carbon upon contact of the gas with the muffle walls as catalyst. A small amount of soot settled
solely on the surface of the powder, not penetrating into the layer, and it was easily removed after the cake had cooled. The
cooled cake was comminuted in a pulping plant, classified, and packed with evacuation. Before packing samples were periodically
taken to determine the properties of the annealed reducing powder.
The investigations were carried out at 675-970~ in the annealing zone. When the temperature is low (<720 K), the
indispensable plasticity of the powder is not attained, and when the temperature is high (>850 K), firm cakes form which, when
comminuted, yield strongly work-hardened powders. By these regimes the required technological properties of the powder were
not attained. Powder of good quality was obtained by reducing annealing with 600-630 K in the heating zone, and 310-325 K at
the discharge. The throughput of the furnace with stable technological regime was 40-50 kg/h with holding for about 1 h in the
heating and annealing zones.
Altogether, including all the batches, about 3 tons of powder were produced. On representative samples we determined
the principal technological characteristics, and also the chemical composition of the powders (Table 2). Powder of batch III
(reduced after oxidation) has the best technological properties. Its bulk density is minimal, 2.4 ~ c m 3 with fairly good fluidity and
highest formability, viz., 4.7 g/cm 3. The oxygen content does not exceed 0.06%.
Immediately after atomization the particles of raw powder have a predominantly round shape and a fairly smooth surface
(Fig. 2a, b). Annealing immediately after atomization eliminates stress and changes the shape of the particles mainly as a result
of the adhesion of small particles to larger ones (Fig. 2c). At the same time the surface of individual particles and of the
conglomerate is somewhat loosened because of the reduction of the surface oxides. Oxidation of raw powder greatly changes the
surface, deforming it on account of the accretion of the mass of metal. The surface of each particle becomes raised (Fig. 2d, e)
but remains fairly dense. When oxidized powder is reduced, the relief of the particles is retained: the surface remains wrinkled
(Fig. 2f). However, thanks to the removal of oxygen the density of the surface layer is reduced, the particle becomes more
ductile. The nature of the change of the surface of the powder particles in the process of treatment is in good agreement with
the data on their technological characteristics (Table 2).
An additional series of experiments was carried out with specimens compacted from atomized powder of batches II and
III, and also of electrolytical powder marques PMS-1 and PMS-V at a pressure of 300-400 MPa, then sintered at 1000~ for 1 h.
All the specimens were calibrated at a pressure of 700 MPa.

434
 T A B L E 2. Technological Characteristics of Atomized and Electrolytical
Copper Powders

Content of
elements, ~ %
Particle-size I ~%[ ~ IO~,
Powder
(batch)
o 83
i' I:ol
PMR-I:
initial (I) 99,6 0,20 0,05 17,3 19,8 32,6 29,6 3,4 29 7,5 6,0 7,5
annealed ( I I )
oxidized 99,9 0,06 0,02 18,4 17,6 28,1 35,I 3,0 35 5,8 31,8 7,6
99,4 0,50 0,02 17,5 20,1 33,4 29,0' 3,5 . . . .
annealed after
oxidation (III)99,9 0,06 0,02 21,1 23,9 34,5 20,5 2,4 36 4,7 42,0 7,7
PMS-I 99,7 0,20 0,05 0,2 8,0 11,2 80,4 1,9 -- 5,2 39--40 7,2
PMS-V 99,8 0,I0 0,05 9,0 45,1 20,6 25,1 2,7 33 -- 60,0 7,6

*All the powders contained the same amount of iron (0.02%), arsenic
(0.005%), lead (0.05%), and tin (0.01%).
**At a compacting pressure of 400 MPa.

TABLE 3. Mechanical Characteristics of Specimens of Atomized and Electro-

lyrical Copper Powders

Density ]Relative[ Obend, Hardness, Resistivity,

after cal- 1 ~ ~'longa- I
Powder ibration, MPa ~cion, % 1 MPa HB ~'m
g/cm a I / I
PMR-I :
batch II 8,56 145 12,2 405 46,9 0,2
batch I I I 8,62--8,80 178--221 17--19 -- 7,60--78,0 0,180--0,182
PMS-2 8,78--8,85 220--224 9,4--14,3 670--805 76,3--80,4 0,186--0,193
203--229 9,6--12,4 -- -- --
PMS-V 8,73--8,82 250 8,3--9,7 709 76,3--80,4 0,188--0,194
PM$-I 8,78--8,81 241 17,5 670 76,3--74,1 0,182

The specimens from oxidized and reduced powder were distinguished by high ductility comparable with the analogous
characteristic of electrolytical powders (Table 3). Moreover, the specimens from atomized powders have greater porosity: 17-19%
as against 9-14% in electrolytical powders. The electrical resistivity of the powders (0.180-0.182).10 -7 ~-m is below the
permissible limit of 0.22-10-7 Q-m.
Thus the technology of obtaining high-quality powder for predominantly electrotechnical purposes was introduced at the
Alaverdy Mining and Metallurgical Integrated Works. The powder can be used successfully in the radio industry, in the chemical
and general engineering branches, and also in electronics.

LITERATURE CITED

1. R. I. Grandzol, Water Atomization of Steel and Other Metal. PhD., Drekel, Philadelphia (1983).
2. B. Champagne and R. Angers, "REP atomization mechanisms," Powder Metall. Int., 16, 125-128 (1984).
3. I. I. Dunkley, "The production of metal powders by water atomization," Powder Metall., 10, No. 1, 350-356 (1978).
4. O. S. Nichiporenko, S. S. Naboichenko, and A. V. Pomosov, Powdered Copper and Its Alloys [in Russian], Metallurgiya,
Moscow (1988).
5. O. S. Nichiporenko, "The state of the art in the production of metal powders in the USSR and prospects of their
application in the economy," Poroshk. Metall., No. 9, 1-11 (1990).

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