Metallurgist, Vol. 58, Nos. 1–2, May, 2014 (Russian Original Nos.

1–2, January–February, 2014)

DEVELOPING A MOLD AND A METHOD FOR

COMPACTING TUNGSTEN POWDERS AND
TUNGSTEN-BASED COMPOSITE POWDERS

L. A. Barkov,1 S. A. Mymrin,2 UDC 621.722

M. N. Samodurova,1 and V. A. Ivanov1

The industrial technology which has been used since the beginning of the last century to make products
from tungsten powders is still complicated and involves multiple operations. The technology is time-
consuming because engineering studies that determine the parameters of the operations of compacting,
sintering, welding, and shaping the tungsten compacts need to be performed before the first large batch of
commercial products can be made. A factorial experiment showed that these operations can be made less
labor-intensive by constructing regression relations for the density of the powder, sample weight, and the
forces in the compaction process. New designs of molds have been developed together with a new method
of compacting tungsten powder.
Keywords: powder, tungsten, compaction, compact, mold.

Russian scientists P. G. Sobolevskii and V. V. Lyubarskii invented and introduced the process of compacting metal
powders in molds at the beginning of the Nineteenth Century. In 1826, they organized the industrial compaction of platinum
powder to make coins, medals, crucibles, cups, and other products.. Unfortunately, after Sobolevskii’s death, the process of
compacting powders in molds and powder metallurgy in general languished for almost 100 years.
The practice of compacting metal powders in molds experienced a rebirth at the beginning of the Twentieth Century
in connection with the rapid growth of the electrical industry. The production of electric lights required tungsten and molyb-
denum products that could only be made by powder metallurgy. American scientist W. D. Coolidge is considered the inventor
of processes and sectional molds for compacting powders of such refractory metals as tungsten and molybdenum. At the
beginning of the Twentieth Century, Coolidge – who was head of the research laboratory at the General Electric Company –
invented and later refined a technology for obtaining semifinished products (compacts) from tungsten and molybdenum pow-
ders and then using the compacts to obtain bars, rods, and wire [2]. Coolidge’s inventions were put to practical use in a tech-
nology developed by General Electric during the period 1905–1910.
Analysis of published research on the compaction process and mold design. As Coolidge noted in [3], the process
of compacting tungsten powder in molds is complicated and involves multiple operations. First of all, the powder must be
characterized by a high degree of chemical purity (with an impurity content no greater than 0.05%). The powder that is to
be compacted must have a certain granulometric composition, prescribed values for average particle size, and the necessary
shape, specific surface, and bulk density. To obtain a powder of the specified granulometric composition, the compaction pro-
cess must be preceded by mixing (averaging) of powders of different batches to obtain an average weight of 200–1000 kg.

1
South Ural State University, Chelyabinsk, Russia; e-mail: sm@susu.ac.ru.
2
PROMIN Scientific and Production Association, Chelyabinsk, Russia.

Translated from Metallurg, No. 1, pp. 68–75, January, 2014. Original article submitted July 12, 2013.

48 0026-0894/14/0102-0048 ©2014 Springer Science+Business Media New York

TABLE 1. Conditions for Pressing Tungsten Compacts at Foreign Companies [6]

Dimensions of Pressing force Density of compact,

Company, country Sample weight, g
compact, mm unit force total force g/cm3

RADIUM, Germany 10 × 10 × 320 170–180 51–54 300 10

12.5 × 12.5 × 290 600 215 550 12
PLANSEE, Austria
25 × 25 × 400 150–200 150–200 2800 11.2
6.5 × 6.5 × 200 100 13 190–200 10.7–12
GENERAL
10 × 10 × 300 170–180 50–53 280 9.6–10
ELECTRIC, U.S.
25 × 25 × 400 150–200 150–200 2800 11.0–11.2
12 × 12 × 240 – – 750 –

MUREX, 15.5 × 15.5 × 240 – – 1100 –

Great Britain – – 1750 –
– – 1800 –

According to [4], the average size of Russian-made tungsten powder of grades VCh and VA is 2–3 μm and particle size ranges
from 0.5 to 7 μm.
A second important operation in preparing powder for compaction is its plasticizing (moistening). Russian factories
usually use an ethyl alcohol solution of glycerin as the plasticizer, which reduces the frictional inter-particle and contact
forces in the powder as it is being compacted in the mold [5].
Since the beginning of the last century, the main industrial method used to compact tungsten powders and hetero-
geneous tungsten-based composite powders with ThO2, Y2O3, La2O3, and ZrO2 has been the unidirectional pressing of
square and rectangular compacts in sectional molds. Table 1 [6] shows the dimensions of square compacts and the forces cre-
ated during their pressing. The force conditions which exist during the pressing of compacts of certain sizes are kept within
specified ranges of values at a number of companies. The Murex company usually does not prescribe specific values for the
unit pressing forces metals for compacts of certain sizes. Instead, it only specifies the weight of the powder. The density of
the compacts is 49–61% of the theoretical density of tungsten for the given conditions.
Thus, it follows from the data in Table 1 that the method which has traditionally been used to compact tungsten pow-
ders yields compacts that are characterized by a high degree of porosity – 39–51%. However, the main shortcoming of this
technology is that substantiated values have yet to be established for the main kinematic, force-related, and other conditions
in the formation of compacts while also accounting for the granulometric composition of the powder, the average dimensions
of the particles, and their specific surface and bulk density. At factories that use compact technology, a 15–20-kg sample is
prepared from a large batch of powder before the production process is begun and is pressed into compacts, sintered, weld-
ed, and shaped while varying the process parameters. Wire is an example of one product for which this is done, and it is also
tested afterwards. The standard TI 48-4208-02-30–86, promulgated in the former USSR to make tungsten compacts, pre-
scribes a wide range of unit compacting forces for each size of compact made from tungsten powder:
8 × 8 mm compact 460–740 MPa
12 × 12 mm compact 350–550 MPa
14 × 14 mm compact 300–460 MPa
20 × 20 mm compact 260–300 MPa
Specific variants of the unit-force values for the compaction process are found by developing a “trial” technology
based on the granulometric composition of the powder, the average size of its particles in accordance with the Fisher criterion,

49
 Fig. 1. Disassembled mold for pressing tungsten compacts.

Fig. 2. Mold for pressing compacts: 1) jaws; 2) end plates (“blocks”); 3) bottom plate;
4) die; 5) connecting pins.

and bulk density. Having to create the trial technology significantly slows and complicates the process of optimizing the con-
ditions for the formation of compacts of tungsten powders and, in particular, heterogeneous composite powders.
The first mold for pressing tungsten compacts was developed in Coolidge’s laboratory in 1905 [7, 8]. This mold is
shown in disassembled form in Fig. 1 [9].
The mold consists of two sides, the die, connecting pins, and spring clamps. One of the sides contains a cavity to
hold the powder. The assembled and prepared mold, with the powder inside, is installed on a special hydraulic press equipped
with horizontal and vertical plungers. The horizontal plunger presses against the sides of the mold and then the vertical
plunger, acting through the die, compresses the powder to form the compact. A problem with the die was discovered during
its use at General Electric and companies in Europe. The elastic aftereffect of the compact would cause it to become jammed
in the die lengthwise after the load was removed. A special tool had to be used to extricate the compact from the mold cavi-
ty and often ended up causing it to crack.
A sectional mold designed in Russia (Fig. 2) was used at Russian plants in the 1950s to produce compacts from tung-
sten powder. Use of this mold partially eliminated the problem that had been encountered with the General Electric mold [5].
This mold is installed on a special press, which was described in the monograph [10]. The mold has to be disassembled after
the compact is made, and this requires the use of a drift punch remove the pins. Use of the punch is accompanied by vibra-
tion of the mold, which in turn causes some of the microscopic defects in the highly porous compact to be converted into
macroscopic defects that subsequently lead to fracture of the compact during ensuing stages of processing.
Thus, the goal of the investigation being discussed in this article was to conduct factory tests and analyze the results
in the form of a factorial experiment in order to construct regression relations that describe the dependence of the density and

50
TABLE 2. Main Characteristics of the Initial Tungsten Powders

Bulk Average Specific surface Tap Content of impurities (no greater than), %
Grade of
density ρb, grain in the MTD density,
tungsten
tons/m3 size, μm method, m2/g cm3/100 g Mo Fe Al Si Ca Na O2

4.29 3.35 – 14.0 – – – – – – –

VCh 4.55 4.10 – 14.5 – – – – – – –
5.18 4.55 – 12.5 – – – – – – –
2.24 4.90 0.10 – 0.017 0.004 0.002 0.005 0.004 – –
VA 2.61 – – – 0.025 0.004 0.002 0.004 0.003 0.003 0.38
2.83 4.68 0.11 – 0.030 0.004 0.002 0.005 0.004 0.004 0.35

TABLE 3. Parameters in the Pressing of Compacts of VCh Tungsten and VA Tungsten

Parameters of the powder Dimensions of compact, mm Average

Weight of Unit pressing
Pressing force, density of the
bulk density average grain compact pressure,
kN length height width compacts,
ρb, tons/m3 size, μm sample, kg MPa
tons/m3
VCh tungsten

1.020 441.62 2815.3 503 13.27 12.67 12.125

4.29 3.35
1.020 500.50 3190.7 503 13.03 12.66 12.320
1.030 382.73 2439.9 503 13.17 12.70 12.238
4.55 4.10 1.030 441.62 2815.3 503 13.01 12.69 12.451
1.030 500.50 3190.7 503 12.80 12.69 12.640
1.030 382.73 2439.9 503 12.94 12.67 12.527
5.18 4.55 1.030 441.62 2815.3 503 12.72 12.66 12.738
1.030 500.50 3190.7 503 12.51 12.66 12.922
VA tungsten
0.830 313.4 1922.3 504 12.21 12.17 11.445
2.24 4.90 0.880 451.1 2766.9 504 12.22 12.17 12.032
0.920 569.8 3494.9 504 12.05 12.17 12.533
0.830 284.9 1747.5 504 12.25 12.17 11.271
2.61 – 0.880 432.1 2652.2 504 12.19 12.17 12.034
0.920 569.8 3494.9 504 12.02 12.17 12.646
0.830 308.6 1892.8 504 12.19 12.17 11.405
2.83 4.68 0.880 432.1 2652.2 504 12.21 12.17 12.044
0.920 569.8 3494.9 504 11.99 12.17 12.602

height of the compacts on the bulk density of the powder, the weight of the powder sample, and the pressing forces. We then
wanted to use these results to develop improved mold designs and a new method of compacting tungsten powders.

51
 Finely dispersed tungsten powders of grades VCh and VA (Table 2) were used as the initial materials for a compre-
hensive in-factory study of the cold formation of compacts from tungsten powder. It can be seen from Table 2 that the bulk
densities of the VCh powder (4.29–5.18 tons/m3) and the VA powder (4.29–5.18 tons/m3) correspond to the actual density
ranges in the specifications of the technology.
Tungsten powders of different bulk densities were obtained by mixing coarse-grained and fine-grained powders
together in different proportions. For example, the grade-VCh tungsten powder with the lowest bulk density (4.29 tons/m3)
was obtained by mixing 30% coarse-grained powder with 70% fine-grained powder. Bulk density was determined on a volu-
mometer by the method described by GOST 19440–74. Before being pressed, the averaged tungsten powder was moistened
with a plasticizer (a 1:1 mixture of glycerin and alcohol). Compacts of these powders were obtained in sectional molds on
special P-801 or K25.033 industrial hydraulic presses, which have horizontal and vertical cylinders.
The dimensions of the cavity of the molds used to obtain compacts of VA and VCh tungsten: width 12.7 and 12.65 mm;
length 504 and 503 mm. The pressing force was measured at three points along the compact by using a specially designed
hydraulic capsule. We then chose the average of the three measurements. The height of the pressed compact was measured
with a micrometer at five points along the compact. To strengthen the compacts before their dimensions and density were
measured, they underwent low-temperature sintering in continuous muffle furnaces. The sintering was done in hydrogen at
1200°C over a period of 1 h. The dimensions and density of the pre-sintered compacts were almost identical to the dimen-
sions and density of the pressed compacts. The density of the pre-sintered compacts was measured with a radioisotope den-
simeter designed by the Chirchinsk affiliate of the All-Russia Research Institute of Hard Alloys (VNIITS). We performed the
measurements at six points along each compact and took the average of the resulting values. The weight of the powder sam-
ple used to obtain each compact was checked on a balance.
The results obtained from in-factory study of the cold pressing of tungsten powders were analyzed in the form of a
factorial experiment. The variable parameters: bulk density of the tungsten powders ρb; unit pressing force p; weight of the
powder sample used to obtain a compact m. The density of the compact ρ and its height h were determined as the response
function. Table 3 shows the results obtained from studying the pressing of tungsten powders of grades VCh and VA.
To predict the density characteristics of the tungsten compacts, we constructed regression relations that describe the
dependence of the density and height of the compacts on the bulk density of the powder, the weight of the powder sample,
and the unit pressing forces.
The form of the equations was chosen after comparing several variants that were combination of power functions
and exponential functions. The comparison was made on the basis of the residual variance and the coefficient of multiple
determination. The unknown parameters were evaluated by Marquardt’s method [11] with the use of a standard computer pro-
gram that constructs nonlinear regression relations. As a result, we obtained the following regression equations:
for tungsten of grade VCh
r = 4.7054 + 0.00017p – 4.2872e–0.1486rb; (1)

h = 14.139 – 0.0035p + 2198.62e–36.5771rb; (2)

for tungsten of grade VA

r = 4.0757 + 0.00025p – 4.9388e–0.139rb + 1.4166e–0.0432m; (3)

h = 6.1935 – 0.0445p – 1.7506e–0.6324rb + 11.1803m, (4)

where r = ρ/ρc, rb = ρb /ρc are the relative values of the density of the compact and the bulk density of the powder (ρc = 19.3
tons/m3 – the density of the compacted tungsten).
Regression equations (1)–(4) were used to construct density–pressure graphs for VCh and VA tungsten powders with
different bulk densities (Fig. 3).
It can be seen from Fig. 3 that these relations are linear in character. Meanwhile, the effect of the bulk density of the
powder on unit pressing pressure is greater for VCh powder than for powder of grade VA.

52
 ρ, tons/m3 r
13 0.670 12.6
0.650
3 12.4 0.640
12.7 0.655
12.2 1 0.630
2 3
12.4 0.640 12 0.620
2
1 11.8 0.610
12.1 0.625
11.6 0.600
11.8 0.610 11.4 0.590
380 420 460 500 320 380 440 500 560
p, MPa
a b

Fig. 3. Dependence of the density of the compact on the unit pressure in the pressing of tungsten: a) grade VCh
(1 – ρb = 4.29 tons/m3; 2 – ρb = 4.55 tons/m3; 3 – ρb = 5.18 tons/m3); b) grade VA (1 – ρb = 2.24 tons/m3;
2 – ρb = 2.61 tons/m3; 3 – ρb = 2.84 tons/m3).

Fig. 4. Mold for the compaction of powders.

Let us illustrate the use of Eqs. (1)–(4) in the industrial pressing of powder compacts by using compacts of VA tung-
sten as an example. First we designate ρo as the optimum density of the compact and ho as the optimum height. Then we take
Eqs. (3) and (4) and insert the specified bulk density of the initial powder rb and values of ρo and ho.
System of equations (3) and (4) has only two unknowns – p and m. Solving this system, we determine the values of
unit pressure p and sample weight m that are optimum from the viewpoint of obtaining compacts of the height ho and densi-
ty ρo from powder having the bulk density rb.
System of equations (3) and (4) was solved for VA-grade tungsten by a numerical method. As an illustration, the
results for the specific case h = 12.2 mm, m = 0.874 kg are shown below:

ρb 2.20 2.30 2.40 2.50 2.60 2.70 2.80 2.90 3.00

rb 0.114 0.119 0.124 0.129 0.134 0.139 0.145 0.150 0.155
p, MPa 469; 422 465; 421 464; 419 462; 418 461; 417 460; 415 459; 414 457; 413 455; 412

53
 Fig. 5. The configuration of a multi-station mold before (a) and after (b) the pressing operation [16].

Improving the design of the molds and developing a new method of compaction. To eliminate the design flaws of the
molds shown in Figs. 1 and 2, we designed several new molds for obtaining compacts from powders of refractory metals
[12–3]. The new mold designs are protected by patents.
The molds [12–14, etc.] are intended for use at factories that have specialized hydraulic presses with vertical and
horizontal cylinders. One example is the 520-ton-f P-801 press made by the Odessa Press Factory [10]. Figure 4 shows one
design of presses of this type.
The press works in the following manner. The metal powder is poured into the mold cavity, which is formed by the
two sides 1 and two plates 2. The powder is leveled and the die in place on top of it. Then the mold is placed on the working
platen of the specialized press. The jaws 1 and plates 2 are brought together before the powder begins to be compacted by
the force exerted by the horizontal cylinder (Ph). Here, pins 3 compress elastic elements 4. After the powder has been com-
pacted and the forces from the vertical and horizontal cylinders have been relieved, elastic elements 4 open up the mold cav-
ity and free the compact. The use of such molds at factories that employ compact technology to shape powders has solved
the problem of extricating the compact and increased usable output.
Original designs of molds [15, 16, etc.] were developed for factories that do not have specialized presses with side
clamps but do use compact technology. These molds can be installed on automated presses designed to compact powder.
Figure 5 shows a diagram depicting a multi-station mold before the pressing operation (a) and at the moment it ends (b) [16].
The mold works as follows. The tungsten powder is poured into the three open cavities of the mold when the latter
is in its initial state. At this point, the top end of the die 1 and the ends of bushings 6 are in the same plane. The powder is
leveled after being poured into the cavities. The Russian-made automatic hydraulic press (model DB1240 [17] is one such
press) is then turned on, the mold is placed on its platen, and the force Pv is applied to die 2. During the compression of the
powder of the compact 7, bushings 6 descend and compress elastic elements 5 located between the bottom dies 4 in the press
housing 3. The multi-station press increases the productivity of the compact-forming process several-fold.
However, when automated presses are used instead of presses having with side clamps, problems develop with the
pressability of the powders and the removal of gases and vapors from the powder during the compaction process. In presses
with side clamps, these problems are eliminated by reducing the speed of the top die to 2.5 mm/sec [17]. The compactibili-
ty of the tungsten powder remains satisfactory at this low speed, and there is enough time for most of the gas and vapor to
escape the compact through the gaps (roughly 150 μm wide) between the punch and the walls of the die. In modern foreign
and Russian-made automated presses designed for compacting powders, the punch rarely moves at speeds below 10 mm/sec.
In connection with this, special studies that included factory tests [18] were performed to improve the pressability and com-
pactibility of tungsten powders. It was found that the pressability and compactibility of powder mixtures can be increased
sharply by adding 0.04–0.06-μm nanoparticles obtained with the use of a high-temperature plasma to a standard tungsten
powder (such as grade VA) having a particle size of 1–5 μm. Such a measure decreases the compacting force 35–40% and

54
 Fig. 6. Diagram of a mold with movable sides [21]: a) in the initial position; b) after the pressing operation.

increases the speed of the punch during the pressing operation. A new method of obtaining tungsten compacts from mixtures
containing nanopowders was developed based on the results of factory tests. The method is now protected by a patent [19]
and has been made the basis of a technology that is currently under development.
It is known [20] that the surfaces of the particles which comprise powders of tungsten and such refractory metals as
niobium, tantalum, and molybdenum readily adsorb gas and vapor particles at low temperatures. The adsorbed particles
reduce the pressability and compactibility of the powders. If they remain inside the powders, then after the forces are removed
the pressed compacts will either fracture immediately or have macroscopic defects form in them.
To remove adsorbed particles from the surface of particles comprising powders of tungsten and, in particular, mix-
tures of standard tungsten powders with nanoparticles – which present a very large contact surface for absorption – we have
invented molds equipped with sides that can be moved prior to the compaction operation. The mobile sides apply a force to
the powder in the mold cavity before application of the pressing force and remove particles of gases and vapors from the par-
ticles of the powder [21–23, etc.].
Figure 6 shows a schematic diagram of a mold which has sides that move before the application of the force that com-
presses the powder to form the compact. The mold works as follows. The powder is poured into the cavity formed in the hous-
ing 1 by the sides and end plates 4 and 5. The drive of the clamping slide-block 3 of the dual-acting press is turned on. Moving
downward, the slide rotates plates 4 and 5 about shafts 9 under the force Ps created by the contact between beveled surfaces 6
and 7. Plates 4 and 5 act on the powder located between them as they rotate, forcing gases out of the powder and subjecting it
to preliminary compaction. Since the cavity has not yet been closed from above by the main die 2, the gas and vapor particles
in the powder freely escape through a gap 10 that communicates with the atmosphere. The drive of main die 2 is turned on after
degassing and pre-compaction have ended, and the force Po exerted by the die compresses the compact 8. The angle of rota-
tion of plates 4 and 5 and, thus, the amount of degassing and pre-compaction that take place are controlled by means of
eccentrics 11 as a result of rotation of shafts 12. After the pressing operation is completed, die 2 is raised and clamping slide-
block 3 is retracted. This causes the elastic recovery elements 13 to move plates 4 and 5 back to their original position.
Conclusions. Thus, the findings of foreign and Russian experimental research on the compaction of tungsten powder
were analyzed and designs of sectional molds made in the U.S., Europe, and Russia were examined. The distinctive features
and shortcomings of each of the molds were discussed.
The results of a factorial experiment performed with data from factory tests of tungsten powders of grades VCh and
VA were used to construct regression equations and graphs that characterize the dependences of the density and height of the
compacts on the bulk density of the powders, the weight of the powder samples, and the compacting forces in the molds.
Practical use of the analytical and graphical relations has reduced the amount of time required to develop a “trial” technolo-
gy for determining the kinematic, force-related, and other parameters in the formation of compacts from tungsten powders.

55
 Original (at the inventions level) designs of sectional molds have been developed (and conferred with over 20
patents) for use on specialized presses with side clamps, automatic presses employed in powder metallurgy, and dual-action
presses. Some of the above-described molds are now being used in factories.
A new method was also developed and patented to obtain high-density compacts from tungsten-based composite
powders that contain 0.04–0.06-μm nanoparticles. The powders exhibit a high level of pressability in the compaction opera-
tion, which is carried out with a faster-moving die and 35–40% lower pressing forces.
This investigation was conducted in conjunction with the Federal Targeted Program on Research and Development
in Priority Areas for Growth of the Scientific-Industrial Complex in Russia during the Period 2007–2013 (State Contract
No. 14.513.11.0088 from 06.21.2013).

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