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Effect of Processing Methods and Die Design

Parameters on Green Properties of WC–Co Nanopowder
Pellets
a b
Devender Kumar & K. Singh
a
Mechanical Engineering Department, Thapar University, Patiala, Punjab, India
b
School of Physics and Materials Science, Thapar University, Patiala, Punjab, India
Published online: 15 Jun 2015.

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To cite this article: Devender Kumar & K. Singh (2015): Effect of Processing Methods and Die Design Parameters on Green
Properties of WC–Co Nanopowder Pellets, Materials and Manufacturing Processes, DOI: 10.1080/10426914.2015.1037903

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 Materials and Manufacturing Processes, 0: 1–13, 2015
Copyright # Taylor & Francis Group, LLC
ISSN: 1042-6914 print=1532-2475 online
DOI: 10.1080/10426914.2015.1037903

Effect of Processing Methods and Die Design Parameters on Green

Properties of WC–Co Nanopowder Pellets
Devender Kumar1 and K. Singh2
1
Mechanical Engineering Department, Thapar University, Patiala, Punjab, India
2
School of Physics and Materials Science, Thapar University, Patiala, Punjab, India

Non-uniform and unequal pressing of powder for making green pellet plays an important role in deciding structural properties of
sintering pellets. Various parameters like surface roughness of the die, die-plunger clearance, and flatness of plunger/anvils are among
the most important parameters to be taken care in making a proper die set. This paper presents a comparative study on quality of pellets
formed using four different types of uniaxial powder compression dies with two different processing techniques. In the present study, it has
been observed that the quality of pellet depends largely on the internal surface finish of die barrel, flatness of anvils and the clearance
between die barrel-plunger/anvil, and the processing of powder before compression.
Downloaded by [Thapar University] at 22:19 15 June 2015

Keywords Carbide; Die-design; Green-strength; Nanopowder; Tungsten.

INTRODUCTION know the sensitivity of die design parameters on the

Processing parameter plays an important role, parti-
cularly in structural sensitive properties of solids [1, 2].
Apart from many other parameters, the compaction of
different type of powder depends largely on die-punch
shapes, finish, and pressure, etc. Professional die makers
have refined the overall design parameters over a long
period of time, but still they are unable to deliver
a correct combination of all the sensitive parameters
in one die at a reasonable cost. Most of the times, it
becomes a matter of experience and optimization with
which one can produce an acceptable quality pellet.
Quality of compressed pellet plays an important role
in electrical conductivity, compressive strength, hard-
ness, and other mechanical properties of the sintered
material. Various findings from a sintered pellet are
the basic building blocks for further optimization of
the material composition as well as sintering parameters.
Various defects like the end-capping, lamination, or
cracks in green pellet leads to poor sintering of pellets
with lower density, and higher porosity gives false values
of electrical conductivity or other mechanical properties
[2, 3]. In large extent, this important aspect of pellet
quality and die set parameters are not available
in published literature. Primary die design parameters
like surface roughness, die-plunger clearance, and
flatness of plunger=anvils are the essential quantitative
measures, which are to be specified by the researcher
to the die manufacturers. Along with that, one must
quality of ejected pellet. Most of the time, die manufac-
turers or suppliers are not aware of the overall motive
and sensitivity to the issues involved with the die set.
The aim of the present study is to demonstrate the
importance of basic design parameters with the help of
pellets made with four different die sets shown in Fig. 1
and Table 1. Efforts are also made to demonstrate
the best methods to be followed for pre-processing
of die sets, powder preparation, powder filling, pre-
compression, ejection of pellet, and ways to reduce
plunger travel for minimum friction offered during the
process of nanopowder compression. Few published
literature described the effect of lubricants and powder
size variation on the density variations and final density
achieved [4–10]. Most of the published work was studied
using powders having a particle size ranging from 0.5 to
250 mm. In coarse powder, die wall surface friction is less,
and low surface area reduces internal friction among
the powder particles during compaction. Whereas fine
powders having a particle size of 50–200 nm, offer high
friction with die walls as well as with neighboring parti-
cles. High loading pressure reduces the porosity of green
compact and two-stage compression gives better density
after sintering [11]. Pellets of nanopowder have better
green density than coarser powder of same material
under same compressive load [9–16]. Higher green den-
sity of the pellet leads to better properties for different
industrial applications.

MATERIALS AND METHODS

Received December 24, 2014; Accepted March 9, 2015
Address correspondence to K. Singh, School of Physics and
Materials Science, Thapar University, Patiala, Punjab, India; E-mail:
kusingh@thapar.edu.
Color versions of one or more of the figures in the article can be
found online at www.tandfonline.com/lmmp.
In conventional designs of die set-1, 2, and 3, die body
and plungers=anvils were made of steel. Plunger=anvils
of all the die set were cut from the stock material of
the desired diameter, and cross-section was manually
finished with carbide sandpaper. Cross-section, i.e.,

1
 2 D. KUMAR AND K. SINGH

FIGURE 1.—All parts of different die sets (a) Die set-1. (b) Die set-2. (c) Die set-3. (d) Die set-4.

the contact surfaces of the plunger=anvils were then
polished manually by rubbing abrasive paste. Usually,
the surface finish of conventional dies was poor and
not up to the desired level. Most of the time, the tool
marks were made by the drill bit during the process,
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Tungsten carbide nanopowder (particle size 55 nm) and
vanadium-carbide powder (particle size 600–800 nm) were
supplied by US Research Nanomaterials, USA. Whereas,
cobalt powder (particle size 2 mm) was supplied by Sigma
Aldrich, USA. All above materials have 99% purity. The

and clearly visible with naked eyes. Accuracy in
die-plunger tolerance, finishing of the die barrel, flatness
of the plunger=anvil contact surfaces, and perpendicu-
larity (Fig. 2.(a)), all depends upon the care and
knowledge of the die manufacturer.
Die set-4 was made by shrink fitting the tungsten
carbide blank into a die steel body. Tungsten carbide
was axially drilled, and then it was made up to the
desired internal diameter with wire cut electric discharge
machining (EDM). After boring, the die set-4 was
polished with the help of diamond paste to get a good
surface finish of the order of 0.004 mm. Anvils of the
die set-4 were made of tungsten carbide, which was
further a challenging task for surface grinding as tung-
sten carbide is nonmagnetic, and cannot be fixed on a
magnetic base of surface grinder. A special holder jig
was prepared for holding tungsten carbide anvil of
10 mm in diameter and 6 mm thick, as shown in
Fig. 2(b). Careful surface grinding with a fine grit car-
bide wheel gave us a better surface profile and a good
surface finish of the anvils. In the present study, the
effect of anvil surface profile, die surface finish, and
die-plunger clearance will be investigated.
powders were mixed mechanically in an agate mortar and
a pestle for 2 h, using 20 wt.% cobalt and 2 wt.% vanadium
carbide. Powder blend is then dried at 100 C in vacuum
oven for 1 h to remove any moisture present in the mix-
ture. Uniform distribution of tungsten carbide, cobalt
and vanadium carbide was verified by energy dispersive
spectroscopy (JEOL-JSM -6510, Japan). Figure 3 shows
the uniform distribution of all the powder constituents
across the cross-section of the pellet. Pellet density of a
powder blend of multi size particle found to be more as
compared to the compact made of same size particles,
so proper distribution of all variable size particles is essen-
tial to increase the green density of the pellet [17–19].
The dried powder was again ground for 4 to 5 minutes
in an agate mortar and a pestle, to crush particle
agglomerate present in the mixture. It becomes easy to
fill die cavity more uniformly, which produces high-
density green pellets [13–15, 22–23]. Complete specifica-
tions of all die sets are mentioned in Table 1. All the die
sets were properly cleaned with acetone and lubricated
with McLube 1805A silicon free mold release spray to
reduce die wall friction and increasing the flowability
of powder during filling [24–27]. Die 1, 2, and 4 were

TABLE 1.—Die set specifications.

S. no Detail Die set-1 Die set-2 Die set-3 Die set-4

1 Supplier Ants Ceramics, Ashish Engg. Works, Ants Ceramics, Hard-O-Metals,

Mumbai, India New Delhi, India Mumbai, India Ludhiana, India
2 Die body Steel Steel Steel Steel
3 Top anvil= plunger Steel Steel Steel Tungsten carbide
4 Die liner – – – Tungsten carbide
5 Bottom plunger=anvil Steel Steel Steel Tungsten carbide
6 Bottom plate –– Steel Steel –
7 Pellet size 10 mm 10 mm 15 mm 10 mm
8 Load capacity (Tonns) 15 15 15 22
9 Clearance b=w barrel and 0.16 mm 0.17 mm 0.19 mm 0.02 mm
plunger=anvil
 EFFECT OF PROCESSING METHODS AND DIE DESIGN PARAMETERS FOR GREEN PELLETS
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FIGURE 2.— (a). Defects on the contact surface, due to conventional process of finishing and polishing (figure not to the scale). (b). Surface grinding of die
set-4 anvil (figure not to the scale).
filled with 1 g of the powder and die 3 were filled with
1.5 g of powder as the barrel diameter of die 1, 2, and
4 were 10 mm and die 3 were having 15 mm. Low aspect
ratio is preferred for densely packed particles through-
out the pellet [19]. Pellets with the low aspect ratio were
made from the die set-1 (h=d  0.15), die set-2
(h=d  0.15), die set-3 (h=d  0.1), and die set-4
(h=d  0.15). Conventional top filling process was used
for die set-1, 2, and 3, in which the powder was leveled
by tapping the die body equally from all the directions.
The level of the loosely filled powder was set with careful
observation. Top plunger=anvil was inserted from the
top, and the whole assembly was placed on a hydraulic
press for compression. The simple procedure followed
for making pellets with die set-1, 2, and 3 is demon-
strated in Fig. 4. To die set-4, a new method of filling
powder was followed to minimize the die wall friction
by reducing plunger travel, leveling of filling powder
and minimizing pellet movement during ejection. In
Step 1, the powder was filled in the die barrel from the
bottom side by inverting the die body as shown in
Fig. 5(a). Step 2 – Die body was equally tapped from
outside as per Fig. 5(b) to level the filled powder as much
as possible. Step 3 was an intermediate method termed
FIGURE 3.—Uniform distribution of powder constituents tested by EDS.
3
as a pre-compression step. Tapped volume of the
powder was slowly pressed and sheared manually by
the dummy anvil as shown in Fig. 5(c) so that uneven
surface becomes leveled, and maximum trapped air
comes out from the filled volume through low
clearance before high compression is performed. This
can decrease density variations in green pellet [5, 25, 27].
Pellets of the powder mix were compacted (1.6–
1.7 mm thick) using single acting hydraulic press (Poly-
hedron, India, Model 5010) under compression of
15 tons (206.8 MPa). Conventional uniaxial compression
involves the movement of either top or the bottom plun-
ger. Compression of powder in die set-4 was performed
as demonstrated in Figs. 5(c)–(e) which replicates the
method of pressing powder from the top as well bottom
direction. Manual pre-compression of powder described
in Step 3 reduces unnecessary free movement of the anvil
from initial powder filled state to the high compression
state. Most of the trapped air is ejected in the initial
60% of anvil travel during compression. In our method,
we reduce this travel to half the movement in conven-
tional method by following pre-compression step. The
remaining 70–80% of axial movement of one anvil was
shared by both the anvils, i.e., top and bottom anvils
 4 D. KUMAR AND K. SINGH

FIGURE 4.—Conventional die filling process used for die set-1, 2, and 3. (a) Powder filling from the top and tapping. (b), (c) Powder compression. (d) Pellet
ejection.

move simultaneously. This process partially replicates in Figs. 8(l) and (m). In our study, we have considered
the method of two-side compression while using uniaxial at least three pellets made by all the die sets for comparing
compression press. Dual directional compression their quality, based on the number of defects present in the
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decreases the density gradient in the green pellet at the
both ends [5, 19]. In Step 4, second anvil was slowly
inserted into the die barrel and made to touch with the
upper layer prepared in pre-compression Step 3 and the
whole assembly was fixed on the hydraulic press platform
as shown in Fig. 5(e). During Step 5, compressive pressure
was steadily raised up to 206.8 MPa and released slowly
after holding it for 2 minutes. In Step 6, the pellet was
slowly ejected, without any damage on edges as shown
pellet, green strength, and relative density. Number of
trials required to produce at least three successful pellets
may vary depending on the die design parameters and
the method of powder compression.
Surface roughness of all the die barrels, and plun-
ger=anvil was measured using the surface roughness
tester (Mitutoyo-SJ400 and Stand JIS 2001) as shown
in Figs. 6(a) and (b), respectively. The surface roughness
test was performed with 0.5 mm=sec as measuring speed,

FIGURE 5.—Sequence of processes followed using die set-4. (a) Fill the powder in the cavity from bottom side by inverting the die body. (b) Tapping the die
body for leveling the filled powder. (c) Manually press the filled powder by simultaneously pressing and rotating dummy anvil having a rough surface. (d)
Inverting the assembly in the upward right position and fitted on the press. (e) Compress the powder with high pressure hydraulic press. (f) Eject the pellet
from the bottom side by pressing the plunger and die body in the opposite direction.
 EFFECT OF PROCESSING METHODS AND DIE DESIGN PARAMETERS FOR GREEN PELLETS
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FIGURE 6.—(a).–– Surface Roughness of anvil= plunger of die set-1, 2, 3, and 4, respectively. (b). Surface roughness of barrel of die set-1, 2, 3, and 4,
respectively.
4 mm as evaluation length, 0.5 mm=cm on a vertical plot,
and 200 mm=cm on a horizontal plot as per JIS 2001
standard. Average roughness of the tested surface is
represented by term Ra.
Waviness of the top ends of plunger=anvils had a great
influence of the density gradients in the compact.
Plungers=anvils of all the die sets were evaluated as
per ISO–12085-1996 standard using surface profile
meter (Taylor Hobson, Intra-2). Average roughness of
the tested surface is represented by term Ra. The term
Wdc represents the difference between lowest and highest
point on the measured surface with respect to the
machine reference. The values of the above two para-
meters and graphical representation of all the scanned
points along the measured length indicates the waviness
of the surface. Test results of the surface waviness of all
the die sets are shown in Figs. 7(a)–(h).
The Green strength of the compressed pellets was
calculated using Eq. (1) as per the famous Brazilian test
[28, 29]. Strength of cylindrical specimens was measured
by compressing the specimen along the diameter. The
strength of small samples (rf) was also estimated using
the same principle and verified by some authors in
Refs. [24] and [27]. Pellets made by all the die sets were
fractured under similar conditions using the equation
given below:
rf ¼ 2P=pDt ð1Þ
5
where P is the maximum fracture load in Newton, D is
the pellet diameter in millimeter, t is the pellet thickness
in millimeter, and rf is the green strength in MPa.
General setup of the Brazilian test is shown in
Figs. 9(c). The Green strength of all the successfully
ejected pellets is presented in Table 3.
The relative density of the compressed pellet is one
of the measures to compare effectiveness of the die set.
All the die sets were operated under same compressive
load of 206.8 MPa. High relative density promotes the
densification of the pallet during sintering [30]. The
relative density of any powder compact can be found by
dividing the density of the part compacted in the process
to the theoretical density of that part. In the process, total
volume of the compact is required to be calculated. It is
easy to calculate the volume of bodies having simple shape
and relatively large size by measuring the part dimensions.
However, it is very difficult to calculate the exact volume
of the small pellets having diameter and thickness
in the range of 10 and 1.6 mm, respectively. Physical
measurement of the volume of any pellet may also include
the volume of air present in fine cracks. Measurement of
volume using Archimedes principle is more precise for
pellets of small size. In this process, the pellet was fully
submerged into xylene. The pellet was soaked into xylene
for a few minutes to displace all the air present into the
pores and cracks of the compressed pellet. The weight
of the liquid displaced by the pellet was calculated with
 6 D. KUMAR AND K. SINGH
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FIGURE 7.—(a).––Upper punch waviness of die set-1. (b). Bottom punch waviness of die set-1. (c). Top punch waviness of die set-2. (d). Bottom punch
waviness of die set-2. (e). Top punch waviness of die set-3. (f). Bottom punch waviness of die set-3. (g). Top punch waviness of die set-4. (h). Bottom punch
waviness of die set-4.

high precision weighing machine. The relative density of Average weight of xylene evaporated during the
the pellet was calculated using Eq. (2): measurement was also calculated and added to the
weight of the pellet when immersed into the liquid.
Relative density ¼ Density of xylene was taken as 0.863 g=cm3. Average
values of the relative density for all the pellets
ðweight of pellet in airÞðdensity of xyleneÞ
ð2Þ compressed from different die sets were calculated as
ðweight of pellet in xyleneÞ shown in Table 4.
 EFFECT OF PROCESSING METHODS AND DIE DESIGN PARAMETERS FOR GREEN PELLETS 7
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FIGURE 8.—Pellets made by different die sets (a) Pellet of die set-1 with lamination defect. (b) Pellet of die set-1 with capping defect. (c) High powder
wastage in die set-2. (d) High powder wastage in die set-3. (e) Pellet of die set-2 showing low edge density. (f) Pellet of die set-2 with capping and lamination
defect. (g) Broken pellet of die set-3 with capping defect. (h) Leakage of nanopowder in die set-1 due to high clearance. ((i) and (j)) Leakage of nanopowder
in die set-2. (k) Plunger of die set-3, showing leakage of nanopowder. (l) Pellet compressed between two anvils of die set-4, just after the ejection. (m)
Ejection of pellet from die set-4 with negligible powder wastage. (n) Pellet of die set-4 showing good surface, sharp edges free from capping defect and
lamination defects.

RESULTS AND DISCUSSION Importance of the die-plunger=anvil clearance is

Die-plunger=anvil clearance facilitates the easy explained as below:
movement of plunger=anvils within the barrel and
to provide sufficient clearance to escape the trapped 1. More clearance will provide more space for
air inside the filled powder. Pellet making in the nanopowder to flow in the clearance during
laboratory is a very slow and manual process. compression (Figs. 8(h)–(k))
 8 D. KUMAR AND K. SINGH

FIGURE 9.—(a). –– Profile of pellet made from die set-1, 2, and 3 (figure not to the scale). (b) Profile of pellet made from die set-4 (figure not to the scale).
(c) Brazalian test setup [21, 22].

2. More clearance reduces the strength of pellet at
corners (Figs. 8(d)–(f)).
3. Nanopowder slipped into the die-plunger=anvil
clearance will lead to jamming of plunger=anvil
inside the barrel. The pellet ejection process becomes
a more jerky and most of the time sudden release of
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of the order of 0.02 mm reduces the powder wastage
and jamming problem, but pre-compression step
plays an important role in the whole process.
Good surface finish is always desirable. High surface
finish becomes more important for application of die

the plunger=anvil under high ejection force (to
overcome jamming), break the pellet (Fig. 8(g)).
4. Nanopowder slipped in the clearance, sticks to the
die walls, and offers more restrictions to pellet during
ejection. Under these circumstances, either pellet will
completely break during ejection, or it will get
damaged from the corners (Figs. 8(c)–(k)).
5. More clearance does not guarantee that our plun-
ger=anvil is concentric with the barrel, as there is
no means to keep it at the center during compression.
The offset position of the plunger=anvil gave rise to
jamming of plunger=anvil favored by the presence
of nanopowder slipped into the clearance.
6. Jamming of the plunger=anvil is more likely to hap-
pen if defects shown in Fig. 2(a) are also present
along with the high clearance.
7. As the clearance decreases, the chance of trapping air
is also very high. Clearance plays an important role
in removing inside air, during high speed commercial
manufacturing of powder compressed parts. Trapped
air decreases the green strength of pellet. It is evident
from Figs. 8(h)–(k) and Table 2 that more die-
plunger clearance always leads to more wastage of
nanopowder. More clearance in die set-1, 2, and 3
leads to an average 7–8% of powder wastage
whereas, it is only 1–1.5% in die set-4. Low clearance
set in making pellets of nanopowder. Most of the time
it is restricted by the high cost, die set material proper-
ties, and method of finishing. Poor surface finish gives
rise to the following problems:
1. Rough surface offers more resistance to the move-
ment of the plunger. Even with the low clearance,
surface finish should be high to reduce friction and
wear of contact surfaces.
2. High wall friction also affects the density gradient in
green body.
3. Our main concern in the present study is about the
use of tungsten carbide nanopowder and similar high
hardness nanopowders for making pellet. Hence,
rough surface is more likely to abrade, using high
hardness powders. Repeated surface abrasion during
the compression process will increase the
die-plunger=anvil clearance.
4. Rough surface cannot be smoothed by the surface
lubricant (mold release agent), used for easy ejection
of pellet. However, relatively small irregularities on
the highly polished surface can be easily smoothened
with external lubricant (Fig. 6(b)). Mold release
agent reduces the adhesion of nanopowder to the
die walls as well as it offers very less space for
nanopowder to get stuck into irregularities.

TABLE 2.—Measured surface details.

S. No Detail Parameters Die set-1 Die set-2 Die set-3 Die set-4

1 Surface roughness of plunger=anvil walls Ra (mm) 0.13 0.41 0.25 0.09

Ra ¼ Average roughness
2 Surface roughness of die barrel walls Ra (mm) 0.17 0.42 0.06 0.04
3 Waviness of top plunger=anvil Wdc (mm) 25.52 10.88 14.10 2.22
Wdc ¼ Difference b=w lowest and highest point
Wa ¼ Average waviness Wa (mm) 3.66 1.78 3.47 0.47
4 Waviness of bottom plunger=anvil Wdc (mm) 15.80 6.75 11.91 3.51
Wa (mm) 2.87 1.10 1.48 0.79
 EFFECT OF PROCESSING METHODS AND DIE DESIGN PARAMETERS FOR GREEN PELLETS 9
TABLE 3.—Quality and green strength of pellets compressed with old and new method.

Green
Die Compaction Trial Die punch Pellet Capping Broken Lamination Surface Wt. of filled Wt. of % Powder strength Average green
set method S. no. jamming damaged defect edges defect finish powder (g) Pellet (g) wastage (MPa) strength (MPa)

1 OLD 1 Y Break – – – – – – – –
1 OLD 2 N N Y Y N Poor 1.0026 0.9321 7.03 2.17
1 OLD 3 N Break – – – – – – – –
1 OLD 4 Y Break – – – – – – – –
1 OLD 5 N N Y Y Y Poor 1.0031 0.9309 7.20 2.29
1 OLD 6 Y Break – – – – – – – –
1 OLD 7 N N Y Y Y Poor 1.0019 0.9319 6.99 2.28
1 New 1 N N Y Y Y Poor 1.0033 0.9299 7.32 2.42 2.29
1 New 2 Y Break – – – – – – – –
1 New 3 Y Break – – – – – – – –
1 New 4 N Break – – – – – – – –
1 New 5 N N Y Y N Poor 1.0021 0.9303 7.16 2.31
1 New 6 N N Y Y Y Poor 1.0056 0.9326 7.26 2.27
2 OLD 1 Y Break – – – – – – – –
2 OLD 2 Y Break – – – – – – – –
2 OLD 3 Y Break – – – – – – – –
2 OLD 4 N N Y Y Y Poor 1.0032 0.9231 7.98 2.63
2 OLD 5 Y Break – – – – – – – –
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2 OLD 6 N N Y Y Y Poor 1.0041 0.9229 8.09 2.69

2 OLD 7 Y Break – – – – – – – –
2 OLD 8 N N Y Y Y Poor 1.0039 0.9248 7.88 2.79
2 New 1 Y Break – – – – – – – – 2.82
2 New 2 Y Break – – – – – – – –
2 New 3 N N Y Y N Poor 1.0053 0.9283 7.66 2.89
2 New 4 Y Break – – – – – – – –
2 New 5 N N Y Y Y Poor 1.0029 0.9225 8.02 2.98
2 New 6 N N Y Y N Poor 1.0044 0.9265 7.76 2.94
3 OLD 1 N N Y Y Y Average 1.5031 1.3841 7.92 2.63
3 OLD 2 N N Y Y Y Average 1.5011 1.3799 8.07 2.74
3 OLD 3 Y Break – – – – – – – –
3 OLD 4 Y Break – – – – – – – –
3 OLD 5 N Break – – – – – – – – 2.74
3 OLD 6 N N Y Y Y Average 1.5028 1.3834 7.95 2.77
3 New 1 N Break – – – – – – – –
3 New 2 N N Y Y Y Average 1.5036 1.3903 7.54 2.84
3 New 3 Y N Y Y Y Average 1.5038 1.3877 7.72 2.83
3 New 4 N Break – – – – – – – –
3 New 5 N N Y Y Y Average 1.5009 1.3795 8.09 2.63
4 OLD 1 N N N N N High 1.0012 0.9859 1.53 3.89
4 OLD 2 N N Y N Y Average 1.0019 0.9898 1.21 3.62
4 OLD 3 N N N N Y Average 1.003 0.9902 1.28 3.75
4 OLD 4 N N N N N High 1.0028 0.9885 1.43 3.69 3.88
4 New 1 N N N N N High 1.0022 0.9891 1.31 4.22
4 New 2 N N N N N High 1.0009 0.9895 1.14 3.96
4 New 3 N N N N N High 1.0028 0.9899 1.29 4.1
4 New 4 N N N N N High 1.0031 0.9911 1.20 3.88

5. Rough surface accommodates more nanopowder in
the surface irregularities and tool marks. Nanopow-
der present in these irregularities, obstruct the ejec-
tion of compressed pellet (Figs. 8(h)–(j)), and offers
more resistance to the movement of the plun-
ger=anvil as demonstrated in Fig. 10. The peaks
and valleys are the main cause of poor surface finish,
which leads to very high obstruction during the
ejection of pellet. When the compressive load was
released, most of the internal energy inside the pellet
was utilized for spring back action in axial direction.
Radial spring back is nearly 25% of the axial spring
back in the pellet, but pellet was still under radial
compression along the walls of die. Radial compress-
ive forces and pellet ejection forces are perpendicular
to each other. Rough die wall surface possesses more
peaks and valleys, which damage the peripheral
surface and edges of pellet as shown in Figs. 8(a),
(d)–(G). Most of the pellets were damaged due to
large internal roughness. During the ejection process,
the incoming valleys on the die surface offer an
excess space to the upper layer of the pellet to expand
 10 D. KUMAR AND K. SINGH

TABLE 4.—Relative density of the green pellets compressed with old and new method.

Die Compaction Trial S. Wt. of Wt. of Pellet in Avg. Wt. of xylene Wt. of xylene Density of pellet Relative Average relative
set method No. Pellet (g) xylene (g) Evaporated (g) displaced (g) (g=cm3) density (%) density(%)

1 OLD 2 0.9321 0.1075 0.0129 0.1204 6.68 50.83

1 OLD 5 0.9309 0.0993 0.0129 0.1122 7.16 54.48
1 OLD 7 0.9319 0.1021 0.0129 0.115 6.99 53.21
1 New 1 0.9299 0.0895 0.0129 0.1024 7.84 59.63 55
1 New 5 0.9303 0.0943 0.0129 0.1072 7.49 56.98
1 New 6 0.9326 0.0987 0.0129 0.1116 7.21 54.87
2 OLD 4 0.9231 0.0856 0.0129 0.0985 8.09 61.54
2 OLD 6 0.9229 0.0875 0.0129 0.1004 7.93 60.36
2 OLD 8 0.9248 0.0882 0.0129 0.1011 7.89 60.06 61
2 New 3 0.9283 0.0857 0.0129 0.0986 8.12 61.82
2 New 5 0.9225 0.0835 0.0129 0.0964 8.26 62.84
2 New 6 0.9265 0.0881 0.0129 0.101 7.92 60.23
3 OLD 1 1.3841 0.1477 0.0129 0.1606 7.44 56.59
3 OLD 2 1.3799 0.1414 0.0129 0.1543 7.72 58.72
3 OLD 6 1.3834 0.1399 0.0129 0.1528 7.81 59.45 59
3 New 2 1.3903 0.1315 0.0129 0.1444 8.31 63.22
3 New 3 1.3877 0.1361 0.0129 0.149 8.04 61.15
3 New 5 1.3795 0.1473 0.0129 0.1602 7.43 56.54
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4 OLD 1 0.9859 0.0891 0.0129 0.102 8.34 63.47

4 OLD 2 0.9898 0.0896 0.0129 0.1025 8.33 63.41
4 OLD 3 0.9902 0.0902 0.0129 0.1031 8.29 63.06
4 OLD 4 0.9885 0.0891 0.0129 0.102 8.36 63.63 64
4 New 1 0.9891 0.0831 0.0129 0.096 8.89 67.65
4 New 2 0.9895 0.0845 0.0129 0.0974 8.77 66.71
4 New 3 0.9899 0.0887 0.0129 0.1016 8.41 63.98
4 New 4 0.9911 0.0894 0.0129 0.1023 8.36 63.61

in radial direction. The top-most layer of the pellet
expands and gets fit into the new space followed by
shearing. After this expansion, when we further move
the pellet for ejection, the next roughness peak offers
high resistance to movement of pellet. These obstruc-
tions suddenly release the axial ejecting load with a
jerk and break the pellet from more locations. The
probable cause of damaged pellets in die set-1, 2,
and 3 may be due to alternatively expansion and
compression of pellet layers during the ejection
process. This behavior also initiates the capping
defect. The above phenomenon is demonstrated in
Fig. 10. The 0.004 mm surface finish of die set-4 is
able to produce a pellet with sharp edges, mirror like
peripheral surface finish and free from end capping
defects as well as lamination defects, which can be
clearly observed in Figs. 8(h) and (i). However, a
great care is always required for applying slow and
uniform loads for compression and ejection of pellet.
A true flat surface with an acceptable finish is very
difficult to manufacture. Contact surfaces of the
plunger=anvil must be perpendicular to its lateral sur-
face and free from the defects as shown in Fig. 2(a).
The surface profiles presented in Figs. 9(A) and (B) is
only for general understanding and easy visualization

FIGURE 10.— Sectional view of different positions of compressed pellet during ejection and the effect of peaks and valleys on the edges of pellet (figure not
to the scale).
 EFFECT OF PROCESSING METHODS AND DIE DESIGN PARAMETERS FOR GREEN PELLETS
of the two different shapes and concepts. The actual sur-
face curvature of the plunger=anvils of die set-4 is only a
fraction of curvature shown in Figs. 9(a) and (b). Devi-
ation from the true flatness is the surface waviness or
curvature, and that should be preferred in the style of
the curvature shown in Fig. 9(b). Difference between
the surface waviness of the plunger=anvil of all the die
sets can be observed through Figs. 7(a)–(h). However,
the waviness of plunger surface is 25.52 mm as shown
in Fig. 7(a). This value is considerably high for 10 mm
length. During the manufacturing procedure of die
set-4 it has been observed that the poor surface profile
of plungers=anvils of die set-1, 2, and 3 may be due to
some manufacturing constraints as well as the lack of
the operator’s knowledge about the sensitivity of the
manufacturing details in the present task. It was also
observed that blank pieces of plungers=anvils are gener-
ally cut from the stock material with wire cut electric
discharge machine (EDM). After cutting, they were
manually finished with carbide sandpaper followed by
polishing. Completely manual process increases the
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waviness of the surface. Manual grinding and polishing
wear the blank material more from the outer periphery.
However, the surface of the plungers=anvils polished by
this hand-operated process, looks very smooth and
shiny, but there are undesirable changes occurring in
the surface profile. This happens not only due to lack
of the operator’s knowledge, but some manufacturing
constraints are equally responsible. It is very difficult
to hold a small round piece of 10 or 15 mm in diameter
and 5–6 mm thick, on the magnetic base for surface
grinding. As a result, the pellet formed from convex pro-
filed anvil is concave at both ends (Fig. 9(a)) and weak at
edges. Whereas the pellet formed by concave profiled
anvil of die set-4 is of little convex (Fig. 9(b)) at the flat
ends. Surface profile of die set-4, shown in Figs. 7(g)
and (h), also verifies that the contact surface of the anvil
is a little concave in shape as compared to the profiles of
other die sets. Low aspect ratio pellet requires small cur-
vature, which is sufficient to provide a nominal increase
in the pressure gradient from the center to the outer
edge. Very little literature is available on the effect of
surface finish, die wall friction, and compaction pressure
on the green density of the compressed pellet [5, 19, 22–
26, 30, 32, 33]. In the present study, we find major rea-
sons of getting poor pellets made of tungsten carbide
nanopowder. Surface waviness of all die sets are tabu-
lated in Table 2, and it was observed that waviness of
die set-4 is minimum in comparison to any other die
set. The surface waviness profile of the anvil contact sur-
face is of more importance as compared to surface finish,
due to negligible friction offered at the top contact
surface of the anvil. Surface finish of anvils of die set-3
and 4 (Figs. 6(a) and (b)) are not largely varied, but still
the green pellets made by the two are very different. The
difference in the pellet quality is primarily due to surface
profile and not the surface finish. Although, the aspect
ratio of the pellet made by die set-3 is less than that
of die set-4, but still it is unable to produce a good
pellet. Hence, it can be concluded that waviness of
11
plunger=anvils is of major concern as compared to the
surface finish. The effect of small waviness can be easily
understood by the number of defects associated with the
pellets made by die set-1, 2, and 3. Detailed analysis of
all the pellets produced by die set-1, 2, 3, and 4 is pre-
sented in Table 3. Waviness present on the surfaces of
top and bottom plunger=anvil results in non-uniform
gap between the two, while they are face to face during
compression. Non-uniform gaps are responsible for
compressing the nanopowder into the regions of high
pressing and low pressing throughout the cross-section
of the green pellet. Uniformity of pressure applied
throughout the compact, ultimately determines the micro-
structural homogeneity of green bodies. Variations in the
applied pressure within the green body during com-
pression also contribute to the density gradient in the
compacts after sintering [17]. As per the literature and
our close observations, high waviness in die set-1, 2,
and 3 is also responsible for (i) capping defects, (ii) lami-
nation defects due to density gradient, and (iii) breakage
of pellet due to non-uniform pellet strength and variable
amount of springback in regions of low and high density.
Repeated use of the die set, wear the die walls and
lateral surface of plunger=anvils when used for high
hardness nanopowders. Steel dies wear out very quickly
as compared to tungsten carbide dies. Steel dies are easy
to manufacture, but they cannot maintain the designed
clearance for a long time. Jamming of plunger=anvils
in steel die sets, increase the chance of denting the barrel.
Hard material, like tungsten carbide, can easily bear the
abrasion effect of high hardness nanopowders and better
maintain the designed tolerance over a period.
Powder characteristics, like hall flow, tapped bulk
density, flowability index, particle roughness, particle
size, shape, etc., are widely used to quantify the powder
flow regime. Smooth spherical powder particles with low
cohesiveness and high bulk density show good flowabil-
ity. Tapped bulk density depends upon the tapping style,
density, and surface roughness of powder particles.
Addition of lubricant increases flowability and reduces
cohesiveness of the powder. During compaction of hard
materials, the lubricant increases bonding between the
particles. Although lubricant helps in reducing the fric-
tion and internal defects in the pellet, on the other hand
it increases the porosity of sintered pellets. In case of
ultra-fine powder, large surface area increases the pow-
der cohesiveness. Compaction of cohesive powder with-
out any lubricant medium creates some problems. All
the four die sets were tested using conventional method
and new proposed method of nanopowder compression.
Die set-1, 2, and 3 shows very little improvement in
quality of pellet produced by the new proposed method
as compared to the conventional method. As shown in
Table 3, we observed that there is a decrease in the num-
ber of defects per pellet as well as the number of trials to
produce at least three pellets with both the methods.
Despite the following new proposed method, the num-
bers of defects were still very high and success rate of
 12
making pellet was extremely low. Surface finish of die
set-3 was better, and the aspect ratio was lower than that
of die set-1 and 2, but there was no considerable
improvement in the number of defects, and the number
of trials required to produce a good pellet. The reason
behind may be the more die-plunger clearance and high
surface waviness. New proposed method of nanopowder
compression was unable to compensate the variations in
other die design parameters. All the three important
parameters, i.e., surface roughness, surface waviness,
and die-plunger=anvil clearance should be as low as
possible. Die set-4 was manufactured keeping in mind
the importance of all these parameters. A great care
was given to the workmanship, methods of manufactur-
ing, and selection of material. From the results of die
set-4, shown in Table 3, it is evident that better values
of die design parameters were even not sufficient to pro-
duce a good pellet in each attempt, unless we refine vari-
ous steps involved in the powder compression. Two out
of four pellets made by die set-4 using conventional
method showed minor capping and lamination defect.
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The probable reason may be the improper distribution
of nanopowder inside the die barrel before compression.
Only tapping of the die body from outside is not enough
to assure the even distribution of nanopowder through-
out the cross-section. It was also observed that tapping
itself disturbed the homogeneity of loosely filled nano-
powder. Visual inspection of the surface of filled powder
from the top, through the narrow 10 mm diameter is
always a misleading judgment. We all can understand
and verify the easy looking, but a very sensitive concept,
by a simple experiment of leveling the talcum powder or
any other fine powder in a glass test tube. Equal tapping
from all the directions, definitely facilitates the leveling
of loosely filled powder, but leveling with tapping is
an endless process. That was the reason that we tried
new method for pre-compression as demonstrated in
Fig. 5(C). As a result, there was no defect found in
any of the pellets made by die set-4 using a new method
of compression as demonstrated in Fig. 5 and explained
previously.
Based on different observations and measurements,
the qualities of green pellet compressed with all die sets
are compared. End capping and lamination are the major
issues involved in high-pressure compression. It has been
observed that majority of defects arises due to poor con-
structional specifications of die sets. After releasing the
compressive load, the springback action of compressed
pellet in radial and axial direction is a well-reported
phenomenon by various researchers [4, 30, 31]. There is
an axial expansion of pellet as soon as compressive loads
is removed. The majority of the internal stresses is
released in axial direction. At an elevated compressive
load, the springback in axial direction leads to end
capping defect. The load is maximum at the center and
reduces in a radially outward direction as well as axially
downward, in uniaxial compression [25, 26, 30–32].
High green strength of pellet is required for handling
the pellet from the state of ejection to the positioning
of pellet for sintering. High green strength also indicates
D. KUMAR AND K. SINGH
the probability of minimum defects and high density of
sintered part. Using a diametric compression test, the
average green strength of the pellets obtained from the
die set-1, 2, and 3 in different trials, as represented in
Table 3, are found to be 2.29, 2.81 and 2.73 MPa,
respectively. Whereas the green strength of the pellets
obtained from the die set-4 is 3.88 MPa, which is the
highest among all die sets. Uniformly mixed nanopow-
ders of variable sized particles are closely packed under
high compressive pressure of 206.8 MPa to produce
dense green pellets without using any poly(vinyl
alcohol). Table 4 represents the relative density of green
pellets made by die set-1, 2, 3, and 4, which were found
to be 55%, 61%, 59%, and 64%, respectively. Improved
method of die filling, pre-compression and compression
used in die set-4 leads to achieve high green density as
compared to the other die sets under same compressive
load. High surface finish and better surface profile sup-
port the concept of achieving high-density green pellets,
free from internally trapped air and other defects.
CONCLUSIONS
The surface finish of the die wall and surface profile of
the anvil plays an important role in obtaining a good
green pellet. Surface finish of die walls and surface wavi-
ness of anvils are in the order of 0.04 and 2.2–3.5 mm,
respectively. Relative density of green pellets are 55%,
61%, 59%, and 64% for die set-1, 2, 3, and 4, respect-
ively. Clearance between the die and plunger=anvil is
to be 0.02 mm. The highest green strength is found
3.88 MPa when die set-4 was used for pelletization.
Die set-4 in combination with the new processing
method is better than the other three die sets, using
conventional as well as new processing methods.
FUNDING
The authors would like to thank Technical Education
Quality Improvement Program (TEQIP-II) for financial
support.
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