A. C. Silva, K. S. Macedo, E. M. S. Silva, M. R. Barros, D. F. Lopes, D. Y., Marinho, V. O. Morato, L. T. B. Mendonça, D. L. Florêncio, L.F.

Silva

Manufacture and Characterization of Ferroniobium Alloy

Briquettes

A. C. Silva1, K. S. Macedo1, E. M. S. Silva1, M. R. Barros1, D. F. Lopes1, D. Y.

Marinho1, V. O. Morato1, L. T. B. Mendonça1, D. L. Florêncio1, L.F. Silva2
1 Federal University of Goiás, Catalão, Brazil
2 NioBrás, Catalão, Brazil
ABSTRACT Brazil is the largest producer of Niobium alloys, with a production of 73,668 tons
of Nb2O5 concentrate in 2013, corresponding to a 92.81% of the world production. The
Brazilian Nb ores grades vary from 0.51 to 2.71%. Ferroniobium is an important iron niobium
alloy, with niobium content of 60-70%. It is the main source for niobium alloying of HSLA
steel and covers more than 80% of the worldwide niobium production. In 2013, Brazil produced
46,555 tons of ferroniobium, being around 90% of it for export. In the final stage of the Fe-Nb
production, the alloy needs to be crushed in a jaw crusher, which generate fin particles (around
26% of the feed below 10 mm in NioBrás process). The selling price of the fine particles have
a significant loss in the market, since the fine particles cannot be used directly in steel working.
Given this scenario, a process to agglomerate the ferroniobium fine particles into briquettes
with size and chemical qualities similar to original products was developed. During the
briquetting tests organic (zinc stearate) and inorganic (iron powder and water) binders were
used. The briquettes were characterized both physically and chemically. For the physical
characterization, the briquettes were tested for mechanical resistance, drumming, compressive
strength, water resistance, thermal shock and Brinell hardness. The test contained addition of
3% of zinc stearate, 2% iron powder and 1% water reached a niobium content above 62% and
the levels of contaminants below the standard ferroniobium specifications. The tested briquettes
have chemical and physical properties compatible with sales specifications.

1 INTRODUCTION Industrial applications of Niobium include,

Niobium is a trace element present in Earth but are not limited to, high-strength low-alloy
crust with average grades between 0.3 and 1% steel (HSLA), stainless steel and super alloys.
of Nb2O5. However, some Brazilian deposits The Niobium consumption in micro alloyed
can reach exceptional grades around 3% due structural steels reaches above 80% of its
to supergene enrichment in weathered zones demand (DAMASCENO, 2006).
(MENDES, 2005). Niobium is a metallic, Brazil holds the Niobium bigger deposits in
soft, ductile solid and has a high melting point the world, distributed between the states of
(2,469 °C) one of the highest of the periodical Minas Gerais, Amazonas, Goiás and
table. It is resistant to corrosion, mainly due Rondônia, with a total reserve around 10.8 Mt
to the formation of a thin film in the oxide of pyrochlor exploitable reserves. Brazil is
surface, called passivation layer. When also the bigger producer with an annual
combined Niobium exhibit different production around 88.8 kt of Nb2O5
oxidation numbers, being +5 the most concentrate and 51.7 kt of Ferro Niobium
common. At room temperature Niobium, do Alloy (Fe-Nb), with Nb content ranging from
not react with hydrogen, air, water or acids, 60 to 70%. Canada holds the second position
except for hydrofluoric and its mix with nitric in the world marketing with approximately a
acid (SOUSA et al., 2013). reserve of 200 kt and annual production
around 5 kt (DNPM, 2015). Figure 1 shows
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Brazilian’s Niobium production between the
years 2000 and 2014. It is possible to see a
development in the Niobium marketing until
2010, when the steel marketing started to face
a severe economic crisis. An improvement in
the marketing was noticed after 2012 and
2014 end up being, together with 2009, the
years with higher production in the period.
Figure 1. Brazilian’s Niobium production
(2000-2014).
of Goiás the company production is destined
to exportation. In NioBrás, after the
aluminothermy, the final stage of the Fe-Nb
production is the comminution of the freshly
produced alloy, normally using a jaw crusher
(see figure 2). This stage often generate
particles under 10 mm, considered fine
particles and not able to be used direct in the
steel making process because only of their
size. Other operations that generate fine
particles are Fe-Nb screening and handling
(especially the commutation between convey
belts), reaching a production around 95 tons
per month (equivalent to 26% of the Fe-Nb
production) of fines. Fe-Nb fine particles are
divided in three different classes according to
their granulometry and generation process:
under 2 mm (type A), between 1 and 5 mm
(type B) and between 3 and 15 mm (type C).
Figure 3 shows samples of the three types of
fines.

Brazilian’s most exported Niobium product is

Fe-Nb, responding for over 90% of the
Niobium exportations. According to the
Brazilian official Mineral Agency (DNPM,
2015) in 2014, the total exportation of this
product was 71 kt, corresponding to US$ 1.7
billion.
Industrial activities such as mining and
metallurgy can produce many types of
residues, including fine particles. Several
different initiatives have been adopted to
minimize the production of fine particles
and/or to recover then. These particles can be
generated in process such as ore blasting,
transport, hauling, screening, comminution
and even handling. The recovery of fine
particles can lead to an increase in the
production or in the production of by-
products. Taking that in consideration many
efforts have been done in order to reduce the
emissions of fine particles and to try to give Figure 2: Fe-Nb alloy production flowsheet.
then a better destination, avoiding potential
environmental and health issues.
NioBrás is company from the Chinese
group CMOC and is one of the two companies
that produce Fe-Nb in Brazil (around 35% of
the Brazilian production). Situated in the state

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A. C. Silva, K. S. Macedo, E. M. S. Silva, M. R. Barros, D. F. Lopes, D. Y., Marinho, V. O. Morato, L. T. B. Mendonça, D. L. Florêncio, L.F. Silva

could be very economic attractive to both

supplier and consumer.
The agglomeration process aim in produce
material with size adequate to the future
application and the correct choose between
the available methods depends on a very
careful analyses. According to Carvalho &
Brinck (2010), this involves not only
laboratory work in order to produce the
agglomerate, but also its physical and
chemical characterization. Among the
agglomeration techniques, the most important
(a) ones in mineral processing are pelleting,
sintering and briquetting.
Moraes & Kawatra (2011) tested how
binders successfully used in the pelletizing of
Brazilian hematitic iron ores, using disk
pelletizer, would perform in the processing
of an American magnetite concentrate by
balling drums. Although the results were very
good, the operational cost of the pelleting was
relatively high when compared with the other
two methods.
Telles, Espinosa & Tenório (2013)
developed a sintering process to agglomerate
(b) electric arc furnaces dust in order to recycle
this material in the steelmaking. In their
process, the dust had to be first agglomerated
as micro-pellets and then sintered.
Lucena et al (2008) were able to produce a
low-cost charcoal wastes briquetted to be
used in blast furnaces and for energy
generation using a piston extruder. On the
other hand, Silva et al (2016) were able to
agglomerate limestone fines using a batch
briquetting process. In both case the
operational cost where small.

2 METHODOLOGY
(c) Taking in consideration the fact that the Fe-
Figure 3: Fe-Nb fine particles: (a) under 2 Nb fine particles has very small moisture
mm or type A, (b) between 1 and 5 mm or content, high melting point (1,900 ºC) and is
type B and (c) between 3 and 15 mm or type very abrasive the briquetting was choose as
the most feasible technique to agglomerate
C.
the fine particles.
Seeking a more efficient production concept
regarding the increase of Fe-Nb incorporation 2.1 Fe-Nb Briquette Manufacture
in the metal bath during the steel making Samples of the Fe-Nb fines from the alloy
process, the agglomeration of the Fe-Nb fine comminution, screening and handling were
particles was studied, once this by-product sent to two different companies in Brazil to be
agglomerated called Höganäs and Renova.
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The differences, beside the manufacture costs

and geometry, were the briquetting
technology used by the two companies.
Höganäs used a piston extruder and Renova
used a high-pressure roll press. Each company
produced two different briquettes composed
by a blend of the fine particles type
composition (see Table 1). The briquettes
were labelled as H (from Höganäs) and R
(from Renova) followed by the percentage of
the fines.
Table 1. Briquettes composition regarding
the fine particles type. (a) (b)
Briquettes A B C
R100-0-0 100 0 0
R0-100-0 0 100 0
H50-40-10 50 40 10
H60-40-0 60 40 0

Three binding agents were used two organic

and one inorganic. The organic binders were
zinc stearate (Zn(C18H35O2)2) and zinc
palmitate (Zn(C16H31O2)2) in a proportion of
70 and 30% respectively. Iron powder with
very low impurities grade was used as
inorganic binder. Table 2 shows the
proportion of water and binders used in the
briquettes manufacture. The homogenization
of the particles was performed in a mixing
tank, where the fine particles were added first
and then water and the binders.
Table 2. Binders and water composition
percentage (in mass) in the briquettes.
Organic Iron powder Water
binder (%) (%) (L)
3.0 2.0 1.0
During the briquettes manufacture samples of
the material where collected: before, during
and after the briquetting. The samples where
than homogenised and sent to X-ray
diffraction with Rhodium anode and
Nondispersive Infrared spectroscopic
(NDIR).
Figure 4 shows one photograph of the four
types of briquettes. It is possible to notice the
differences in geometry (Höganäs’ briquettes
were cylinders and Renova’s were soap like
shape) and surface quality in the
manufactured briquettes.
(c) (d)
Figure 4. Fe-Nb briquettes: (a) R100-0-0; (b)
R0-100-0; (c) H50-40-10 e (d) H60-40-0.
2.2 Fe-Nb briquettes characterization
The manufactured briquettes where tested in
the Mineral Processing Lab of the Federal
University of Goiás (LaMPPMin). All tests
were performed in triplicate.
2.2.1 Shatter Test
Shatter test (or Impact Resistance Test or
Drop Test) determines the briquette strength
to withstand repeated drops, simulating
impacts that occur naturally during handling
and transportation. Before heat treatment
(curing), the impact strength of the briquettes
can be determined by dropping it from a
height of 0.3 m direct onto a steel plate with
10 mm thickness. The procedure must be
repeated until the briquette loses 5% of its
initial mass (CARVALHO & BRINCK,
2010).
According to the same authors if the
briquette had been subjected to heat treatment

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A. C. Silva, K. S. Macedo, E. M. S. Silva, M. R. Barros, D. F. Lopes, D. Y., Marinho, V. O. Morato, L. T. B. Mendonça, D. L. Florêncio, L.F. Silva

to increase its mechanical strength, then the expand by different amounts. This differential
height of the drop should be changed to 1.5 m. expansion can be understood in terms of stress
In both cases (cured or not) the drop height or of strain, equivalently. At some point, this
can be changed to 0.6, 0.9, 1.2 and 1.5 m, for stress can exceed the strength of the material,
example. For uncured briquettes, 3 drops causing a crack to form.
from 0.3 m are considered a reasonable value, The shock temperature can be defined as
while for cured ones the number of drops shift the maximum temperature that the briquette
to 10. resist without lose more than 10% of its mass,
Eighteen briquettes from each type were without collapse or explode, during a fast
submitted to shatter tests from 0.3, 0.5, 0.75, temperature elevation.
1.0, 1.25 and 1.5 m height. Briquettes were weighted and placed in a
steel cylinder with holes in the lid and placed
2.2.2 Uniaxial compression and tension in a muffle oven with temperatures ranging
An important test to measure the maximum from 300 to 550 oC and 20 minutes of
load that a briquette can support before its residence time. After this time, the briquettes
rupture is the uniaxial compression test. A were removed from the oven and let rest in
compressive load was applied direct to the room temperature before a new weighing. The
briquette using a hydraulic press until the maximum temperature reached was the
briquette rupture, as described by the temperature when the briquette start to
Brazilian Association of Technical Standards combust (defined as ignition temperature).
(ABNT) NBR 12767/92. Sixty briquettes where submitted to thermal
To evaluate the tension resistance the shock test.
method created by Professor Lobo Carneiro
was used. This method calculates the tensile 2.2.5 Brinell hardness test
strength through a diametric compression test. According to Callister and Rethwisch (2013),
Altogether twenty-six briquettes where in the Brinell test, a hard, spherical indenter is
used in both tests. Briquettes manufactured by forced into the surface of the material to be
Renova could not be tested using Lobo tested. The diameter of the used tungsten
Carneiro test because of their geometry. carbide indenter was 10.00 mm (0.394").
Standard loads range between 500 and 3000
2.2.3 Water absorption kg in 500-kg increments; during a test, the
According to Cunha et al. (2006) in this test, load is maintained constant for a specified
briquettes must be complete submerged in time (between 10 and 30 s). Harder materials
water for 24 hours. After this time, the require greater applied loads. The Brinell
briquettes must be removed from water and hardness number, HB, is a function of both the
put to rest in room temperature for 10 minutes magnitude of the load and the diameter of the
in order to remove the water layer adsorbed in resulting indentation. Twenty-five briquettes
their surface and then weighted. Then they where used measure the Brinell hardness.
must be dried in a drying oven at 80 °C for 2
hours. In order to return the briquettes to room 2.2.6 Tumbler drum test
temperature they must be put to rest again for The tumbler drum test is derived from the R-
20 minutes and weighted again. The amount 556 of the MICUM standard for coke of the
of water that is absorbed by the briquette is International Organization for
important when the briquettes can be stored in Standardization (ISO). In this test, 1.5 kg of
open areas (CARVALHO & BRINCK, 2010). briquettes are placed in a steel test drum with
Altogether forty-eight Fe-Nb briquettes 29 cm long and 30.5 cm diameter fitted with
where tested. four steel angles with 6.5 cm wider, fixed
lengthwise inside the drum. The drum is
2.2.4 Thermal shock rotated at 25 rpm for eight minutes (200
Thermal shock occurs when a thermal revolutions in total).
gradient causes different parts of an object to
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The effect of tumbling on the briquette is

tested as follows. The briquette is first sieved
by hand to remove material that passes a
31.75 mm (1.25”) screen. This is to prevent
the finer particles cushioning the effect of
rumbling on the coarse material during the
test. After tumbling, the material is sieve-
analysed to measure the size reduction that
has occurred. These results are combined with
the sieve analysis of the fine material
excluded from the tumbler test to give a total
Figure 5. Granulometric analyse of the Fe-
evaluation of the briquette quality.
Nb fine particles before the agglomeration.
3 RESULTS AND DISCUSSION (a) under 2 mm or type A, (b) between 1 and
5 mm or type B and (c) between 3 and 15
3.1 Characterization of the Fe-Nb Fines mm or type C.
Figure 5 shows the granulometric analyse of
the Fe-Nb fine particles before the Table 3 shows the X-ray diffraction results of
agglomeration. It is possible to notice that the Fe-Nb fine particles characterization
particles type A (under 2 mm) and type B compared with the standard composition of
(between 1 and 5 mm) are well classified, this alloy as expected by the steel making
fitting to their label. On the other hand, market. Iron and niobium content must be at
particles type C (between 3 and 15 mm) where least 87% of the alloy composition. Due to the
actually smaller than expected. In fact, mineral association at NioBrás mine site, the
particles type C were smaller than 7 mm. major contaminants are P, Ti and Mn. It is
possible to notice that all three types of fine
particles have composition adequate to be
used in steel making.

Table 3. Standard Fe-Nb alloy composition and X-ray diffraction results of the fine particles.
Element (%)
Type
Nb P Fe Ti Mn Si Ta Pb S Al C
Standard 62- 67 < 0.20 25-30 < 1.00 < 0.50 < 3.00 < 0.50 < 0.20 < 0.15 < 1.00 < 0.15
A 64.56 0.15 29.18 0.33 0.30 2.95 0.31 0.19 0.07 0.40 0.14
B 65.17 0.17 28.65 0.25 0.30 2.85 0.31 0.19 0.09 0.31 0.14
C 65.25 0.15 27.97 0.24 0.35 2.68 0.29 0.18 0.07 0.23 0.13

3.2 Fe-Nb Briquettes Characterization Main body Fragments

3.2.1 Shatter Test
Table 4 shows photographs of the briquettes
before and after (main body and fragments) R100-0-0
shatter test for the four different briquettes
manufactured.

Table 4. Fe-Nb briquettes before and after

(main body and fragments) shatter test.
Briquette Before After
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A. C. Silva, K. S. Macedo, E. M. S. Silva, M. R. Barros, D. F. Lopes, D. Y., Marinho, V. O. Morato, L. T. B. Mendonça, D. L. Florêncio, L.F. Silva

3.2.2 Uniaxial compression and tension

Figure 7 shows the average results found in
R0-100-0 the uniaxial compression test for the four
types of briquettes and the results for the
uniaxial tension test for the cylindrical
briquettes.

H60-40-
0

H50-40-
10

Figure 6 summarizes the average resistance

of the briquettes regarding the number of Figure 7. Average uniaxial breakdown load
drops at different heights supported in the (compression and tension) results.
shatter test.
Comparing the photographs before and The cylindrical briquettes, manufactured by
after the test (Table 4) and the Figure 5 is Höganäs, obtained the best results in the
possible to notice that cylindrical briquettes uniaxial compression test. This fact could be
manufactured by Höganäs had a high related with their geometry once the
tendency in complete fragment themselves cylindrical shape provided a better contact
after a few drops, even from the smallest surface. The soap shaped briquettes has a poor
heights. The higher resistance was observed contact surface with the hydraulic press,
for the briquette R-0-100-0 manufactured by normally being just one contact point and not
Renova. Although this briquette was able to a surface.
resist more drops than the others at any tested Regarding the tension, the cylindrical
heights, for height higher than 1.0 m all type briquettes showed a resistance around 50% of
of briquettes showed a similar behaviour the compression resistance. Compared with
losing 5% or more of their initial mass in less other materials this is a high value, for
than 10 drops. example concrete tension resistance is around
10% of the compression resistance.

Figure 6. Average shatter test results.

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3.2.3 Water absorption

Table 5 shows three different stages of the
water absorption test (before immersion in
water, after and after the briquette had been
dried in drying oven). In one hand, it was not
possible to see any major visual changes on
them, but in the other hand, the briquettes
supported the immersion, even 48 hours,
without any physical degradation or
decomposition, remaining almost intact.

Table 5. Fe-Nb briquettes before and after Figure 8. Average water absorption test
water adsorption test (briquettes immerged results.
for 48 hours).
After This behaviour was noticed only by one type
Briquette Before
Immersion Drying of briquette manufactured by Höganäs (H50-
40-10). The other cylindrical type showed a
peak in mass variation for 48 hours
R100-0-0 immersion. Explanations for this behaviour
could be the hydration of the binder agents,
such as the iron powder, or chemical reactions
(Fe-Nb alloy or residues of the
aluminothermy) process with water.
R0-100-0
3.2.4 Thermal shock
The first result from this test was unexpected.
The briquettes start combusting after a certain
temperature (see Figure 9). Since the Fe-Nb
alloy was produced through aluminothermy,
H60-40-0 it was expected that all combustible material
were complete burnt in that process. That was
not the case. Every test performed at
temperatures above 600 oC ignited the
briquettes. The flame produced remained
H50-40-10
burnt for almost 12 hours after the briquettes
ignition, no matter with one of the four types
tested.
Table 6 shows photographs of the
briquettes before and after (main body and
Figure 8 shows the water absorption test fragments) thermal shock test for the four
results. It is possible to notice that all different briquettes manufactured.
briquettes had their mass enhanced after the Figure 10 shows the average fragments
test at least by 1% after 48 hours of immersion percentage generated at different
in water. Although the Renova briquettes had temperatures during the tests. No clear pattern
the high mass gain during the test, the could be observed between the briquettes
briquettes behaviour was quiet unusual, since behaviour regarding the fragments generation
a plateau was expected describing a water during the test. It is possible to highlight that
saturation level. the briquette R100-0-0 supported 100 ºC more
than the briquette R0-100-0 and H50-40-10
before they start combusting.
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A. C. Silva, K. S. Macedo, E. M. S. Silva, M. R. Barros, D. F. Lopes, D. Y., Marinho, V. O. Morato, L. T. B. Mendonça, D. L. Florêncio, L.F. Silva

Figure 10. Average briquettes fragments

percentage generated at different
temperatures.

3.2.5 Brinell hardness test

Figure 11 shows the average results found in
the Brinell test. As expected, the found results
Figure 9. Briquettes combusting inside the
were quite low for all briquettes. Since they
steel cylinders.
are agglomerated materials, formed mainly
Table 6. Fe-Nb briquettes before and after the mechanical forces their resistance to
(main body and fragments) thermal shock indentation must be low and, in this case,
test. compatible with a polymeric material or
minerals with Mohs hardness bellow gypsum.
After
Briquette Before
Immersion Drying

R100-0-0

R0-100-0

Figure 11. Briquettes average Brinell

hardness.
H60-40-0
3.2.6 Tumbler drum test
Figure 12 shows the average granulometric
analyse of the briquettes after the tumbler test.
Considering the material passing in sieve with
aperture 3/4" (or 19.0 mm) only the briquette
H50-40-10 R100-0-0 had a considerable resistance,
producing 34% of its mass bellow this
aperture. This result is consistent with the
Brinell hardness result, since the R100-0-0
was the briquette hardener one and the
tumbler test evaluate the shear resistance of
the material. The other briquettes had results
above 80% of passing (98.5% for R0-100-0,
89.2% for H60-40-0 and 81.9% for H50-40-
10).

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IMCET 2017 / ANTALYA / TURKEY / April 11-14
Figure 12. Granulometric analyse of the
briquettes after the tumbler test.
4 CONCLUSIONS
Regarding the shatter test, all tested briquettes
succeeded in the test considering the literature
parameters. However, the found results were
heterogeneous and a trend could not be
stablished. Briquettes manufactured by
Höganäs (cylinders) showed results slightly
more homogeneous than the ones
manufactured by Renova.
It was possible to notice in the uniaxial
compression test that briquettes manufactured
by Höganäs had better results, however
showing a standard deviation higher than
Renova’s briquettes. This fact may be due to
the geometry of them, once Höganäs’
briquettes have a better stress distribution
because of their cylindrical shape. The same
briquettes showed a higher than expected
uniaxial tension resistance.
All briquettes were able to resist the water
absorption test retaining their shapes. For
higher immersion time Höganäs’ briquettes
complete disintegrate, not retaining either
shape or mechanical resistance. In some
briquettes, immersed for 48 hours, it was
possible to notice some oxidation spots on
them. Only one briquette (R0-100-0) did not
gain mass after the test.
Regarding the thermal shock, all briquettes
were successful. Although it was not possible
to stablish a trend from the obtained results,
the briquettes ignition temperature was
stablished bellow 550 oC (450 °C for R0-100-
0 and H50-40-10, 475 °C for H60-40-0 and
550 °C for R100-0-0.
Briquettes showed a low Brinell hardness,
which was expect one they were only
356
agglomerated through mechanical stress,
without the addition of any kind of chemical
binder.
At last, regarding the tumbler test all types
of briquettes generated fine particles during
the test. Although the briquette R100-0-0
showed a higher resistance compared with the
others.
Summarizing the found results both
fabrication methods can be industrially
adopted for briquette production with
parameters acceptable by the steel making
marketing. All fine particle blends tested were
successful regarding the briquette chemical
composition and mechanical properties. It
was not possible to choose one manufacture
method between the two tested because the
found results were quite different. In the end,
the authors suggest the adoption of the
cylindrical briquettes manufactured by
Höganäs as the best choice, combining good
results in most of the tests and the lower
manufacture costs.
ACKNOWLEDGEMENTS
The authors thank financial support from the
Brazilian agencies CNPq, CAPES, FAPEG
and FUNAPE. In addition, we like to thank
NioBrás for the samples donation and
chemical analyses and Federal University of
Goiás.
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