Powder Technology 249 (2013) 212–219

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Powder Technology
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Effect of basicity on sintering behavior of saprolitic nickel laterite in air

Guanghui Li, Qian Zhi, Mingjun Rao ⁎, Yuanbo Zhang, Wen Cai, Tao Jiang ⁎⁎
School of Minerals Processing & Bioengineering, Central South University, Changsha, Hunan 410083, China

a r t i c l e i n f o a b s t r a c t

Article history: Nickel pig iron (NPI) production has been experiencing robust development recently in China. For NPI production
Received 20 December 2012 by smelting technology in either a blast furnace or an electric arc furnace, sintering is imperative to supply a qual-
Received in revised form 29 July 2013 ified feedstock. In this research, the sintering behaviors of saprolitic nickel laterite with various quaternary basic-
Accepted 12 August 2013
ities ((CaO + MgO)/(SiO2 + Al2O3) mass ratio) were investigated in terms of phase transformation,
Available online 27 August 2013
microstructure and fusion temperature. Experimental results show that the main minerals formed during
Keywords:
sintering with natural basicity are refractory materials such as spinel ((Mg,Ni)(Fe,Al,Cr)2O4), forsterite ((Mg,
Saprolitic nickel laterite Fe)2SiO4) and enstatite ((Mg,Fe)SiO3). With increasing basicity from natural basicity (0.50) to 2.0, all the three
Nickel pig iron fusion characteristic temperatures decrease initially and then increase with a valley at the basicity of 1.0. It's re-
Sintering vealed that the addition of an appropriate amount of CaO could lower the liquid temperature and increase the
Basicity amount of melt, improving the sintering consolidation of saprolitic nickel laterite.
CaO © 2013 Elsevier B.V. All rights reserved.

1. Introduction on BF/EAF performance [10]. As for the sintering of saprolitic nickel

Nickel is one of the most important strategic metals, which is mainly
used as refined nickel and ferronickel with variable iron content in the
industrial world, and roughly two-thirds of global nickel production
goes to stainless steel manufacture [1–3]. According to a global and
China nickel industry report [4], the global output of the stainless steel
was over 32.0 million tons in 2011, and would reach 40.0 million tons
in 2012. China is the world leader in stainless steel production as well
as nickel consumption. In 2011, China nickel output approximated to
446,000 tons, with the proportion of electrolytic nickel and nickel pig
iron (NPI) registering 41.5% and 56.5%, respectively [5].
NPI is a low grade ferronickel used as a cheaper alternative to
electrolytic nickel for the production of stainless steel [6]. The alterna-
tive was developed as a response to the high price of electrolytic nickel.
Nickeliferous laterite ore is smelted in either a blast furnace (BF) or an
electric arc furnace (EAF) depending on the desired grade [7]. With
the trend of closing small and less efficient iron making blast furnaces
in China, these small blast furnaces less than 300 m3 have been
switched to NPI production.
Nickeliferous laterite accounts for about 70% of the world's land-
based nickel resources, while only holds 40% of the global nickel output
[8,9]. As nickeliferous laterite ore is the exclusive nickel-bearing materi-
al for NPI production, sintering is imperative in advance of smelting in
either a blast furnace or an electric arc furnace to supply a qualified
feedstock with consistent chemical and physical properties. Therefore,
sinter quality and consistency are bound to have a significant impact
⁎ Corresponding author. Tel./fax: +86 731 88830542.
⁎⁎ Corresponding author. Tel./fax: +86 731 88877656.
E-mail addresses: raomingjun2003@126.com (M. Rao), jiangtao@csu.edu.cn (T. Jiang).
laterite, the high water content and refractory materials generated
from the dehydroxylation of hydrated magnesium silicates during
sintering hinder the generation of melt phase, which brings about
problems such as poor sinter quality, low productivity and high energy
consumption.
Therefore, it's necessary to investigate the sintering behavior of
saprolitic nickel laterite and facilitate the formation of melt phase for
consolidation. Until recently, there is a lack of knowledge about the
sintering behavior of laterite ore. Lv et al. find that forsterite (Mg,
Fe)2SiO4 is the main bonding phase during the sintering of both
Philippine and Indonesia laterites without the addition of CaO in an
experimental scale sinter pot [11]. Our present work was conducted to
investigate the effect of CaO addition on sintering behavior of saprolitic
nickel laterite, aiming at improving the sintering performance and
providing a theoretical basis and technical support for the sinter
production. Optical Microscope, X-ray Diffractometer (XRD), Environ-
mental Scanning Electron Microscope (ESEM) and Energy Dispersive
Spectrometer (EDS) were used to examine the phase transformation
and microstructure of the sinter. Fusion temperatures of the laterite
sample with various basicities were measured to verify the effect of
basicity.
2. Experimental
2.1. Materials
2.1.1. Saprolitic nickel laterite
The saprolitic nickel laterite used in the present work was taken
from Sulawesi Island, Indonesia. The sample was dried at 110 °C for
2 h, and then ground to 100 wt.% passing 0.5 mm for the experiments

0032-5910/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.powtec.2013.08.018
 G. Li et al. / Powder Technology 249 (2013) 212–219 213

Table 1 100 1.5

Main chemical composition of the laterite ore sample (mass fraction, %). Mass change-3.64% Peak 809 C
o

98
Fe2O3 Ni SiO2 MgO Al2O3 CaO Cr2O3 LOIa o
1.0
Peak 597 C
31.91 1.91 26.49 13.42 4.25 2.04 1.68 13.18 96

DSC/(mW/mg)
a o
LOI—loss on ignition. 94
Peak 271 C
0.5

TG/%
Mass change-4.93%

92
0.0
of sintering and fusion temperature determination. A sub-sample was 90 o
Peak 89 C Mass change-3.68%
further ground to 90 wt.% passing 74 μm for chemical composition
and mineral constitute analyses. As shown in Table 1, the laterite is 88 Mass change-0.91% -0.5
characterized as high in magnesia and silica content. According to the
XRD results in our previous work [12], the ore mainly consists of 86
-1.0
lizardite (Mg,Fe)3Si2O5(OH)4, goethite FeO(OH), and hematite Fe2O3. 0 200 400 600 800 1000 1200
o
Temperature/ C
2.1.2. Flux
CaO of analytic grade was used as flux in this work to adjust the Fig. 2. TG-DSC curves of the saprolitic nickel laterite sample.
basicity of sinter, and its particle size is less than 74 μm.
H- Hematite (Fe2O3) E- Enstatite ((Mg,Fe)SiO3)
F- Forsterite ((Mg,Fe)2SiO4) S- Spinel (MgFe2O4)
2.2. Methods S
E
2.2.1. Sintering S
S S
E F S
E S
Simulative sintering experiment was conducted in a horizontal S
S
E S S1300oC
S
resistance furnace, and the schematic diagram of the furnace was S
S
S
shown in Fig. 1(a). The laterite ore sample was mixed with a certain E E S
S F S S 1200oC
quantity of CaO according to the required amount. No solid fuels were S
H
added into the mixture. The mixture was then briquetted by a mold H
S
into a cylindrical briquette with a diameter of 10 mm and height of H SE F S S
H H S H o
1100 C
S
H
15 mm at a pressure of 5 MPa maintained for 1 min. The cylindrical
briquettes were dried at 110 °C for 4 h, and then put into a corundum S H
E F S S S
S
S S
FH F F H FH H 1000 C
o

porcelain boat and sintered in air atmosphere for 10 min at temperature H

H
o
F H H HH 900 C
ranging from 800 °C to 1300 °C. FH E H F
H HF H H H o
800 C
H HH

2.2.2. Fusion temperature determination 10 20 30 40 50 60 70 80

The preparation of the mixture and the heating equipment are the
same as those of the sintering tests. The mixture was shaped by a
mold into a pyramid with a bottom side length of 12 mm and vertical
height of 35 mm. The pyramid was placed on a corundum plate and
heated in the horizontal tube furnace with a heating rate of 10 °C/min
in air atmosphere from 900 °C to 1500 °C. The external shape changing
of each specimen was recorded by a camera every 10 s and character-
ized by the standard as described in the literature [13]. Three character-
istic temperatures were identified (Fig. 1 (b)), namely: (1) deformation
temperature (TD), determined by the temperature at which the tip of
the pyramid becomes spherical; (2) sphere temperature (TS), deter-
mined by the temperature at which the whole pyramid deforms to be
Two-Theta/degree
Fig. 3. XRD patterns of saprolitic nickel laterite briquettes without addition of CaO sintered
at different temperatures for 10 min in air atmosphere.
hemispheric; (3) flow temperature (TF): determined by the tempera-
ture at which the pyramid melts until the vertical height is less than
1.5 mm.
2.2.3. Characterization
TG-DSC analysis of raw ore sample was performed using a thermal
analyzer (Netzsch STA 449 C, Germany) in the temperature range of

a 1 2 3 4 5 6

1. Thermocouple;
2. SiC tube;
3. Pyramid;
4. Al2O3 tube;
b 5. Camera;
6. Computer.
Original TD TS TF
Change of external shape with increasing temperature

Fig. 1. Schematic diagram of horizontal tube furnace (a), and change of external shape of the pyramid during heating (b).
214 G. Li et al. / Powder Technology 249 (2013) 212–219

a b

Enstatite

Forsterite
Spinel

Fig. 4. Optical micrographs of saprolitic nickel laterite briquette without addition of CaO sintered at 1300 °C for 10 min in air atmosphere.

a b
2 Spinel

c d
Enstatite Forsterite

Fig. 5. ESEM–EDS results of saprolitic nickel laterite briquette without addition of CaO sintered at 1300 °C for 10 min in air atmosphere; (a): backscattered electron image, (b): EDS spec-
trum of spot 1, (c): EDS spectrum of spot 2, (d): EDS spectrum of spot 3.
 G. Li et al. / Powder Technology 249 (2013) 212–219 215

Silicate Melting
point/ oC
Forsterite
(Mg2SiO4) 1898
O
Enstatite
(MgSiO3) 1577
Wollastonite
M (CaSiO3) 1558

Calcium silicate
(Ca2SiO4) 2130
Cuspidine
(Ca3SiO5) 2070

Rankinite
(Ca3Si2O7) 1410
Diophide
(CaMgSi2O6) 1391
Akermanite
(Ca2MgSi2O7) 1590
N
Merwinnite
(Ca3MgSi2O8) 1598

Fig. 6. CaO–MgO–SiO2 system ternary phase diagram and melting points of different silicates [15,16].

30 °C to1200 °C with a heating rate of 10 °C/min, and in air atmosphere. backscatter electron mode operating in a low vacuum of 0.5 Torr and
After sintering, X-ray diffraction (XRD) patterns of sintered briquettes 20 keV. The specimens were coated with gold prior to the detection.
were recorded by a diffractometer (RIGAKU D/Max 2500, Japan)
under the conditions of radiation: Cu Kα, tube current and voltage:
3. Results and discussion
250 mA, 40 kV, scanning range: 10–80° 2θ, step size: 0.02° 2θ and
scanning speed: 8°/min. The polished sections of sintered briquettes
3.1. Sintering characteristics of saprolitic nickel laterite without addition
were prepared to observe the phase changes and analyze the elemental
of CaO
content of the phases, using Optical Microscopy (LEICA MDI5000 M,
Germany) and Environmental Scanning Electron Microscopy (ESEM,
3.1.1. Phase transformation
FEI QUANTA 200, Holland) equipped with an EDAX energy dispersive
Phase transformation of the saprolitic nickel laterite without the
X-ray spectroscopy (EDS) detector. ESEM images were recorded in
addition of CaO (natural basicity) sintered at different temperatures
for 10 min was examined. In advance, TG-DSC analysis of the laterite
sample was carried out and the result is presented in Fig. 2. The evapo-
ration of free water, crystallization water in the goethite and constitu-
tion water in the lizardite contribute to the endothermic peak at
89 °C, 271 °C and 597 °C, respectively. The exothermic peak that occurs
F - Forsterite ((Mg,Fe)2SiO4) S - Spinel ((Mg,Ni)(Fe,Al,Cr)2O4 ) E - Enstatite ((Mg,Fe)SiO3 ) at 809 °C is due to the crystallization of silicate. Thus, during the
D - Diopside (CaMgSi2O6) A - Akermanite (Ca2MgSi2O7) M - Merwinnite (Ca3Mg(SiO4)2)
S
sintering process, high energy consumption is demanded due to the
M
A
SAM
M M S MM A
S M S
R 2.0
decomposition of goethite and lizardite.
S
A
M
XRD results of the sintered briquettes are shown in Fig. 3. At the tem-
S S S
A A M A M M S MM A M R 1.8 perature of 800 °C, the major mineral constituents are hematite (Fe2O3)
A
S
and forsterite ((Mg,Fe)2SiO4) which are generated from the dehydra-
AS
A A A A M AA A SA
M A
A S S
A R 1.6 tion of goethite and dehydroxylation of lizardite, respectively. With
A
S
the sintering temperature increasing to 900 °C, MgSiO3 (amorphous)
A A A ADS AA A
A
SA
A A A
A S
S
A R 1.4
transforms into enstatite (MgSiO3) [14], which could also be confirmed
S
A
by the above-mentioned exothermic peak at 809 °C of TG-DSC analysis.
DS
A F A DA D A D S D AF D
S S
DD R 1.2 At the temperature of 1000 °C, some spinel (MgFe2O4) is detected. With
S
D
S
the sintering temperature increasing further, the content of Fe2O3
S
F DD
D D
S
F DSD F DS DD R 1.0 continuously decreases and vanishes at temperature in the excess of
D
S
1200 °C. Meanwhile, the amount of spinel as well as the enstatite
S S
D D F DS D
F DD
S
F S D R 0.8 increases significantly.
E S S S S
D E E D
S
E S R 0.6
E S
E F S E S S R 0.5 3.1.2. Microstructure
Optical micrographs and ESEM–EDS results of the polished cross-
10 20 30 40 50 60 70 80
section of briquette with natural basicity sintered at 1300 °C are
Two - Theta / degree
shown in Figs. 4 and 5, respectively. The micrographs in Fig. 4 indicate
Fig. 7. XRD patterns of saprolitic nickel laterite briquettes with different basicities sintered that there is no obvious melt phase generated at the sintering tempera-
at 1300 °C for 10 min in air atmosphere. ture of 1300 °C, and the consolidation is mainly performed by solid state
216 G. Li et al. / Powder Technology 249 (2013) 212–219

a Spinel b

1
2
3

c d
Forsterite Diopside

Fig. 8. ESEM–EDS analyses of saprolitic nickel laterite briquette with basicity of 1.0 sintered at 1300 °C for 10 min in air atmosphere; (a): backscattered electron image, (b): EDS spectrum
of spot 1, (c): EDS spectrum of spot 2, (d): EDS spectrum of spot 3.

reactions. Mineral particles of spinel, enstatite and forsterite remain
relatively independent. Spinel ((Mg,Ni)(Fe,Al,Cr)2O4) exists in the
form of solid solution through the ion substitution between Ni2+and
Mg2+ as well as Al3+, Fe3+ and Cr3+ according to Fig. 5(b).
3.2. Sintering characteristics of saprolitic nickel laterite with addition of
CaO
Experimental results of saprolitic nickel laterite without the addition
of CaO sintered at 1300 °C demonstrate that the main mineral constitu-
ents are refractory materials such as spinel, forsterite and enstatite,
whose melting points are 1750 °C, 1898 °C and 1577 °C, respectively
[15]. These refractory minerals are unfavorable for the formation of
melt phase for consolidation in the sintering operation.
Therefore, regarding the sintering of saprolitic nickel laterite, an
alternative bonding phase rather than the calcium ferrite is needed
compared with high-grade iron ore. The CaO–MgO–SiO2 system ternary
phase diagram as shown in Fig. 6 indicates that in the MgO–SiO2 binary
system, mineralogical constituents are refractory minerals with high
melting point. The silicate with the lowest melting point diopside
(CaMgSi2O6) could be generated during the range of MgO/SiO2 ratio
from 0.16 to 0.54 (as the line MN–MO shown in Fig. 6). The MgO/SiO2
ratio of sample used in this study is 0.5 which is in this range. With
the increase of CaO content, the melting point of the ternary system
decreases initially and then increases. While, with the further increasing
CaO content, diopside transforms into akermanite (Ca2MgSi2O7) and
merwinite (Ca3Mg(SiO4)2) successively, leading to the increase of the
melting point again. Therefore, it can be concluded that the suitable
amount of CaO is capable of reducing the melting point of saprolite-
type laterite ore at a given MgO/SiO2 ratio, and is favorable of reducing
sintering temperature.
3.2.1. Phase transformation
Based on the analysis of CaO–MgO–SiO2 system ternary phase dia-
gram, CaO was mixed with the laterite sample attempting to enhance
the formation of diopside for better consolidation. Additionally,
according to the XRD and ESEM–EDS results from Figs. 3 and 5, Al2O3
mainly exists in the form of spinel after sintering, consuming a
proportion of MgO content. Therefore, Al2O3 content in the raw
laterite sample should be taken into consideration when evaluating
the effect of CaO on the sintering behavior. Consequently, quaternary
 G. Li et al. / Powder Technology 249 (2013) 212–219 217

3 a b
Diopside

c d
Akermanite Forsterite

Fig. 9. ESEM–EDS analyses of saprolitic nickel laterite briquette with basicity of 1.2 sintered at 1300 °C for 10 min in air atmosphere; (a): backscattered electron image, (b): EDS spectrum
of spot 1, (c): EDS spectrum of spot 2, (d): EDS spectrum of spot 3.

a b
Pores
Diopside
Forsterite

Spinel

Fig. 10. Optical micrographs of the polished cross-section of saprolitic nickel laterite briquette with basicity of 1.0 sintered at 1300 °C for 10 min in the air atmosphere.
218
1440
1420 Deformation Temperature
Sphere Temperature
Flow Temperature
1400
1380
Temperature/oC
1360
1340
1320
1300
1280
1260
0.4 0.6 0.8 1.0 1.2 1.4 1.6
(CaO+MgO)/(SiO2+Al2O3)
Fig. 11. Effect of basicity on fusion temperatures of saprolitic nickel laterite.
basicity ((CaO + MgO)/(SiO2 + Al2O3) mass ratio) was adopted in
the present research.
Briquettes with various basicities were sintered at the temperature
of 1300 °C for 10 min. XRD results of the sintered briquettes are
shown in Fig. 7. With the basicity increasing from natural basicity
(0.5) to 1.0, diffractions of enstatite taper off while those of diopside
are enhanced gradually. With the basicity rising from 1.0 to 2.0,
diffractions of diopside decrease and disappear at the basicity of 1.6.
Meanwhile, akermanite and merwinite begin to appear with an exces-
sive amount of CaO. These results demonstrate that the formation of
diopside is achieved at the basicity ranging from 0.6 to 1.4, and the op-
timal basicity is 1.0. An excessive basicity is detrimental to the stability of
diopside, due to the formation of akermanite and merwinite.
3.2.2. Microstructure
The ESEM–EDS analyses of briquettes with basicities of 1.0 and 1.2
sintered at 1300 °C are shown in Figs. 8 and 9, respectively. Fig. 8
supports the XRD result of Fig. 7, demonstrating that the major mineral
constituents are forsterite, spinel and diopside at the basicity of 1.0. As
the basicity increases to 1.2, a portion of diopside transforms into
akermanite (Fig. 9(c)).
Fig. 10 presents the micrographs of polished cross-section of
sintered briquette with the basicity of 1.0. Combined with the results
of ESEM–EDS, it can be concluded that the minerals in regions presented
in light gray, dark gray and puce are diopside, akermanite and forsterite,
respectively. Minerals with high melting points such as spinel and
forsterite are embedded in diopside and present decentralized state.
Many large pores can be found in Fig. 10(a) which indicates that the
melt phase is generated abundantly and bonded together with spinel
and forsterite. Therefore, the quality of the laterite sinter is improved
markedly.
3.3. Fusion temperature
Experimental results (Figs. 3 and 5) reveal that the main mineral con-
stituents of saprolitic laterite ore with natural basicity sintered at
1300 °C are refractory materials including spinel, forsterite and enstatite
whose melting points are 1750 °C, 1898 °C and 1577 °C, respectively
[15]. Consequently, as shown in Fig. 11, the fusion characteristic temper-
atures of the laterite ore with natural basicity namely TD, TS, and TF are
1385 °C, 1395 °C and 1407 °C, respectively. Fig. 11 indicates that CaO
has a significant effect on the fusion temperatures. With the basicity in-
creasing from natural basicity (0.50) to 2.0, the fusion characteristic tem-
peratures (TD, TS, and TF) of the laterite ore decrease initially and then
increase with a valley at the basicity of 1.0, at which TD, TS and TF are
1272 °C, 1299 °C and 1306 °C, respectively. The variation tendency of
G. Li et al. / Powder Technology 249 (2013) 212–219
fusion characteristic temperatures supports the analysis in CaO–MgO–
SiO2 system ternary phase diagram (Fig. 6), and is also in consistent
with the phase transformation of laterite ore sintering with varying basic-
ity (Fig. 7). As mentioned previously, the formation of diopside is achieved
at the optimal basicity of 1.0, while an excessive basicity is detrimental to
the stability of diopside, leading to the formation of akermanite and
merwinite. Thus, the fusion characteristic temperatures would increase
with the transformation of diopside into akermanite and merwinite.
The mineral with low melting point is crucial for the formation of pri-
mary melt phase. Diopside with the lowest melting point of 1391 °C in
the CaO–MgO–SiO2 system is the optimal choice for a bonding phase
during sintering. The formation and stability of diopside are obviously
influenced by the addition of an amount of CaO, and the optimal basicity
for the sintering of saprolitic nickel laterite is 1.0. In addition, it should be
1.8 2.0
noticed that the simulative sintering conditions in this work such as
combustion zone maximum temperature and sintering atmosphere
differ from the actual sintering conditions to some extent. In this case,
sintering behavior of saprolitic nickel laterite may also be different and
further research should be done to clarify the difference.
4. Conclusions
The sintering behavior of saprolitic nickel laterite with varying basicity
adjusted by the addition of CaO was investigated in the air, attempting to
find a way to improve the sintering performance of the saprolitic nickel
laterite. The following conclusions are obtained:
(1) Mineralogical constituents of saprolite nickel laterite sintering
with natural basicity (R = 0.5) are refractory minerals with
high melting point namely spinel ((Mg,Ni)(Fe,Al,Cr)2O4), forsterite
((Mg,Fe)2SiO4) and enstatite ((Mg,Fe)SiO3), which are unfavor-
able to the formation of melt phase for consolidation.
(2) Quaternary basicity ((CaO + MgO)/(SiO2 + Al2O3) mass ratio)
should be adopted to evaluate the effect of CaO on sintering
behavior of saprolitic nickel laterite, as Al2O3 consumes a portion
of MgO to form spinel during the sintering.
(3) CaO has a significant effect on the phase transformation, micro-
structure and fusion temperatures during the sintering of the
saprolitic nickel laterite. With the basicity rising from natural ba-
sicity (0.5) to 1.0, diffractions of enstatite taper off while diopside
increases gradually. Moreover, an excessive basicity results in the
akermanite and merwinite. With the basicity increasing from
natural basicity (0.50) to 2.0, the fusion characteristic tempera-
tures of the laterite ore decrease initially and then increase
with a valley at the basicity of 1.0.
(4) An appropriate amount of CaO addition is able to facilitate the
formation of melt phase and improve the consolidation of the
sintering of saprolite nickel laterite, and the optimal basicity for
the sintering of saprolitic nickel laterite is 1.0.
Acknowledgments
The authors wish to express their thanks to the National Natural Sci-
ence Foundation of China (51174230 and 51234008), Program for New
Century Excellent Talents in University (NCET-11-0515) and the Hunan
Provincial Innovation Foundation for Postgraduate (CX2011B124) for fi-
nancial support for this research.
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