Minerals Engineering 24 (2011) 1556–1562

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

The reduction of nickel from low-grade nickel laterite ore using a solid-state
deoxidisation method
Bo Li, Hua Wang ⇑, Yonggang Wei
Engineering Research Center of Metallurgical Energy Conservation and Emission Reduction Ministry of Education, Kunming University of Science and Technology,
Kunming 650093, China

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

Article history: The reduction of nickel from low-grade nickel laterite ore using a solid-state deoxidisation method was
Received 22 May 2011 studied. The effects of temperature, time, reductant type and CaO content on the conversion percentage
Accepted 12 August 2011 of the total nickel to metallic nickel (aNi) in the nickel laterite ore reduction process were investigated.
Available online 15 September 2011
The results showed that aNi was strongly influenced by the reaction temperature in both gas–solid and
solid–solid reduction processes, and a higher temperature was more favourable for nickel reduction.
Keywords: Because the reduction mechanism of nickel laterite ore (NiO + CO ? CO2 + Ni) is indirect, a higher aNi
Nickel laterite ore
(>80%) can be obtained by increasing the CO and anthracite content. In the gas–solid reduction process,
Conversion percentage
Metallic nickel
a longer reaction time favoured nickel reduction, and the conversion percentage decreased when a gas-
Solid state deoxidisation eous reductant was used at 850 °C because of phase transformation. In the solid–solid reduction process,
the conversion percentage of the total nickel to metallic nickel first increased and then decreased with
increasing reduction time and CaO content. In both reduction processes, taenite was found by XRD in
the reduced ore because of iron oxide reduction and metallic nickel formation. SEM revealed that the
nickel laterite ore was transformed from large granular and sandwich structures to small granular and
flocculent structures during the reduction process.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction grade ores and substantial energy input. Hydrometallurgical

In recent years, there has been an increased focus on the utilisa-
tion of low-grade nickel laterite ore, along with a growing demand
for stainless steel and a declining supply of sulphide ores (Zhai
et al., 2010). Among these sulphide ores, nickel laterite ore com-
prises 73% of the world’s nickel resources and will be the dominant
source of nickel in the future. With the continuous depletion of
high-grade nickel ores such as millerite and niccolite, nickel later-
ite ores have become the major source for the production of nickel
metal. However, currently, only 42% of the world’s production of
nickel comes from nickel laterite ore because the concentration
of nickel in the ore is low (Jungah et al., 2010). Therefore, in the
long term, it will be necessary to optimise nickel extraction from
nickel laterite ore.
Both pyrometallurgical and hydrometallurgical processes have
been applied commercially to recover nickel from nickel laterite
ore. Pyrometallurgical techniques are suited to treat saprolite, with
processes typically involving drying, calcining, reduction and electric
furnace smelting to produce a ferronickel or nickel sulphide matte.
The disadvantages of these processes include the requirement of high
⇑ Corresponding author.
E-mail address: wanghuaheat@hotmail.com (H. Wang).
processes are more applicable to limonite ores and include ammo-
nia–ammonium carbonate leaching, atmospheric leaching with sul-
phuric acid and high-pressure acid leaching. These processes have
the disadvantages of low extraction of nickel and substantial energy
and reagent requirements (Guo et al., 2009).
Several investigations of nickel oxide or nickel laterite ore
reduction have been performed. For example, Krasuk et al. studied
the reduction of nickel oxide with CO, Utigard et al. studied the
reduction kinetics of Goro nickel oxide using hydrogen and James
et al. used X-ray diffraction (XRD) to study nickel oxide reduction
by hydrogen. Nickel laterite ore reduction by H2- and CO-contain-
ing gases in a horizontal tube furnace and in a laboratory-scale flu-
idised bed reactor was studied by Olli, Valix et al. mixed reducing
gases to study the effect of sulphur on laterite ores during high-
temperature reduction. Li et al. completed a simulation study on
the pre-reduction and calcination processing of nickel laterite ore
with coke to determine the effect of temperature, time, atmo-
sphere and CaO content on the nickel reduction rate. Enriching
metallic nickel from nickel laterite ore using a thermal carbon
reduction-magnetic separation process with activated carbon
powder as the reductant was investigated by Xu et al.
(Krasuk and Smith, 1972; Utigard et al., 2005; James et al., 2003;
Olli et al., 1995; Valix and Cheung, 2002; Li et al., 2009; Xu et al.,
2010).

0892-6875/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.mineng.2011.08.006
 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562 1557

-100 3. Experimental
-150
The chemical composition of low-grade nickel laterite ore was
-200 iO analysed by chemical analysis. The XRD experiments were per-
2N
O 2=
-250 2 Ni+ formed on a Japan Science D/max-R diffractometer apparatus with
G (KJ. mol-1)

CO 2 Cu Ka radiation (k = 1.5406 Å), an operating voltage of 40 kV and a

-300 =2
+ O2 current of 40 mA. The diffraction angle (2h) was scanned from 5° to
440 O
2C 80°. The morphology and particle size were determined using
-350
scanning electron microscopy (SEM) on a Philip XL30 scanning
-400 2C
+O electron microscope. Simultaneous differential scanning calorime-
=2
2 CO try (DSC) and thermogravimetric (TG) analysis were performed on
-450
a NETZSCH STA 449F3 unit under a nitrogen atmosphere, at a heat-
-500
ing rate of 10 °C/min.
-550 Nickel laterite ore contains a large amount of water, with a
moisture content on a dry basis of up to 50%, in the form of ad-
0 200 400 600 800 1000 1200 1400 1600 1800
sorbed and crystallised water. Drying was performed at 650 °C in
T (ºC)
a corundum crucible within a muffle furnace for 1 h. Dried nickel
Fig. 1. Standard Gibbs free energy (DGH) of carbon oxide and nickel oxide. laterite ores were ground to a 100 mesh-size using a laboratory-
scale ball mill. The sample was then screened using a sieve and
In this study, the reduction of nickel from low-grade nickel granulated according to the experimental requirements.
laterite ore was performed using a solid-state deoxidisation meth- The reduction of nickel from low-grade nickel laterite ore was
od. Moreover, both gaseous and solid reductants were used, and performed in a fixed bed apparatus, as shown in Fig. 2. In the
the effects of the reduction temperature, reduction time, CO reduction process using a gaseous reductant, gases, which included
content, carbon content and CaO content on the nickel reduction CO and CO2, were metered into the reactor using a mass flow me-
process were examined. The reduction characteristics of nickel ter. The reduction procedure involved flushing the tube with nitro-
from nickel laterite ore were studied on a thermodynamic basis, gen prior to heating. Reducing gases were then metered into the
using the conversion percentage and phase analysis. tube while it was heated to the required temperature. After the
reduction was completed, nitrogen was metered into the reactor
2. Thermodynamic basis for nickel reduction
while it was cooled. In the reduction process using a solid reduc-
tant, anthracite (the reductant) and the ore powder were uniformly
In the process of the reduction of nickel from nickel laterite ore,
mixed in a glass container and were then added to a fixed bed
the main reactions of nickel oxide to metallic nickel are shown as
apparatus. The temperature was kept for limited time when it
follows (Li et al., 2009):
reached the reduction temperature of nickel laterite ore, and then
C þ CO2 ¼ 2CO DGH ¼ 166550  171T J=mol ð1Þ nitrogen was metered into the reactor while it was cooled. The car-
bon content was determined based on the amount of anthracite
NiO þ C ¼ Ni þ CO DGH ¼ 124800  175T J=mol ð2Þ added. The samples were analysed by chemical separation and
instrumental analysis, and the conversion percentage of the total
nickel to metallic nickel (aNi) was calculated using the following
NiO þ CO ¼ Ni þ CO2 DGH ¼ 40590  0:42T J=mol ð3Þ
formula. Where WNi is the metallic nickel content (%), and W is
H
The standard Gibbs free energies (DG ) of carbon oxide and the total nickel content (%).
nickel oxide are shown in Fig. 1. As shown in this graph, the lowest
temperature at the atmospheric pressure at which the NiO reduc- W Ni
aNi ¼  100%
tion by fixed carbon will occur is 440 °C. In addition, the curve of W
the standard Gibbs free energy of forming NiO is higher than that
of CO2, and the standard Gibbs free energy of reaction (3) is nega- 4. Results and discussion
tive at the standard atmospheric pressure; therefore, NiO is easily
reduced by CO. 4.1. Characterisation of raw nickel laterite ore
In fact, nickel laterite ore is a complex ore, which include NiO,
Fe2O3, Fe3O4, etc., so other reactions simultaneously take place in The chemical composition of the raw nickel laterite ore is
the reduction process. Based on the reduction of trevorite, shown in Table 1. The ore contained approximately 1.09 mass%
NiOFe2O3, with the preferential reduction of nickel oxide to metal- Ni, 9.12 mass% Fe, 2.47 mass% Al2O3, 37.6 mass% SiO2 and 29.08
lic nickel can be stated (4)–(6) (Olli et al., 1995): mass% MgO, which is typical of low-grade nickel laterite ore com-
bined with lizardite. The ultimate analysis of anthracite is shown in
3NiO  Fe2 O3 þ CO ¼ 3NiO þ 2Fe3 O4 þ CO2 ð4Þ
Table 2. The anthracite contained approximately 87.43 mass% C,
2.89 mass% H, 1.08 mass% O, 1.63 mass% N and 0.35 mass% S.
NiO þ 2Fe3 O4 þ CO ¼ Ni þ 2Fe3 O4 þ CO2 ð5Þ
Anthracite is not pure carbon, but carbon content of anthracite is
very high.
Ni þ Fe3 O4 þ CO ¼ Ni þ 3FeO þ CO2 ð6Þ
Fig. 3 shows the XRD pattern of the nickel laterite ore. XRD anal-
The further reduction of wustite to metallic iron takes place: ysis indicated that lizardite [(Mg,Al)3[(Si,Fe)2O5](OH)4], quartz
[SiO2], magnetite [Fe3O4] and hematite [Fe2O3] are the primary
FeO þ CO ¼ ½FeNi þ CO2 ð7Þ
crystalline phases. Additionally, no crystalline nickel structures
According to the experimental conditions, the reduction process were observed, suggesting that the structure of nickel is predomi-
can be carried out to the reduction (6), but the reduction (7) is dif- nately amorphous, or its concentration is below the detection limit
ficult to carry out. These results demonstrate that it is feasible to (Jungah et al., 2010). Goethite was not detected in this sample,
reduce nickel oxide from nickel laterite ore using a solid-state indicating that adsorbed water was removed from the nickel later-
deoxidisation method. ite ore, changing goethite to hematite through heating.
1558 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562

Fig. 2. Schematic diagram of the reduction apparatus.

Table 1
The chemical composition of nickel laterite ore (unit: mass%).
-lizardite
Elements Ni Co Fe Cr2O3 MgO Al2O3 CaO SiO2
Content 1.09 0.023 9.12 0.34 29.08 2.47 0.030 36.48
-quartz
-magnetite
-hematite
Intensity (cps)

Table 2
The ultimate analysis of anthracite (unit: mass%).

Elements C H O N S
Content 87.43 2.89 1.08 1.63 0.35

TG/DSC was used to determine the thermal properties of nickel

laterite ore, as shown in Fig. 4. As a result of the endothermic and
exothermic processes, two main peaks were observed in the DSC
thermogram. The first main peak at 610 °C is the result of the re-
moval of crystallised water from lizardite, which corresponds to
20 40 60 80
a weight loss of 9.6%. Lizardite also decomposes to form an amor-
2 Theta (º)
phous magnesium silicate phase. The second main peak at 820 °C is
the result of a change in structure, which corresponds to a phase Fig. 3. XRD patterns of nickel laterite ore.
transformation from lizardite to forsterite (Flavio, 1992).
Fig. 5 shows the SEM images of nickel laterite ore. The internal
structure of the nickel laterite ore is loose, which is favourable for 4.2. The reduction of nickel from nickel laterite ore using a gaseous
water storage. Sandwich and granular structures were also found. reductant
The sandwich structure is thick, and the edges and corners are
composed of granular structures. Mineralogical analyses have re- 4.2.1. Effect of reduction temperature
vealed that nickel laterite ore is mainly composed of lizardite in Based on the experimental requirements, the reduction temper-
a sandwich-like morphology and quartz in an irregular hexagonal ature was varied in the range of 600 and 1000 °C. Fig. 6 shows the
granular structure (Li et al., 2011). conversion percentage of the total nickel to metallic nickel as a
 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562 1559

100 7 90
exo
98 6
80

Reduction rate (%)

96 5
Peak:610ºC 70

DSC/ (mW/mg)
94
4
TG (%)

92 60
3
Peak:820ºC
90
2 50

88
Mass Change:-9.60% 1
40
86 600 700 800 900 1000
0 Temperature (ºC)
200 400 600 800 1000 1200
Temperature (ºC) Fig. 6. Conversion percentage of the total nickel to metallic nickel as a function of
reduction temperature.
Fig. 4. Thermogram for nickel laterite ore.

function of the reduction temperature. The aNi generally increased

with increasing reduction temperature. A slight decrease in the con- 100
version percentage was observed at 850 °C, which can be attributed
to the phase transformation of lizardite–forsterite (Flavio, 1992). 90
Increasing the reduction temperature (>850 °C) was favourable for
the reduction reaction. Among conversion percentage at 800 °C,
Reduction rate (%)

80
The decreased conversion percentage at 900 °C may be attributed
to the presence of metallic iron and the formation of an Fe–Ni alloy
caused by the association of nickel with iron oxides. 70

4.2.2. Effect of reduction time 60

The reduction time had a strong influence on the conversion
percentage of the total nickel to metallic nickel, as shown in 50
Fig. 7. The conversion percentage increased with increasing reduc-
tion time, with an aNi of 36% after a reduction time of 10 min and
40
an aNi of 83% after a reduction time of 60 min. Gas–solid reactions 10 20 30 40 50 60
consist of three steps including external diffusion, internal diffu- Time (min)
sion and interfacial chemical reaction (Hua, 2004). A decrease in
the reduction time does not allow the reaction to proceed fully, Fig. 7. Conversion percentage of the total nickel to metallic nickel as a function of
resulting in a decrease in the conversion percentage of the total reduction time.
nickel to metallic nickel.

4.2.3. Effect of CO content
A mixed gas of CO and CO2 was selected as the gaseous reduc-
tant for this reduction process. As shown in Fig. 8, the conversion
percentage of the total nickel to metallic nickel increased rapidly
with increasing CO content, with a maximal aNi of 96%. In addition,
the conversion percentage reached 90% at a CO content of 30% and
then leveled off. This phenomenon was attributed to the fact that
increasing the CO content enlarges the chemical reaction interface,
thereby increasing the conversion percentage of the total nickel to
metallic nickel. In fact, to obtain a higher conversion percentage,
the CO content must be greater than its equilibrium concentration
in the reaction at a certain temperature.

Fig. 5. SEM image of nickel laterite ore. (a)1000 (b)2000.

1560 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562

100 90

90
80
Reduction rate (%)

Reduction rate (%)

80

70 70

60
60
50

40 50
10 20 30 40 50 1 2 3 4 5 6 7 8 9 10
CO content (%) Carbon content (%)

Fig. 8. Conversion percentage of the total nickel to metallic nickel as a function of Fig. 11. Conversion percentage of the total nickel to metallic nickel as a function of
CO content. carbon content.

90 90

80
Reduction rate (%)
Reduction rate (%)

70
85

60

50
80
40

30

20 75
500 600 700 800 900 1000 0 5 10 15 20 25
Temperature (ºC) CaO content (%)

Fig. 9. Conversion percentage of the total nickel to metallic nickel as a function of Fig. 12. Conversion percentage of the total nickel to metallic nickel as a function of
reduction temperature. CaO content.

90
1800
80 -Forsterite[Mg2(SiO4)]
1600
-Taenite[Fe,Ni]
1400
Reduction rate (%)

70
1200
Intensity (cps)

60
1000

50 800

600
40
400
30
200

20 40 60 80 100 120 0
Time (min) 10 20 30 40 50 60 70 80
2 Theta (º)
Fig. 10. Conversion percentage of the total nickel to metallic nickel as a function of
reduction time. Fig. 13. XRD pattern of reduced nickel laterite ore.
 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562
Fig. 14. SEM images of reduced nickel laterite ore. (a) 1000 (b) 5000.
4.3. The reduction of nickel from nickel laterite ore using a solid
reductant
4.3.1. Effect of reduction temperature
Fig. 9 shows the conversion percentage of the total nickel to
metallic nickel as a function of the reduction temperature. The
reduction temperature had an obvious influence on the conversion
percentage of the total nickel to metallic nickel, as the aNi
increased with an increase in the reduction temperature. The
lowest aNi was 27% at a temperature of 500 °C, and the highest
aNi was 84% at a temperature of 1000 °C. The activation of mineral
aggregates and the molecular motion of the reactive gas increased,
the reaction velocity increased and the reaction time decreased
with an increase in the reduction temperature. The study of
dynamics shows that the reactive mode is determined by the
reduction temperature, and the controlling steps at the initial, mid-
dle and later stages are chemical reaction-controlled, mixed-con-
trolled and diffusion-controlled, respectively (Li et al., 2009).
However, the decrease in the conversion percentage at 850 °C
was unexpected because of the solid–solid reaction, which was
not affected by the phase transformation, improving the conver-
sion percentage.
4.3.2. Effect of reduction time
The effect of the reaction time on the conversion percentage of
the total nickel to metallic nickel is shown in Fig. 10. The conver-
sion percentage increased with an increase in the reduction time
but decreased slowly as the time increased above 80 min. The
maximal aNi was approximately 80% when the reduction time
was 80 min. This peak in the conversion percentage may be attrib-
uted to the reductant being consumed gradually with an increasing
reduction time, the CO2 concentration increasing with an increase
in the reduction time, and the boundary of the gas–solid reaction
filling with CO2 gas, inhibiting the progress of the reduction
reaction.
4.3.3. Effect of carbon content
In this experiment, anthracite was selected as the solid reduc-
tant and was ground to increase the surface area and promote
contact with the ore. As shown in Fig. 11, the aNi increased rapidly
with an increase in the carbon content but did not change signifi-
cantly when the carbon content was increased beyond 3%. Because
the reduction of nickel from low-grade nickel laterite ore is indirect
(Shi et al., 2009), when the carbon content reached a certain
optimal value, an additional increase in the carbon content created
a large amount of residual carbon, which hindered the indirect
reduction.
4.3.4. Effect of CaO content
Fig. 12 shows the conversion percentage of the total nickel to
metallic nickel as a function of the CaO content. The aNi first
1561
increased and then decreased with increasing CaO content. The
maximal aNi was approximately 86% when the CaO content was
10%. Because part of the NiO combines with SiO2 to form olivine
in the phase transformation process, NiO was replaced by CaO from
the olivine due to the alkaline oxide effect (CaO +
2NiOSiO2 = CaOSiO2 + 2NiO). The use of CaO as an additive in so-
lid-state deoxidation improves the reduction reaction of NiO in
the nickel laterite ore by increasing its activity. However, when
the CaO content was excessive, the solid-state reaction was hin-
dered, and the effective specific surface area for the reduction reac-
tion of nickel laterite ore with anthracite decreased.
4.4. Characterisation of reduced nickel laterite ore
4.4.1. Phase composition of reduced nickel laterite ore
The XRD pattern of the reduced nickel laterite ore is shown in
Fig. 13. The diffraction peaks of the product match with the stan-
dard diffraction peaks of forsterite and taenite. The key feature of
this result is the transformation of magnesium hydrosilicate to
the forsterite phase in the reduced nickel laterite ore. Taenite [Fe,
Ni] is a newly formed material that appeared in the reduction
product. Simple nickel was not discovered because the metallic
nickel concentration is below the detection limit and part of the
metallic nickel combines with iron, which is reduced by the so-
lid-state deoxidisation method to form a new mineral phase
(Swamy et al., 2003; Chang et al., 2008).
4.4.2. Morphology analysis of reduced nickel laterite ore
The SEM images of reduced nickel laterite ore are shown in
Fig. 14. The surface morphology of the reduced ore has changed
relative to the raw ore (Fig. 5). Large granular and sandwich struc-
tures were clearly seen before the reduction process, but small
granular and flocculent structures were observed after the reduc-
tion. The results show that the specific surface area increased
and the the size of particles decreased, both of which were benefi-
cial to the reduction of nickel from low-grade nickel laterite ore.
5. Conclusions
In this study, the nickel extraction from low-grade nickel later-
ite ore was performed using a solid-state deoxidisation method. It
was shown that an aNi of greater than 90% could be obtained from
nickel laterite ore using a CO and CO2 mixture as a gaseous reduc-
tant, and an aNi of up to 80% could be obtained from nickel laterite
ore using anthracite as a solid reductant.
The effects of the reduction temperature, reduction time and CO
content on the conversion percentage using a gaseous reductant
were investigated. The results showed that the conversion percent-
age of the total nickel to metallic nickel increased with increasing
reaction temperature and time initially, and then remained steady
with further increases, but decreased abruptly at a temperature of
1562 B. Li et al. / Minerals Engineering 24 (2011) 1556–1562
850 °C. As CO is the active species in the reductant, a satisfactory
aNi can be achieved when the CO content in the gaseous mixture
is greater than 30%. In the solid–solid reduction process, similar
influences of temperature and anthracite content on the reduction
rate were observed. A reaction time of 80 min and a CaO content of
10% corresponded to the maximal aNi.
During the reduction process, taenite [Fe, Ni] was formed,
which promoted nickel recovery from nickel laterite ore. The sur-
face morphology of nickel laterite ore was also improved by the
reduction process.
Acknowledgement
The project was sponsored by the National Natural Science
Foundation of China (No. 50906035).
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