Vacuum 188 (2021) 110166

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Vacuum
journal homepage: http://www.elsevier.com/locate/vacuum

Removal of arsenic from dusts produced during the pyrometallurgical

refining of copper by vacuum carbothermal reduction
Cong Li, Rong-Liang Zhang *, Jia Zeng, Qin-Yao Lu, Chao-Fan Tang, Lin-Kai Zhou, Wei Zhang,
Hong-Ru Zhang, Yan-Yan Gao, Jia-Feng Chen, Jin-Tao Cao
School of Metallurgical and Materials Engineering, Jiangsu University of Science and Technology, Jiangsu, Zhangjiagang, 215600, China

A R T I C L E I N F O A B S T R A C T

Keywords: Removal of arsenic using the low-temperature vacuum carbothermal reduction method was investigated by
Pyrometallurgical refining furnace taking dusts with high contents of arsenic and copper from furnaces for pyrometallurgical refining of Cu as raw
Dusts with high contents of arsenic and copper materials. Based on TGA-DSC, differential thermal analysis was applied to the raw materials; by virtue of various
Vacuum carbothermal reduction
methods including XRD, ICP, and SEM: the phases, chemical compositions and morphologies of dusts and
Arsenic removal
evaporation residues were separately analysed; on the basis of thermodynamic analysis, the influences of the
evaporating temperature, residual pressure, reductant dosage, and evaporation time on the removal rates of As
and other valuable metals were explored. The results show that at an evaporating temperature of 350 ◦ C, the
residual pressure of 100 Pa, reductant dosage of 25%, and evaporation time for 50 min, the As removal rate can
reach 93.48% while guaranteeing that the other metals are essentially not evaporated. This realises the selective
separation of As from the other valuable metals. The evaporation products are higher-purity As2O3, which can be
used as a primary As2O3 product. The valuable metals are concentrated in evaporation residues, being conducive
to subsequent recovery by leaching with waste acids.

1. Introduction pollution [5]. Hydrometallurgy aims to transfer the solid-phase target

Fuel combustion and the effect of gas and physical and chemical
reactions (e. g. volatilisation and oxidation) of metals on carrying ma­
terials at high temperature usually occur in the pyrometallurgical
refining of copper [1]. Under the effects thereof, dusts rich in various
volatile elements (such as Cu, Pb, Zn, In, Bi, Sb, Sn, and As) and their
compounds are generated, which are potentially valuable resources [2,
3]. Without their recovery, the dusts can not only induce severe envi­
ronmental pollution but also lead to a significant waste of resources. At
present, the processing methods for dusts from furnaces for pyrometal­
lurgical refining of Cu mainly include pyrometallurgy, hydrometallurgy,
and combinations thereof. Pyrometallurgy-based As removal processes
generally involve volatilisation roasting, reduction roasting, and melting
methods [4]. Among them, the pyrometallurgy-based As removal pro­
cess has developed to become the most mature; however, there are many
disadvantages, including the production of many intermediates, much
pollution, a low As removal rate, high energy consumption, impure
As2O3 due to metal loss; low As recovery rate, low As2O3 concentration
in dusts; generation of secondary dusts and significant environmental
elements into the leaching solution after leaching the target elements
with a suitable leachant. According to the type of leachant, hot-water
leaching, acid leaching, alkaline leaching, and bioleaching are used
[6,7], however, with the hydrometallurgy process, there are long,
tedious procedures required; the leaching solution contains high acid
and alkaline contents and is therefore highly corrosive, thus having high
requirements on the durability of equipment; the products are crude or
enriched, some of which need further processing [8]. In terms of the
combination of pyrometallurgy and hydrometallurgy, after performing
the oxidising roasting by adding the soda ash and caustic soda, the
roasted residues are leached with hot water; afterwards, the sodium
arsenates in filtrates are cooled and crystallised so as to recycle the As, or
various reagents (such as calcium salts and ferric salts) are added to the
filtrate to remove the As [9,10]. Nevertheless, the process presents the
following drawbacks: high consumption of materials, high production
cost, restriction on the application of As products, or generation of more
hazardous wastes containing As residues [11].
Aiming at the current status of techniques available for processing
dusts from furnaces for pyrometallurgical refining of Cu, a novel

* Corresponding author.
E-mail address: zhangrljx19201@163.com (R.-L. Zhang).

https://doi.org/10.1016/j.vacuum.2021.110166
Received 31 January 2021; Received in revised form 22 February 2021; Accepted 23 February 2021
Available online 27 February 2021
0042-207X/© 2021 Elsevier Ltd. All rights reserved.
C. Li et al.
technique for removing As using low-temperature vacuum carbothermal
reduction and leaching evaporation residues with waste acids was pro­
posed to process dusts with high As and Cu contents from the furnaces
for pyrometallurgical refining of Cu. As for the As removal process based
on vacuum carbothermal reduction, the As is removed by taking carbon
as the reductant at a low temperature and recycled as the primary As2O3
products, however, other valuable metals are not evaporated and remain
abundant in evaporation residues. The whole process of removing As
based on low-temperature vacuum carbothermal reduction was con­
ducted in a closed vacuum system, showing a friendly operating envi­
ronment. Only the process of removing As with the low-temperature
vacuum carbothermal reduction was introduced.
2. Tests
2.1. Raw materials
The dusts from furnaces for pyrometallurgical refining of Cu in
Zhangjiagang United Copper Co., Ltd, Jiangsu Province, China were
used as the raw materials during the tests. The main chemical compo­
sitions and phase analysis of dusts from the furnaces for pyrometallur­
gical refining of Cu are shown in Table 1 and Fig. 1: the As content was as
high as 14.41% while the Cu content reached 19.8% in these dust
specimens. Other valuable metals were also present in large amounts:
the contents of Pb and Zn were 9.50% and 8.84%, respectively, showing
high potential recycling value; the contents of K, Fe, and Ca were quite
low. The raw materials mainly contained fourteen elements (Cu, As, Zn,
Pb, S, Sn, Sb, Se, K, Fe, Ca, Ni, Zr, and Cr), accounting for 58.96% (mass
fraction) of raw materials. The As in dusts mainly appears as As2O3 and
As2O5 phases in the mass ratio of 1.935:1, while Cu appears as CuO,
Cu2O and Cu(NH4)2(SO4); moreover, Pb is mainly present as Pb2OSO4
and PbSO4 phases while Zn appears as ZnSO4.
2.2. Test instruments and equipment
The test instruments and equipment include an SK-2-10 tubular
resistance furnace, a 2XZ-I rotary vane vacuum pump, a DP-AF (vac­
uum) precision digital pressure gauge, a TCE-II intelligent temperature
controller, a condenser chamber depending on air cooling and a vacuum
chamber functioning through electrical heating (self-made, temperature
control by thermocouples).
2.3. Test methods
A certain amount of dusts could be placed in a porcelain boat. After
the vacuum chamber was heated to a certain temperature, the porcelain
boat was placed into the vacuum chamber. The vacuum chamber was
vacuumised and we began to calculate the evaporation time. After
evaporation and cooling, the evaporation products and evaporation
residues were separately removed from the condenser chamber and the
vacuum chamber and then weighed and sampled; moreover, the con­
tents of various elements in evaporation products and evaporation res­
idues were measured by the EDTA volumetric methods and applying an
ICAP-7000 inductively coupled plasma (ICP) emission spectrometer
respectively. Subsequently, the removal rates η of various elements are
calculated according to the following equation:
m1 − m2
η= × 100%
m1
Table 1
Composition analysis (mass fraction (%)) of dusts with high As and Cu contents from furnaces for pyrometallurgical refining of Cu.
compositions Cu As Zn Pb S Sn
Contents 19.80 14.41 8.84 9.50 2.28 1.22
2
Vacuum 188 (2021) 110166
where, m1 and m2 refer to the masses of various elements in dusts before
evaporation and those in residues after evaporation, respectively.
The morphologies and particle sizes of the evaporation products and
evaporation residues were separately observed and measured by utilis­
ing the JSM-6510LA scanning electron microscope; the XRD-6000 X-ray
diffractometer was used to conduct phase analysis of evaporation
products and evaporation residues.
3. Thermodynamic analysis and basic principle for separating
As2O3 from others
3.1. Thermodynamic analysis
According to the compositional characteristics of dusts containing As
and Cu, thermodynamic analysis was applied to the vacuum carbo­
thermal reduction process by referring to the manual for thermology
[12–14]. The possible reactions in the reduction process are listed in
Table 2.
The results of thermodynamic analysis (see Fig. 2) show that the
Gibbs free energies in reaction equations 3.0, 3.14, and 3.16 are mini­
mised at the same reaction temperature. This indicates that, as the
temperature rises, As2O5 in raw materials will react with carbon to
generate As2O3 before decomposition, thus finally generating elemen­
tary As. In Equation 3.1, the Gibbs free energy at about 700 ◦ C is
negative, which implies that CO cannot be generated; furthermore, the
indirect reduction cannot occur until the temperature exceeds 700 ◦ C. At
the same temperature, the Gibbs free energies in Equations 3.9 and 3.10
are more negative than those in Equations 3.2 and 3.3. This indicates
that ZnSO4 and PbSO4 separately react with CO to generate zinc sul­
phide and lead sulphide before their decomposition. The Gibbs free
energies in Equations 3.7 and 3.8 are negative once the reaction tem­
perature exceeds 300 ◦ C. This shows that As2O5 in dusts containing As
and Cu possibly reacts with carbon at a low temperature, triggering their
direct reduction to generate As2O3. It can be obtained from the figure
that, in terms of experiencing the carbothermal reaction, the order of
priority of the main phases in dusts specimens containing As and Cu is as
follows: As2O5, As2O3, PbSO4, and ZnSO4.
3.2. Basic principle for separating As2O3 from others
The difference in vapor pressure of each substance in the dusts at a
temperature is the basic principle for separating As2O3 from others, such
as PbO, ZnO and CuO.
The components in the dusts include mainly As2O3, PbO, ZnO and
CuO. Relationships between saturation vapor pressure of As2O3, PbO
and ZnO, and temperature are expressed as follows [15]:
/
lgPθAi2 O3 = 4.993 − 1001.425 (T + 6.990), T = − 139.3̃194.15 ◦ C (1)
/
lgPθPbO = 9.331 − 11048.802 (T + 240.480), T = 451̃1198 ◦ C (2)
/
lgPθZnO = 9.980 − 15781.354 (T + 273.150), T = 1226.95̃1676.95 ◦ C (3)
The saturation vapor pressure values of As2O3, PbO and ZnO were
calculated at 200–750 ◦ C according to Eqs. (1)–(3). It can be seen that
the differences in the saturation vapor pressure values of As2O3, PbO and
ZnO in the dusts are obvious. At 200–750 ◦ C, the saturation vapor
pressure values of As2O3 are 336630.57–1394682.36 Pa, while PbO and
ZnO evaporate little because their saturation vapor pressure values are
less than 513 Pa and 0.9 Pa respectively. The value of PθAs2 O3 /PθPbO is more
Sb Se K Fe Ca Ni Zr Cr
0.94 0.77 0.42 0.32 0.04 0.040 0.040 0.34
C. Li et al. Vacuum 188 (2021) 110166

Fig. 1. XRD analysis of dusts with high As and Cu contents from furnaces for pyrometallurgical refining of Cu.

analyser (Mettler Toledo, Switzerland). In a protective nitrogen atmo­

Table 2
sphere, the heating rate is 10 ◦ C/min. The result of differential thermal
Possible reactions in the reduction process.
analysis is shown in Fig. 3.
Type of reaction Reaction equation Number As shown in Fig. 3, between 274 and 425 ◦ C, the mass of material
the direct reduction C + O2(g) = CO2(g) 3.0 decreases. There is an endothermic peak between 278 and 413 ◦ C,
C + CO2(g) = 2CO(g) 3.1 occurring at 357 ◦ C. Moreover, this is within the range in which As2O3
1/4ZnSO4+C– 3.2
–CO(g)+1/4ZnS
volatilises. Between 20 and 278 ◦ C, the thermo-gravimetric and differ­
1/4PbSO4+C– –CO(g)+1/4PbS 3.3
CuO + C––CO(g)+Cu(s) 3.4
ential thermal curves are shallow and only a slight chemical reaction
2CuO + C– –CO(g)+ Cu2O(s) 3.5 occurs.
Cu2O + C––CO(g)+2Cu(s) 3.6
As2O5+2C– –As2O3(g)+2CO 3.7 4.2. Influences of different conditions on the As removal rate
As2O3+3C = 2As(s.g)+3CO 3.8
the indirect reduction 1/4PbSO4+CO(g) = CO2(g)+1/4PbS 3.9
1/4ZnSO4+CO(g) = CO2(g)+1/4 ZnS 3.10 The factors influencing the As removal rate and the purity of As2O3
CuO + CO(g) = CO2(g)+Cu(s) 3.11 mainly include the evaporating temperature, residual pressure (that is,
Cu2O + CO(g) = CO2(g)+2Cu(s) 3.12 the pressure in the system), evaporation time, and reductant dosage.
As2O3(s.g)+3CO = 2As+3CO2(g) 3.13
As2O5+2CO(g) = As2O3(s.g)+2CO2 3.14
other reactions 4As(s) = As4(g) 3.15
4.2.1. The influence of the evaporating temperature on the As removal rate
4As(g) = As4(g) 3.16 Under a residual pressure of 100 Pa, over an evaporation time of 50
As2O5––As2O3(s.g)+O2 3.17 min with a reductant dosage of 25%, the influence of the evaporating
2ZnSO4––O2+2ZnO+2SO2(g) 3.18 temperature on the As removal rate was analysed. The result is displayed
2PbSO4––O2+2PbO+2SO2(g) 3.19
in Fig. 4.
As shown in the figure, the evaporating temperature greatly in­
than 2720.20 Pa, while PθAs2 O3 /PθZnO is larger at the temperature range. fluences the As removal rate. As the temperature rises from 250 ◦ C to
The saturation vapor pressure of CuO is very low. For example, the 350 ◦ C, the As removal rate increases from 73.9% to 91.98%. The reason
saturation vapor pressure of CuO is less than 1 Pa at 1350 ◦ C [15]. why the As removal rate increases significantly is that the evaporation
Therefore, As2O3 with high vapor pressure evaporates into gas phase, rate of As2O3 increases with the increase of the temperature. At tem­
while PbO, ZnO and CuO with low vapor pressures remain in residual peratures between 350 ◦ C and 700 ◦ C, the As removal rate decreases
liquid or residue. (from 91.98% to 51.74%) with increasing temperature. The reason for
It is easy to separate As2O3 from others under vacuum condition. this is that the As2O3 in dusts is transformed into arsenates with a low
Since the evaporation rate of substance at a pressure in vacuum is much vapor pressure with increasing temperature. In this condition, it is
higher than that at a normal pressure at the same temperature, and the difficult for As to be evaporated, thus leading to the reduction of the As
evaporation temperature required at a pressure in vacuum is much removal rate. Nevertheless, the removal rates of the other metals in­
lower than that at a normal pressure at the same evaporation rate [16]. crease within the temperature range during the test owing to the oxides
of the metals having a lower vapor pressure. The removal rates of Cu, Pb,
4. Results and discussion and Zn increase from 0.51%, 0.46%, and 0.25%–6.58%, 6.93%, and
6.93%, respectively. Therefore, it is feasible to realise the effective
4.1. Differential thermal analysis of raw materials separation of As from the other valuable metals. Through the test, the
suitable evaporating temperature is determined to be 350 ◦ C.
Differential thermal analysis was applied to raw materials in dusts
containing As and Cu by using the TGA-DSC1 thermogravimetric

3
C. Li et al.
Fig. 2. The relationship between the Gibbs free energy and temperature during possible reactions in the reduction process.
4.2.2. The influence of the residual pressure on the As removal rate
At an evaporating temperature at 350 ◦ C, over an evaporation time of
50 min with a reductant dosage of 25%, the influence of the residual
pressure on the As removal rate was explored. The result is displayed in
Fig. 5.
As2O3 belongs to the evaporable matters. When the residual pressure
of the system is lower than 1 atm, that is, a vacuum is applied, the As
removal rate increases remarkably. Under residual pressures from 50 to
500 Pa, the As removal rate increases with the reduction of the residual
pressure from 500 to 100 Pa. The As removal rate reaches 68.6% at a
residual pressure of 500 Pa while it increases to 93.63% as the residual
pressure decreases to 100 Pa; at a residual pressure of between 50 and
100 Pa, the As removal rate changes little with changes in residual
pressure. The reason for this is that the residual pressure does not
significantly affect the rate of evaporation below a certain value: how­
ever, when the residual pressure is lowered from 500 to 50 Pa, the
4
Vacuum 188 (2021) 110166
removal rates of Cu, Pb, and Zn increase from 0.67%, 0.48%, and
0.74%–2.78%, 5.59%, and 2.71%, respectively. This reveals that the
reduction of the residual pressure will exert a certain influence on the
removal rates of Pb, Cu, and Zn. According to the test result, the optimal
residual pressure is 100 Pa.
4.2.3. The influence of the evaporation time on the As removal rate
The influence of the evaporation time on the As removal rate was
investigated at an evaporating temperature of 350 ◦ C, under a residual
pressure of 100 Pa with a reductant dosage of 25%. The result is shown
in Fig. 6.
The loner the evaporation time, the higher the As removal rate
within the time range set in the test; if the evaporation lasts for 30 min,
the As removal rate is 80.22% and it increases to 93.59% when the
evaporation time is increased to 50 min; in addition, the As removal rate
starts to decrease slowly when the evaporation time exceeds 50 min.
C. Li et al.
Fig. 3. Differential thermal analysis: dusts containing As and Cu.
Fig. 4. The influence of the evaporating temperature on the removal rate.
Fig. 5. The influence of the residual pressure on the removal rate.
When the evaporation time is increased from 30 to 90 min, the removal
rates of Cu, Pb, and Zn increase from 0.16%, 0.35%, and 0.84%–4.01%,
3.27%, and 4.18%. This indicates that a longer evaporation time will
influence the removal rates of Pb, Cu, and Zn to some extent. According
to the test result, the evaporation time should be set to 50 min.
5
Vacuum 188 (2021) 110166
Fig. 6. The influence of the evaporation time on the removal rate.
4.2.4. The influence of the reductant dosage on the As removal rate
Under conditions involving evaporation at 350 ◦ C for 50 min under a
residual pressure of 100 Pa, the influence of the reductant dosage on the
As removal rate was surveyed. The result is displayed in Fig. 7.
As the reductant dosageis varied in the range from 5% to 25%, the
larger the reductant dosage, the higher the As removal rate; at the
reductant dosage of 5%, the As removal rate is 75.39% and it rises to
93.51% when the reductant dosage grows to 25%; moreover, the As
removal rate begins to decrease slowly when the reductant dosage ex­
ceeds 25%. The possible reason is that the growth of the reductant
dosage is conducive to decomposition of zinc sulphate and lead sulphate
into the zinc oxide and lead oxide, respectively. In this context, the
arsenic trioxides in the dust specimens are transformed into arsenates
with a low vapor pressure, such that the As is hard to evaporate, thus
resulting in the decrease of the As removal rate. With the growth of the
reductant dosage from 5% to 50%, the removal rates of Cu, Pb, and Zn
increase from 0.71%, 0.3%, and 0.35%–5.1%, 3.57%, and 4.71%,
respectively. The increase of the reductant dosage contributes to the
growth of the removal rates of Pb, Cu, and Zn. The optimal reductant
dosageis 25% based on the test result.
4.3. Analysis of evaporation products
Based on above analysis on influences of various factors on the As
removal rate and the purity of As2O3 in evaporation products, the
optimised technological conditions were found to be as follows: evap­
oration at 350 ◦ C under a residual pressure of 100 Pa for 50 min with a
Fig. 7. The influence of the reductant dosageW on the removal rate.
C. Li et al. Vacuum 188 (2021) 110166

reductant dosage of 25%. When conducting tests under these conditions,

the As removal rate could reach 93.48%. The evaporation residues were
sampled, and their characteristics were analysed.

4.3.1. XRD analysis

Fig. 8 shows the result of X-ray diffraction (XRD) analysis on the
samples of evaporation products. By comparing the standard cards by
American Society for Testing and Materials (ASTM), the positions and
intensities of various main diffraction peaks of the samples are consis­
tent with those of the cubic crystal As2O3. This indicates that the samples
of As2O3 contained cubic crystals. As shown in the figure, the X-ray
diffraction peaks are sharp, indicative of the crystal perfection of As2O3.
There are smaller number of other impurity peaks at the diffraction
peaks, and the As2O3 shows higher purity. The result of XRD analysis of
evaporation residues is displayed in Fig. 9: the majority of the metallic
As has been removed and a small portion of the As appears as arsenates.
The other valuable metals exist in the form of composite salts.
Fig. 8. The XRD pattern of As2O3.

4.3.2. SEM and EDTA analyses

Fig. 10 shows the SEM image of the As2O3 evaporation product: the
distribution range of the particle size and shapes of the As2O3 shows that
the particle size of samples of As2O3 evaporation product consisting of
octahedral cubic crystals is in the range between 1 and 2.5 μm, with a
mean average crystal size of about 2 μm. The result (Fig. 11) of energy
disperse spectroscopy (EDS) reveals that the evaporation products only
contain elements As and O. According to the results (Table 3) of EDTA
and EDS analysis, it is found that the mass fraction of As in evaporation
products of As2O3 is 72.78%, while O is 23.29%, while that in the pure
As2O3 reaches 75.74%. The purity of the evaporation products As2O3 is
converted to 96.01%, that is, the evaporation products are high-purity
As2O3, which can be used as primary As2O3 products. The evaporation
residues contain elements As (1.24%), Cu (24.23%), Pb (11.67%), and
Zn (10.92%); evaporation residues are rich in valuable metals, which is
conducive to their subsequent recovery by using leaching with waste
acids.

5. Conclusions
Fig. 9. The XRD pattern of residues.
(1) The evaporating temperature, residual pressure, evaporation
time, and reductant dosage all influence the As removal rate to
some extent. The evaporating temperature shows quite a signif­
icant influence on the As removal rate: as the temperature rises
from 250 ◦ C to 350 ◦ C, the As removal rate constantly increases
while it declines with further increases in temperature from
350 ◦ C to 700 ◦ C. The As removal rate increases greatly with the
reduction of the residual pressure. As the evaporation continues,
the As removal rate rises at first and then declines. When the
reductant dosageis increased from 5% to 25%, the As removal
rate gradually increases while it starts to decrease slowly on the
condition that the reductant dosage exceeds 25%. Within ranges
of the conditions assessed during these tests, the other valuable
metals (including Cu, Pb, and Zn) exhibit an extremely low rate of
evaporation owing to their oxides having a low vapor pressure,
therefore, the rates of removal of these valuable metals are low,
thus realising the effective separation of As from the other valu­
able metals.
(2) Under the optimised technological conditions, that is, evapora­
tion at 350 ◦ C for 50 min under a residual pressure of 100 Pa with Fig. 10. SEM image of As2O3.
a reductant dosage of 25%, the As removal rate can reach 93.48%
while guaranteeing minimal evaporation of oxides of other abundant in evaporation residues, which is conducive to their
valuable metals. subsequent recovery based on leaching with waste acids.
(3) Under the optimised technological conditions selected during the
tests, the samples of evaporation product (As2O3) appear as cubic Declaration of competing interest
crystals, showing a higher purity; these can be used as primary
As2O3 products. The valuable metals (such as Cu, Pb, and Zn) are The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence

6
C. Li et al. Vacuum 188 (2021) 110166

Fig. 11. EDS image of As2O3.

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