TY - JOUR
T1 - Novel route to synthesize complex metal sulfides
T2 - Hydrothermal coupled dissolution-reprecipitation replacement reactions
AU - Xia, Fang
AU - Zhou, Jinwen
AU - Brugger, Joël
AU - Ngothai, Yung
AU - O'Neill, Brian
AU - Chen, Guorong
AU - Pring, Allan
PY - 2008/4/22
Y1 - 2008/4/22
N2 -
A novel route for the synthesis of complex metal sulfides using hydrothermal coupled dissolution-reprecipitation reactions is reported. Two thiospinels, (Ni,Fe)
3
S
4
(violarite) and Co
3
S
4
(linnaeite), were synthesized using (Fe,Ni)
9
S
8
(pentlandite) and Co
9
S
8
(cobaltpentlandite) as precursors. The Fe/Ni ratio of (Ni,Fe)
3
S
4
can be adjusted by varying the reaction conditions, for example, temperature (125-145 °C), pH (2.90, 3.90, 5.00), and precursor stoichiometry ((Fe
x
Ni
1-x
)
9
S
8
, x = 0.4, 0.5, 0.55, 0.6). Pure (Ni,Fe)
3
S
4
can be synthesized by utilizing a flow-through hydrothermal cell rather than a static hydrothermal cell as the fluid flow improves mass transfer and flushes away the Fe
2
O
3
byproduct from the reaction front. Synthesis times range from 10 to 20 days, compared to the traditional dry synthesis route for (Ni,Fe)
3
S
4
that requires 3 months annealing to obtain a product of only 72 ± 3 wt % purity. This synthesis route is ideal for preparing compounds with low thermal stabilities (<500°C).
AB -
A novel route for the synthesis of complex metal sulfides using hydrothermal coupled dissolution-reprecipitation reactions is reported. Two thiospinels, (Ni,Fe)
3
S
4
(violarite) and Co
3
S
4
(linnaeite), were synthesized using (Fe,Ni)
9
S
8
(pentlandite) and Co
9
S
8
(cobaltpentlandite) as precursors. The Fe/Ni ratio of (Ni,Fe)
3
S
4
can be adjusted by varying the reaction conditions, for example, temperature (125-145 °C), pH (2.90, 3.90, 5.00), and precursor stoichiometry ((Fe
x
Ni
1-x
)
9
S
8
, x = 0.4, 0.5, 0.55, 0.6). Pure (Ni,Fe)
3
S
4
can be synthesized by utilizing a flow-through hydrothermal cell rather than a static hydrothermal cell as the fluid flow improves mass transfer and flushes away the Fe
2
O
3
byproduct from the reaction front. Synthesis times range from 10 to 20 days, compared to the traditional dry synthesis route for (Ni,Fe)
3
S
4
that requires 3 months annealing to obtain a product of only 72 ± 3 wt % purity. This synthesis route is ideal for preparing compounds with low thermal stabilities (<500°C).
UR - https://www.scopus.com/pages/publications/43249091107
U2 - 10.1021/cm7033883
DO - 10.1021/cm7033883
M3 - Article
AN - SCOPUS:43249091107
SN - 0897-4756
VL - 20
SP - 2809
EP - 2817
JO - Chemistry of Materials
JF - Chemistry of Materials
IS - 8
ER -