Hydrotalcite precursor technique nitrogen-sulfur co-doped carbon loaded transition metal sulfide solid solution, preparation method and application thereof
A nitrogen-sulfur co-doping, transition metal technology, applied in molybdenum sulfide, electrochemical generators, structural parts, etc., can solve the problems of reducing active material metal sulfide, difficult mass production, reducing specific capacity, etc., to achieve cycle The effect of good stability, low cost and high discharge capacity
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Embodiment 1
[0036] 1) 0.03mol Co(NO 3 ) 2 ·6H 2 O, 0.009mol Fe(NO 3 ) 3 9H 2 O,0.001mol Al(NO 3 ) 3 9H 2 O, add 80ml of deionized water after mixing, and ultrasonically dissolve for 20min. Then weigh 0.02mol Na 2 CO 3 and 0.064mol NaOH, after mixing, add 80ml of deionized water, ultrasonic 20min to fully dissolve. In the colloid mill reactor, the fully dissolved salt solution and the alkali solution were quickly mixed evenly, the rotation speed was 70r / min, and the reaction time was 3min. After the reaction, transfer the obtained slurry to a polytetrafluoroethylene reactor, and crystallize at 120°C for 24 hours. After the heating is completed, take out the polytetrafluoroethylene reactor and cool it to room temperature naturally. Wash with deionized water and ethanol several times, centrifuge, and then dry at 60°C for 24 hours to obtain cobalt-iron-aluminum hydrotalcite.
[0037] 2) Grind the cobalt-iron-aluminum hydrotalcite obtained in step 1) and AY49 at a mass ratio of 1:5...
Embodiment 2
[0042] 1) The preparation of cobalt-iron-aluminum hydrotalcite is the same as in Example 1, except that the divalent cobalt salt is CoSO 4 .7H 2 O, the ferric salt is FeCl 3 .
[0043] 2) Grind the cobalt-iron-aluminum hydrotalcite obtained in step 1) and AY25 at a mass ratio of 1:5 to make them evenly mixed, place them in a high-temperature atmosphere furnace, and pass in N 2 Gas, the flow rate is 50mL / min. Raise the temperature in the furnace to 800°C with a heating rate of 2°C / min, keep it for 200min, and then naturally cool to room temperature to obtain a black powder.
[0044] 3) The black powder was acid-washed with 0.9 mol / L hydrochloric acid at 80°C for 12 hours to obtain a nitrogen-sulfur co-doped carbon-supported composition (Co 0.85 Fe 0.15 ) 9 S 8 sulfides, denoted as (Co 0.85 Fe 0.15 ) 9 S 8 / NSC. The battery test results are summarized in Table 1.
Embodiment 3
[0046] 1) The preparation of cobalt-iron-aluminum hydrotalcite is the same as in Example 2, except that the ferric salt is Fe 2 (SO 4 ) 3 , the trivalent aluminum salt is Al 2 (SO 4 ) 3 .
[0047] 2) Grind the cobalt-iron-aluminum hydrotalcite obtained in step 1) and AY23 at a mass ratio of 1:3 to make them evenly mixed, place them in a high-temperature atmosphere furnace, and inject Ar gas at a flow rate of 50mL / min. Raise the temperature in the furnace to 700°C with a heating rate of 2°C / min, keep it for 300min, and then naturally cool to room temperature to obtain a black powder.
[0048] 3) The black powder was acid-washed with 2.0 mol / L acetic acid at 80°C for 6 hours to obtain a nitrogen-sulfur co-doped carbon-supported composition (Co 0.83 Fe 0.17 ) 9 S 8 Sulfide, denoted as (Co 0.83 Fe 0.17 ) 9 S 8 / NSC. The battery test results are summarized in Table 1.
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