Transition metal-pyrophosphate negative electrode active material, preparation method thereof, and lithium secondary battery or hybrid capacitor containing it
A technology of transition metals and pyrophosphates, which is applied in the manufacture of active material electrodes, hybrid capacitor electrodes, hybrid/electric double layer capacitors, etc., to achieve the effects of improving capacity characteristics, low average voltage, and increasing voltage
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[0062] The present invention provides the preparation method of the transition metal-pyrophosphate of the above chemical formula 1, comprising: step (i), obtaining a precursor comprising a transition metal compound and phosphate; and step (ii), for the above step (i) The obtained precursor is subjected to heat treatment.
[0063] Specifically, the method for preparing a transition metal-pyrophosphate according to an embodiment of the present invention may include a step of obtaining a precursor comprising a transition metal compound and a phosphate (step (i)).
[0064] The above-mentioned transition metal-containing compound and phosphate can be obtained as a precursor by mixing according to the stoichiometric equivalent. At this time, in order to mix the above-mentioned compounds as well as possible, it is preferable to obtain a homogeneously mixed precursor by a normal grinding method such as a planetary ball mill.
[0065] According to an embodiment of the present inventio...
Embodiment 1
[0109] Example 1: Mn 2 P 2 o 7 preparation of
[0110] mn 2 P 2 o 7 The synthesis of is carried out according to a common solid-phase reaction method in which precursors are mixed in a manner corresponding to the chemical equivalent and heat-treated.
[0111] MnO 2 and NH 4 h 2 PO 4 After quantifying at an equivalent of 2:1, a planetary ball mill was used to mix the above-mentioned substances as well as possible. After adding alumina balls and ethanol as a dispersion medium, grinding was performed at a speed of 350 rpm for one hour to obtain a precursor in which the raw materials were uniformly mixed.
[0112] The above precursor was heat-treated in air at 700°C for 12 hours to obtain Mn 2 P 2 o 7 .
Embodiment 2
[0113] Embodiment 2: Preparation is coated with the Mn of carbon layer 2 P 2 o 7
[0114] The Mn prepared in the above example 1 2 P 2 o 7 After being dispersed in sucrose solution and heated by microwave, the Mn 2 P 2 o 7 A carbon coating is formed on it.
[0115] Specifically, with Mn(PO 3 ) 2 Gross weight is a basis, after preparing the sucrose solution of about 60 weight percent, make above-mentioned Mn(PO 3 ) 2 Disperse in the prepared sucrose solution and stir for more than 30 minutes. Hydrolysis by means of microwave heat treatment was then carried out at a temperature of 200°C. The heat treatment described above was performed in argon as an inert atmosphere. Mn coated with a carbon layer by the hydrolysis described above using water and ethanol 2 P 2 o 7 After several washes, carbon-coated Mn was obtained by drying 2 P 2 o 7 .
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