CN109950525A - A kind of Nb of mao of tripe shape2O5The preparation method of lithium ion battery electrode material - Google Patents
A kind of Nb of mao of tripe shape2O5The preparation method of lithium ion battery electrode material Download PDFInfo
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- CN109950525A CN109950525A CN201910283694.7A CN201910283694A CN109950525A CN 109950525 A CN109950525 A CN 109950525A CN 201910283694 A CN201910283694 A CN 201910283694A CN 109950525 A CN109950525 A CN 109950525A
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Abstract
A kind of Nb of mao of tripe shape2O5Analytically pure oxalic acid hydrate niobium is added in distilled water obtains A first by the preparation method of lithium ion battery electrode material;Then glucose is added in distilled water and obtains B;A and B are mixed into obtain mixed liquor C;Mixed liquor C is cooled to room temperature after hydro-thermal reaction to obtain precipitating in homogeneous reaction instrument;Resulting sediment is dried to obtain predecessor D in a vacuum drying oven;It takes predecessor D to be added in distilled water and obtains solution E;It takes melamine to be added in oleic acid again and obtains solution F;Solution E and solution F are mixed and precipitated after carrying out secondary water thermal response cooled to room temperature;By resulting sediment be freeze-dried hair tripe shape Nb2O5Lithium ion battery electrode material.The method that the present invention uses secondary hydro-thermal, prepares the hair tripe shape Nb that crystallinity is preferable, is evenly distributed2O5Nano material, can be in favor of regulating and controlling the structure and pattern of material prepared, simple process and low cost as carbon source and surfactant using different oleic acid additive amounts.
Description
Technical field
The invention belongs to battery material technical fields, are related to a kind of preparation method for preparing lithium ion battery negative material,
More particularly to the Nb of a kind of mao of tripe shape2O5The preparation method of lithium ion battery electrode material.
Background technique
Due to the development and progress of science and technology, there is crisis in the non-renewable energy such as coal, oil and natural gas, tap a new source of energy by
Concern.Lithium ion battery is as the device for realizing electric energy and the mutual inversion of phases of chemical energy, with consumer electronic product quality and quantity
Raising, as a kind of clean energy resource, by large-scale application in the modern life.
Currently, developing many transition metal oxides in the market as lithium ion battery electrode material, they are most of
Alloying reaction and conversion reaction occurs, along with very big volume expansion, and Nb2O5As one of transition metal oxide, it
Intercalation [Augustyn V, Come J, Lowe M, et al.High-rate electrochemical energy occurs
storage through Li+intercalation pseudocapacitance.Nature Materials,2013,12
(6): 518-522], volume expansion is smaller.[Griffith K, Forse A, the Griffin J, et such as Kent J.Griffith
al.High-rate intercalation without nanostructuring in metastable Nb2O5bronze
Phases.Journal of the American Chemical Society, 2016,138 (28): 8888-8899] it utilizes and forges
Burning method is prepared for the Nb of four kinds of different crystal forms2O5, there is TT phase, T-phase, B phase and H phase.Document records [Zeng G, Wang H, Guo
J,et al.Fabrication of Nb2O5/C nanocomposites as a high performance anode for
Lithium ion battery.Chinese Chemical Letters, 2017,28 (4): 755-758] T-phase Nb2O5Have
Fake capacitance behavior, since the interplanar distance of its (001) isAnd the diameter of lithium ion only hasTherefore lithium ion is embedding
Enter or deviate from T-Nb2O5(001) crystal face more relatively easily.But the Nb of intercalation occurs2O5Also have simultaneously
Disadvantage, such as the lower electric conductivity of itself, this disadvantage are paid close attention to by numerous researchers, they are adjusted by changing its pattern
It controls its nanosizing and carries out compound and doping to it to be modified, improve its electric conductivity.
There is no largely improve Nb for current existing method2O5The electric conductivity of itself, to improve it as lithium ion
The specific discharge capacity of cell negative electrode material.And existing preparation method process complexity is cumbersome, with high costs, therefore, exploitation one
The preparation Nb that kind is inexpensive, reaction time is short2O5The method of electrode, this has very big research significance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation cost is cheap, the Nb of the special hair tripe shape of sample topography2O5Lithium ion
The preparation method of battery electrode material, can be prepared by preparation method of the invention be uniformly dispersed, the hair tripe shape of stable structure
Nb2O5Lithium ion battery electrode material, and this electrode material shows very high specific discharge capacity.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) the analytically pure oxalic acid hydrate niobium of 0.60~1.0g is added in 30ml distilled water first and is stirred evenly, obtained transparent
Solution A;
2) then the glucose of 1.2~2.0g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle, in 120~160 DEG C of hydro-thermal reactions in homogeneous reaction instrument after being sealed,
It is precipitated after cooled to room temperature after reaction;
5) predecessor D will be dried to obtain in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed;
6) it takes the predecessor D of 1.0~1.8g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.2~0.6g to be added in 30~60ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, in 160~200 DEG C of progress secondary waters
Thermal response precipitates after cooled to room temperature after reaction;
9) by after the resulting sediment of step 8) is washed respectively, alcohol is washed in freeze drying box dry hair tripe shape Nb2O5
Lithium ion battery electrode material.
Step 3) the ultrasonic disperse time is 20~60min.
The packing ratio that step 4) the mixed liquor C is added to reaction kettle is 30~60%.
Step 4) the hydro-thermal reaction time be 12~for 24 hours.
The drying temperature of the step 5) vacuum oven is 60~80 DEG C.
Step 8) the hydro-thermal reaction time be 12~for 24 hours.
Step 9) the freeze-drying temperature is -40~-30 DEG C, and drying time is 8~12h.
The method that the present invention uses secondary hydro-thermal, prepares the hair tripe shape Nb that crystallinity is preferable, is evenly distributed2O5Nanometer material
Material, can be in favor of regulating and controlling the structure of material prepared as carbon source and surfactant using different oleic acid additive amounts
And pattern, simple process and low cost.
Detailed description of the invention
Fig. 1 is the Nb of hair tripe shape prepared by the embodiment of the present invention 12O5The XRD spectrum of lithium ion battery electrode material.
Fig. 2 is the Nb of hair tripe shape prepared by the embodiment of the present invention 12O5The SEM photograph of lithium ion battery electrode material.
Fig. 3 is the Nb of hair tripe shape prepared by the embodiment of the present invention 12O5The cycle performance picture of lithium ion battery electrode material.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1:
1) the analytically pure oxalic acid hydrate niobium of 0.6g is added in 30ml distilled water first and is stirred evenly, obtain clear solution A;
2) then the glucose of 1.2g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse 20min obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle by 30% packing ratio, in 120 DEG C in homogeneous reaction instrument after being sealed
Hydro-thermal reaction for 24 hours, precipitates after cooled to room temperature after reaction;
5) forerunner will be dried to obtain in 70 DEG C in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed
Object D;
6) it takes the predecessor D of 1.8g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.6g to be added in 60ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 160 DEG C
It should be precipitated after cooled to room temperature after reaction for 24 hours;
9) hair will be obtained in -40 DEG C of dry 8h in freeze drying box after the resulting sediment of step 8) is washed respectively, alcohol is washed
The Nb of tripe shape2O5Lithium ion battery electrode material.
T-Nb has successfully been prepared using the present invention as can be seen from Figure 12O5.It can be seen that its diffraction maximum corresponds to
(001), (180), (181), (002), (380) and (202) crystal face illustrates that sample is pure T-Nb2O5。
As can be seen from Figure 2, prepared hair tripe shape Nb2O5It is uniformly dispersed, many spillikins can be clearly seen and grow in piece
On, as the shape of hair tripe.
Fig. 3 is hair tripe shape Nb prepared by embodiment 12O5The cycle performance picture (current density 100mA/g) of nano material.
In the case where current density is 100mA/g, the specific capacity of product is reached for 375mAh/g, and after 40 circle of circulation, Nb2O5The ratio of electrode
Capacity also has the trend of rising.Therefore by Nb2O5When as lithium ion battery negative material, very high electric discharge specific volume is shown
Amount and good invertibity.
Embodiment 2:
1) the analytically pure oxalic acid hydrate niobium of 0.7g is added in 30ml distilled water first and is stirred evenly, obtain clear solution A;
2) then the glucose of 1.4g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse 30min obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle by 50% packing ratio, in 150 DEG C in homogeneous reaction instrument after being sealed
Hydro-thermal reaction 15h is precipitated after cooled to room temperature after reaction;
5) forerunner will be dried to obtain in 60 DEG C in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed
Object D;
6) it takes the predecessor D of 1.6g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.5g to be added in 50ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 170 DEG C
21h is answered, is precipitated after cooled to room temperature after reaction;
9) hair will be obtained in -30 DEG C of dry 12h in freeze drying box after the resulting sediment of step 8) is washed respectively, alcohol is washed
The Nb of tripe shape2O5Lithium ion battery electrode material.
Embodiment 3:
1) the analytically pure oxalic acid hydrate niobium of 0.8g is added in 30ml distilled water first and is stirred evenly, obtain clear solution A;
2) then the glucose of 1.6g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse 40min obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle by 60% packing ratio, in 16 DEG C in homogeneous reaction instrument after being sealed
Hydro-thermal reaction 12h is precipitated after cooled to room temperature after reaction;
5) forerunner will be dried to obtain in 80 DEG C in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed
Object D;
6) it takes the predecessor D of 1.4g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.4g to be added in 45ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 180 DEG C
18h is answered, is precipitated after cooled to room temperature after reaction;
9) hair will be obtained in -35 DEG C of dry 10h in freeze drying box after the resulting sediment of step 8) is washed respectively, alcohol is washed
The Nb of tripe shape2O5Lithium ion battery electrode material.
Embodiment 4:
1) the analytically pure oxalic acid hydrate niobium of 0.9g is added in 30ml distilled water first and is stirred evenly, obtain clear solution A;
2) then the glucose of 1.8g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse 50min obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle by 40% packing ratio, in 130 DEG C in homogeneous reaction instrument after being sealed
Hydro-thermal reaction 20h is precipitated after cooled to room temperature after reaction;
5) forerunner will be dried to obtain in 65 DEG C in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed
Object D;
6) it takes the predecessor D of 1.2g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.3g to be added in 40ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 190 DEG C
15h is answered, is precipitated after cooled to room temperature after reaction;
9) hair will be obtained in -40 DEG C of dry 11h in freeze drying box after the resulting sediment of step 8) is washed respectively, alcohol is washed
The Nb of tripe shape2O5Lithium ion battery electrode material.
Embodiment 5:
1) the analytically pure oxalic acid hydrate niobium of 1.0g is added in 30ml distilled water first and is stirred evenly, obtain clear solution A;
2) then the glucose of 2.0g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse 60min obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle by 50% packing ratio, in 140 DEG C in homogeneous reaction instrument after being sealed
Hydro-thermal reaction 18h is precipitated after cooled to room temperature after reaction;
5) forerunner will be dried to obtain in 75 DEG C in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed
Object D;
6) it takes the predecessor D of 1.0g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.2g to be added in 30ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 200 DEG C
12h is answered, is precipitated after cooled to room temperature after reaction;
9) hair will be obtained in -30 DEG C of dry 9h in freeze drying box after the resulting sediment of step 8) is washed respectively, alcohol is washed
The Nb of tripe shape2O5Lithium ion battery electrode material.
Claims (7)
1. the Nb of a kind of mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that the following steps are included:
1) the analytically pure oxalic acid hydrate niobium of 0.60~1.0g is added in 30ml distilled water first and is stirred evenly, obtain clear solution
A;
2) then the glucose of 1.2~2.0g is added in 30ml distilled water and is stirred evenly, obtain clear solution B;
3) solution A and solution B are mixed, then ultrasonic disperse obtains mixed liquor C;
4) mixed liquor C is added in reaction kettle, in 120~160 DEG C of hydro-thermal reactions, reaction in homogeneous reaction instrument after being sealed
After precipitate after cooled to room temperature;
5) predecessor D will be dried to obtain in a vacuum drying oven after the resulting sediment of step 4) is washed respectively, alcohol is washed;
6) it takes the predecessor D of 1.0~1.8g to be added in 30ml distilled water to stir evenly, obtains solution E;
7) it takes the melamine of 0.2~0.6g to be added in 30~60ml oleic acid again, stirs evenly, obtain solution F;
8) solution E and solution F are mixed, is stirred evenly, is added in reaction in kettle, it is anti-to carry out secondary hydro-thermal in 160~200 DEG C
It answers, is precipitated after cooled to room temperature after reaction;
9) by after the resulting sediment of step 8) is washed respectively, alcohol is washed in freeze drying box dry hair tripe shape Nb2O5Lithium from
Sub- battery electrode material.
2. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
Step 3) the ultrasonic disperse time is 20~60min.
3. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
The packing ratio that step 4) the mixed liquor C is added to reaction kettle is 30~60%.
4. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
Step 4) the hydro-thermal reaction time be 12~for 24 hours.
5. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
The drying temperature of the step 5) vacuum oven is 60~80 DEG C.
6. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
Step 8) the hydro-thermal reaction time be 12~for 24 hours.
7. the Nb of according to claim 1 mao of tripe shape2O5The preparation method of lithium ion battery electrode material, it is characterised in that:
Step 9) the freeze-drying temperature is -40~-30 DEG C, and drying time is 8~12h.
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