CN104701498B - A kind of preparation method of biological carbon/ammonium vanadate anode material for lithium-ion batteries - Google Patents
A kind of preparation method of biological carbon/ammonium vanadate anode material for lithium-ion batteries Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries, biomass precast body is cleaned and is dried after shredding, add concentrated nitric acid and carry out homogeneous reaction, obtain product；Then carbonization in tube-type atmosphere furnace after being dried by product sucking filtration, obtains carbonized product；Carry out carbonized product washing sucking filtration, the most i.e. obtain the biological carbon of loose structure；Finally biological carbon is joined the NH obtained in deionized water by ammonium metavanadate4VO3Solution, i.e. can get biological carbon/ammonium vanadate anode material for lithium-ion batteries after putting into hydro-thermal sensing heating instrument.The biological carbon that the present invention prepares/ammonium vanadate composite, has the electric conductivity of excellence, and specific capacity and stability have also been obtained and significantly improves, preparation method of the present invention is simple, and reaction temperature is low, and the response time is short, and without subsequent treatment, environmentally friendly, large-scale production can be suitable for.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries preparation field, be specifically related to a kind of biological carbon/ammonium vanadate
The preparation method of anode material for lithium-ion batteries.
Background technology
Oxyvanadium compound and vanadate intercalation materials of li ions are due to relative inexpensiveness, and synthetic method is simple, specific volume
Amount high becomes the focus of Recent study.Ammonium vanadate nano material is as the important vanadic acid of a class
Salt, has the layer structure that vanadium oxygen polyhedron is constituted, wherein, NH4+It is positioned at the layer that vanadium oxygen polyhedron is formed
Between so that it is there is the open architecture that can embed metal ion and the characteristic that thermal induced phase transition occurs.Therefore,
Ammonium vanadate is generally of preferable conductivity performance, and has higher theoretical specific capacity, is expected to become a class
Novel lithium ion battery electrode material.
Prepare NH at present4V3O8Method mainly have: the sedimentation method and hydro-thermal method.Wherein, hydro-thermal method is one
Plant effectively route of synthesis.The pattern of synthesis also has a shuttle shape, flower-shaped and banding etc..But the sedimentation method are closed
Become NH4V3O8There is the shortcomings such as course of reaction is wayward, have side reaction generation, product purity low, water
Full-boiled process synthesis NH4V3O8There is the shortcomings such as reaction temperature is of a relatively high, the response time is longer.And vanadic acid
Ammonium is little due to itself electrical conductivity, causes its electric conductivity poor.
Summary of the invention
It is an object of the invention to provide the preparation of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries
Method, with the defect overcoming above-mentioned prior art to exist, can prepare conduction by the preparation method of the present invention
Excellent performance, specific capacity height, stable cycle performance and the biological carbon/vanadic acid ammonia composite of life-span length.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
The preparation method of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries, comprises the following steps:
(1) biomass precast body is cleaned removing surface impurity, shred to obtain homogeneous bulky A；
(2) homogeneous bulky A is dried to obtain block B；
(3) carry out homogeneous reaction after adding concentrated nitric acid in block B, obtain product C；
(4) carry out carbonization after being dried by product C sucking filtration, obtain carbonized product D；
(5) carbonized product D is added soak with ethanol, then with sucking filtration after distilled water and washing with alcohol, then
It is dried, obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is 0.10～0.30mol/L
NH4VO3Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5～2.0, to NH4VO3In solution F
Add biological carbon E according to the mass ratio that E:F is 1:10～1:20, then the mixture obtained is proceeded to reactor
In, after reactor is sealed, it is placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400～800KHz
By room temperature to 160～220 DEG C, and it is incubated 10～30min, is then cooled to 60～80 DEG C, be incubated 10～20
Min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, then powder body product is used deionized water respectively
With soaked in absolute ethyl alcohol and washing, then it is dried, grinds, obtain NH4V3O8/ C nano complex.
Further, in step (1), biomass precast body is Pericarpium Musae, Crusta Penaeus seu Panulirus, Chinese parasol leaf, little
One in Wheat Straw or corn straw.
Further, in step (1), the size dimension of homogeneous bulky A is 4～6mm.
Further, homogeneous bulky A is dried at room temperature for 0.5～1h by step (2) and obtains block B.
Further, in step (3), the concentration of concentrated nitric acid is 2～5mol L-1。
Further, in step (3), the condition of homogeneous reaction is: with the heating rate liter of 15 DEG C/min
Temperature is incubated 20～50min to 150 DEG C～180 DEG C, then naturally cools to room temperature.
Further, carbon in tube-type atmosphere furnace is moved into after product C sucking filtration being dried by step (4)
Changing, described tube-type atmosphere furnace is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to by 10min
50 DEG C, after 75min is warmed up to 600～800 DEG C, and insulation 60～180min at this temperature.
Further, in step (8) by powder body product respectively by deionized water and soaked in absolute ethyl alcohol and
The detailed process of washing is: first with deionized water, powder body product is soaked 10～20min, then uses deionization
Water washs 5～10 times, then by soaked in absolute ethyl alcohol 10～20min, then with absolute ethanol washing 5～10
Secondary.
Further, the baking temperature in step (8) is 80～110 DEG C, and the time is 6～8h.
The preparation method of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries, comprises the following steps:
(1) by Chinese parasol leaf clean remove surface impurity, shred size dimension is the homogeneous blocks of 4mm
Shape A；
(2) homogeneous bulky A is dried at room temperature for 0.5h and obtains block B；
(3) adding concentration in block B is 2mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 20min after 150 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is full of nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 600 DEG C, it is incubated 180min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after three times, is then dried, and obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.20mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:10 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400KHz by room temperature to
160 DEG C, and it is incubated 10min, then it is cooled to 60 DEG C, is incubated 10min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
10min, is then washed with deionized 5 times, then uses soaked in absolute ethyl alcohol 10min, then with anhydrous
Washing with alcohol 5 times, is then dried 6h at a temperature of 80 DEG C, then grinds dried solid product,
Obtain the NH of porous flake4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
Compared with prior art, the present invention has a following useful technique effect:
Biomass precast body of the present invention prepares biological carbon, use biological carbon and ammonium metavanadate prepare biological carbon/
Ammonium vanadate anode material for lithium-ion batteries, owing to biological carbon has bigger interlamellar spacing, is possible not only to as lithium
The quickly transmission offer condition of ion, increases the capacity of material, it is also possible to form intramolecular hydrogen bond, stable
The structure of material, and then the cyclical stability of material can be improved.Additionally biological carbon is having of short texture
Sequence porous material, has bigger specific surface area, can be effectively increased contacting of electrode material and electrolyte
Area, and then the electric conductivity of material can be significantly improved.The present invention is by electric conductivity excellent for biological carbon and vanadium
The specific capacity that acid ammonia is high has organically been compounded in together, prepares biological carbon/ammonium vanadate composite, will
The biological carbon turned waste into wealth is combined with having height ratio capacity/ammonium vanadate material, and the migration for electronics carries
Supply good passage, added the migration velocity of electronics, improve the electric conductivity of material, can be more preferable
Realize fast charging and discharging.It is raw that the present invention selects have the hydro-thermal actinobolia synthesis that synthesis temperature is low, the cycle is short
Thing carbon/ammonium vanadate composite, prepared biological carbon/ammonium vanadate composite, there is the electric conductivity of excellence
(the original conductivity of ammonium vanadate can be made to obtain the lifting of the order of magnitude), and specific capacity is (former by ammonium vanadate
The specific capacity having 260mAh/g rises to 350mAh/g) have also been obtained and significantly improve, prepared by the present invention
Method is simple, and reaction temperature is low, and the response time is short, and without subsequent treatment, environmentally friendly, permissible
It is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction (XRD) of the anode material for lithium-ion batteries of the embodiment of the present invention 1 preparation
Collection of illustrative plates；
Fig. 2 is that the scanning electron microscope (SEM) of the biological carbon that the embodiment of the present invention 1 step (5) obtains shines
Sheet；
Fig. 3 is the scanning electron microscope (SEM) of the anode material for lithium-ion batteries of the embodiment of the present invention 1 preparation
Photo.
Detailed description of the invention
Below embodiments of the present invention are described in further detail:
The preparation method of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries, comprises the following steps:
(1) by biomass precast body, (biomass precast body is Pericarpium Musae, Crusta Penaeus seu Panulirus, Chinese parasol leaf, Semen Tritici aestivi
One in straw or corn straw) clean remove surface impurity, shred size dimension is 4～6mm
Homogeneous bulky A；
(2) homogeneous bulky A is dried at room temperature for 0.5～1h and obtains block B；
(3) adding concentration in block B is 2～5mol L-1Concentrated nitric acid after carry out homogeneous reaction, all
The condition of phase reaction is: be incubated after being warming up to 150 DEG C～180 DEG C with the heating rate of 15 DEG C/min
20～50min, then naturally cool to room temperature, obtain product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 600～800 DEG C, it is incubated 60～180min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after three times, is then dried, and obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is 0.10～0.30mol/L
NH4VO3Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5～2.0, to NH4VO3In solution F
Add biological carbon E according to the mass ratio that E:F is 1:10～1:20, then the mixture obtained is proceeded to reactor
In, after reactor is sealed, it is placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400～800KHz
By room temperature to 160～220 DEG C, and it is incubated 10～30min, is then cooled to 60～80 DEG C, be incubated 10～20
Min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
10～20min, then it is washed with deionized 5～10 times, then by soaked in absolute ethyl alcohol 10～20min, so
Rear absolute ethanol washing 5～10 times, be then dried 6～8h at a temperature of 80～110 DEG C, then to after drying
Solid product grind, obtain the NH of porous flake or nano bar-shape4V3O8/ C nano complex, is
Biological carbon/ammonium vanadate anode material for lithium-ion batteries.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
(1) by Chinese parasol leaf clean remove surface impurity, shred size dimension is the homogeneous blocks of 4mm
Shape A；
(2) homogeneous bulky A is dried at room temperature for 0.5h and obtains block B；
(3) adding concentration in block B is 2mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 20min after 150 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 600 DEG C, it is incubated 180min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after after three times, is then dried, obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.20mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:10 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400KHz by room temperature to
160 DEG C, and it is incubated 10min, then it is cooled to 60 DEG C, is incubated 10min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
10min, is then washed with deionized 5 times, then uses soaked in absolute ethyl alcohol 10min, then with anhydrous
Washing with alcohol 5 times, is then dried 6h at a temperature of 80 DEG C, then grinds dried solid product,
Obtain the NH of porous flake4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
It will be seen from figure 1 that positive electrode good crystallinity prepared by the present embodiment, purity is higher；From figure
2 it can be seen that biological carbon E prepared in step (5) is porous flake；From figure 3, it can be seen that this
Biological carbon prepared by embodiment/ammonium vanadate positive electrode is porous flake.
Embodiment 2
(1) by wheat stalk clean remove surface impurity, shred size dimension is the homogeneous blocks of 6mm
Shape A；
(2) homogeneous bulky A is dried at room temperature for 1h and obtains block B；
(3) adding concentration in block B is 5mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 50min after 180 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 800 DEG C, it is incubated 60min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then uses washing with alcohol again three times with distilled water wash
Sucking filtration after after three times, is then dried, obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.10mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 2.0, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:20 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 800KHz by room temperature to
220 DEG C, and it is incubated 30min, then it is cooled to 80 DEG C, is incubated 20min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
20min, is then washed with deionized 10 times, then uses soaked in absolute ethyl alcohol 20min, then with anhydrous
Washing with alcohol 10 times, is then dried 8h at a temperature of 110 DEG C, then grinds dried solid product,
Obtain the NH of porous flake4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
Embodiment 3
(1) by corn straw clean remove surface impurity, shred size dimension is the homogeneous blocks of 5mm
Shape A；
(2) homogeneous bulky A is dried at room temperature for 0.6h and obtains block B；
(3) adding concentration in block B is 4mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 30min after 160 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 700 DEG C, it is incubated 100min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after after three times, is then dried, obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.30mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 1.0, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:15 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 500KHz by room temperature to
170 DEG C, and it is incubated 15min, then it is cooled to 65 DEG C, is incubated 15min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
15min, is then washed with deionized 8 times, then uses soaked in absolute ethyl alcohol 15min, then use anhydrous second
Alcohol washs 8 times, is then dried 7h at a temperature of 100 DEG C, then grinds dried solid product,
Obtain the NH of porous flake4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
Embodiment 4
(1) by Pericarpium Musae clean remove surface impurity, shred size dimension is the homogeneous bulky of 5mm
A；
(2) homogeneous bulky A is dried at room temperature for 0.5h and obtains block B；
(3) adding concentration in block B is 3mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 40min after 170 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 600 DEG C, it is incubated 150min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after three times, is then dried, and obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.20mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 1.5, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:10 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 600KHz by room temperature to
180 DEG C, and it is incubated 25min, then it is cooled to 70 DEG C, is incubated 10min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
10min, is then washed with deionized 5 times, then uses soaked in absolute ethyl alcohol 15min, then use anhydrous second
Alcohol washs 8 times, is then dried 7h at a temperature of 90 DEG C, then grinds dried solid product,
NH to nano bar-shape4V3O8/ C nano complex, is biological carbon/ammonium vanadate lithium ion cell positive
Material.
Embodiment 5
(1) Crusta Penaeus seu Panulirus is cleaned removing surface impurity, shred to obtain the homogeneous bulky A that size dimension is 6mm；
(2) homogeneous bulky A is dried at room temperature for 1h and obtains block B；
(3) adding concentration in block B is 2mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 50min after 180 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 800 DEG C, it is incubated 80min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after three times, is then dried, and obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.30mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 2.0, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:20 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 700KHz by room temperature to
220 DEG C, and it is incubated 30min, then it is cooled to 80 DEG C, is incubated 20min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
20min, is then washed with deionized 10 times, then uses soaked in absolute ethyl alcohol 10min, then with anhydrous
Washing with alcohol 5 times, is then dried 6h at a temperature of 110 DEG C, then grinds dried solid product,
Obtain the NH of nano bar-shape4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
Claims (9)
1. the preparation method of biological carbon/ammonium vanadate anode material for lithium-ion batteries, it is characterised in that
Comprise the following steps:
(1) biomass precast body is cleaned removing surface impurity, shred to obtain homogeneous bulky A；
(2) homogeneous bulky A is dried to obtain block B；
(3), after adding concentrated nitric acid in block B, it is warming up to 150 DEG C with the heating rate of 15 DEG C/min
～after 180 DEG C, it is incubated 20～50min, then naturally cool to room temperature, obtain product C；
(4) carry out carbonization after being dried by product C sucking filtration, obtain carbonized product D；
(5) carbonized product D is added soak with ethanol, then with sucking filtration after distilled water and washing with alcohol, then
It is dried, obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is 0.10～0.30mol/L
NH4VO3Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5～2.0, to NH4VO3In solution F
Add biological carbon E according to the mass ratio that E:F is 1:10～1:20, then the mixture obtained is proceeded to reactor
In, after reactor is sealed, it is placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400～800KHz
By room temperature to 160～220 DEG C, and it is incubated 10～30min, is then cooled to 60～80 DEG C, be incubated 10～20
Min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, then powder body product is used deionized water respectively
With soaked in absolute ethyl alcohol and washing, then it is dried, grinds, obtain NH4V3O8/ C nano complex.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that in step (1) biomass precast body be Pericarpium Musae, Crusta Penaeus seu Panulirus, Chinese parasol leaf,
One in wheat stalk or corn straw.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that in step (1), the size dimension of homogeneous bulky A is 4～6mm.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that in step (2), homogeneous bulky A is dried at room temperature for 0.5～1h and obtains block
Shape B.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that in step (3), the concentration of concentrated nitric acid is 2～5mol L-1。
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that move into tubular type atmosphere after being dried by product C sucking filtration in step (4)
Carbonization in stove, described tube-type atmosphere furnace is passed through nitrogen, and the condition of carbonization is: 10min is by tube-type atmosphere furnace
It is warmed up to 50 DEG C, after 75min is warmed up to 600～800 DEG C, and insulation 60～180min at this temperature.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that by powder body product respectively with deionized water and dehydrated alcohol leaching in step (8)
The detailed process of bubble and washing is: first with deionized water, powder body product is soaked 10～20min, then spends
Ionized water washs 5～10 times, then by soaked in absolute ethyl alcohol 10～20min, then uses absolute ethanol washing
5～10 times.
The system of a kind of biological carbon/ammonium vanadate anode material for lithium-ion batteries the most according to claim 1
Preparation Method, it is characterised in that the baking temperature in step (8) is 80～110 DEG C, the time is 6～8h.
9. the preparation method of biological carbon/ammonium vanadate anode material for lithium-ion batteries, it is characterised in that
Comprise the following steps:
(1) by Chinese parasol leaf clean remove surface impurity, shred size dimension is the homogeneous blocks of 4mm
Shape A；
(2) homogeneous bulky A is dried at room temperature for 0.5h and obtains block B；
(3) adding concentration in block B is 2mol L-1Concentrated nitric acid after, with the liter of 15 DEG C/min
Temperature ramp is incubated 20min after 150 DEG C, then naturally cools to room temperature, obtains product C；
(4) move in tube-type atmosphere furnace after product C sucking filtration being dried and carry out carbonization, tubular type atmosphere
Stove is passed through nitrogen, and the condition of carbonization is: tube-type atmosphere furnace is warmed up to 50 DEG C by 10min, and 75min heats up
After 600 DEG C, it is incubated 180min, obtains carbonized product D；
(5) carbonized product D is added soak with ethanol, then use washing with alcohol again three times with distilled water wash
Sucking filtration after three times, is then dried, and obtains biological carbon E of loose structure；
(6) being dissolved in deionized water by ammonium metavanadate, prepared concentration is the NH of 0.20mol/L4VO3
Solution F；
(7) by NH4VO3The pH value of solution F is adjusted to 0.5, to NH4VO3In solution F according to
E:F is that the mass ratio of 1:10 adds biological carbon E, then proceeds in reactor by the mixture obtained, will be anti-
After answering still to seal, be placed in hydro-thermal sensing heating instrument, with the induction frequencies of 400KHz by room temperature to
160 DEG C, and it is incubated 10min, then it is cooled to 60 DEG C, is incubated 10min, obtains suspension；
(8) suspension is centrifugally separating to obtain powder body product, powder body product is first soaked with deionized water
10min, is then washed with deionized 5 times, then uses soaked in absolute ethyl alcohol 10min, then with anhydrous
Washing with alcohol 5 times, is then dried 6h at a temperature of 80 DEG C, then grinds dried solid product,
Obtain the NH of porous flake4V3O8/ C nano complex, is just being biological carbon/ammonium vanadate lithium ion battery
Pole material.
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